Foaming compositions and methods for making and using the composition

Information

  • Patent Grant
  • 6479560
  • Patent Number
    6,479,560
  • Date Filed
    Wednesday, May 24, 2000
    24 years ago
  • Date Issued
    Tuesday, November 12, 2002
    22 years ago
Abstract
A low-temperature foam compositions and that are produced from an epoxy compound and an acid source can be substantially free of polyurethane or isocyanate chemistry. The disclosed compositions and precursors thereof reduce, if not eliminate, the presence of conventional undesirable compounds and by-products thereof.
Description




FIELD OF THE INVENTION




The invention relates to foam compositions, precursors thereof and methods for making foam compositions and foam containing articles.




BACKGROUND OF THE INVENTION




Foams are employed in a wide range of commercial applications including applications requiring thermal and sound insulation such as automotive and construction environments, among others. In the automotive industry, foams are typically formed in situ, and can be used to fill cavities such as pillars and rocker panels, and to dampen sound transmission. In situ foam formation has typically been accomplished by using a polyurethane foam based on isocyanate chemistry. Certain polyurethane foam components and by-products thereof are believed to have an undesirable environmental impact. Consequently, there is a need in this art for a low-temperature foam which is cost-effective and substantially free of undesirable materials.




SUMMARY OF THE INVENTION




The invention is capable of solving problems associated with conventional foam formulations by providing foam compositions and precursors thereto which do not require the use of isocyanates. The inventive compositions and precursors can thereof reduce, if not eliminate, the presence of conventional undesirable compounds and by-products thereof while providing benefits associated with conventional foams, e.g, sound/vibration dampening, thermal insulation, structure reinforcement, floatation, energy dissipation, among other benefits. In addition, the inventive foam has a reduced cured and tack time in comparison to conventional polyurethane foams. These properties in turn improve the efficiency of manufacturing processes that employ foam.




One aspect of the invention relates to a method of reacting an epoxy compound and a hydrogen donor or acid compound at ambient conditions to produce a foam. This reaction can produce a relatively large exotherm. The heat released by the exothermic reaction can be sufficient to drive an endothermic blowing agent, thus creating a foam virtually instantaneously. In fact, the exothermic reaction can be sufficiently large to cause a blowing agent entrapped within, for example, thermoplastic powders to expand thereby forming a foam.




Another aspect of the invention relates to a method of containing the foam during expansion by expanding the foam within a containment or control means. The control means confines the expanding foam and determines the direction of expansion. While any suitable control means can be employed, a polymeric bag or sack is desirable. If desired, the polymer bag comprises an adhesive material, e.g., the bag adhesive is activated by the exothermic foam reaction and affixes the resultant foam to a substrate. The polymeric bag can be fabricated from a virtually unlimited array of materials and configured into any desirable shape, e.g., a honeycomb structure, replicating an automotive cavity, etc.




The inventive foam can be employed in a wide array of end-uses. Examples of such uses include thermal insulation such as appliances, e.g., refrigerators, hot water heaters, etc; aircraft; commercial or residential construction such as spray or rigid insulation for walls, doors, cavity/widow sealant, acoustical control, etc.; packing material, e.g., foam-in-place; marine foams; environmental control, e.g., spill containment; footware; furniture; toy and consumer goods; protective equipment such as pads, helmets, etc.; fluid filtration; transportation industry uses, e.g., sound dampeners, structural supporting material, etc. for cars, trucks and heavy duty vehicles; vehicle repair; gasketing material; medical uses such as casts, emergency immobilization, etc.; artistic medium such as decorative brick/block, figures, etc.; among others.











BRIEF DESCRIPTION OF THE DRAWINGS





FIG. 1

is a graphical representation of the foam reaction rate and temperature as a function of percent acid.





FIGS. 2A and 2B

are a schematic drawings of assemblies that can be employed for dispensing the inventive foam within a defined cavity or area.











DETAILED DESCRIPTION




The invention is based, at least in part, on the surprising discovery that superior foam compositions can be produced from epoxy compounds and acids or hydrogen donor compounds, and in particular, a reaction of the epoxy compounds with the acid source.




Moreover, the inventive compositions can be polyurethane and/or isocyanate free. By “free” it is meant that the inventive compositions before or after foaming contain less than about 10 wt. % polyurethane and/or isocyanurates, isocyanate, and in most cases 0 wt. %. While the presence of such compounds does not adversely affect the reaction described below in greater detail, these materials can be obviated by employing the inventive formulations. The instant invention, therefore, provides a foam which can be used with or instead of urethane/isocyanate based foams and foaming systems.




The inventive foam composition is typically obtained from the reaction of one or more foam precursors. The precursor(s) comprise (i) at least one epoxy compound, and (ii) at least one acid source, i.e., a hydrogen donor or an acid, e.g., phosphoric acid, or a compound such as a photoinitiator which can upon activation provide a hydrogen donor or an acid, and (iii) at least one expansion or blowing agent, among other components. An exothermic reaction between the epoxy and hydrogen donor or acid can activate the expansion or blowing agent thereby producing a foam.




The foam precursor(s) can comprise a single phase system that is activated in response to a source of energy, e.g., heat, UV or electron beam or laser radiation, among other energy sources, or a two component system (an A side precursor and a B side precursor) that are contacted together to produce a foam. When a two component system is employed the epoxy and acid source are provided in separate “side” components.




Alternatively, the foam precursor(s) can comprise a two component system that is activated in response to a source of, e.g., heat, UV or electron beam or laser radiation, among other energy sources. The two component system can include an acid source as well as a photoinitiator.




The first component of the precursor(s), an epoxy compound, comprises about 10 to about 80 wt % of the precursor(s). Examples of suitable epoxy compounds include bis-phenol A epoxy, bis-F epoxy, epoxy-modified elastomers, epoxy-modified polybutene, epoxy-modified polybutadiene, epoxy-modified ethylene-propylene-diene rubber (EPDM), cycloaliphatic epoxy, novolac compounds, and mixtures thereof, among others. When a two component system is employed, the epoxy is located on the A-side, or otherwise prevented from prematurely reacting with the acid or other precursors.




The first component of the precursor can be tailored by adding one or more modifiers. For best results, the modifier is solublized by the epoxy or miscible with the epoxy. Examples of suitable modifiers can comprise at least one member selected from the group consisting of styrene and co-polymers thereof, vinyls and co-polymers thereof, elastomers such as nitrile. ethylene acrylic rubber, mixtures thereof, among others compounds that do not adversely impact the exothermic reaction. Some commercially available materials that can be employed as a modifier comprise Kraton® (Shell Chemical), Vamac® (DuPont), Piccolastic® (Hercules), Phenoxy® (Paphen), SAA® (styrene-allyl-alcohol copolymer (ARCO), G-Cryl® (Henkel), Rohagum® (Rhomtech), acrylate modified acidic adhesion promoting agent (acid functional oligomer, RadCure®), mixtures thereof, among others. Normally, the epoxy modifier comprises about 2 to about 50 wt. % of the composition prior to foaming.




A second component of the precursor(s) is the acid source. When a two component precursor system is employed, the acid source is present in the “B side” of the foam precursors. The hydrogen donor or acid usually comprises about 1% to about 30 wt. % of the precursor, and in particular, about 3% to about 15% of precursor B-side precursors. Examples of suitable acid sources include Lewis acids such as sulfonic acids, phosphoric acid, citric acid, carboxylic acid, glycolic, tannic, 1,2,4,5-Benzenenetracarboxylic acid, citraconic acid, L-(+)-Citrulline, fumaric, maleic, azelaic, oxalic acids, and mixtures thereof, among others. Particularly desirable results have been achieved by employing at least one of sulfonic, phosphoric acids and other acid functional compounds, e.g., acid functional acrylics. Depending upon the desired reaction rate and resultant foam characteristics, a relatively concentrated acid can be employed. An example of such a concentrated acid comprises a phosphoric acid that is substantially free of water. By “substantially free” it is meant that the acid contains less than about 10 wt. % and normally less than about 5 wt. % water. Substantially water free acid can be obtained by distilling commercially available acids, e.g., 75% phosphoric acid can be concentrated by distillation. In the case of phosphoric acid, concentration by distillation permits obtaining at least one of meta, ortho and pyro-phosphoric acids. At least one of ortho or pyro-phosphoric acid and mixtures thereof are effective as an acid source when a relatively strong and rigid foam is desired, e.g., an acid source comprising about 50 to greater than 90 wt. % ortho-phosphoric acid. If desired, the acid can comprise an acid functionally equivalent to the hydrogen donor released by a UV photoinitiator, e.g., replace a portion of the photoinitiator with its corresponding acid.




In one aspect of the invention, an acid substantially free of water is employed to obtain a foam precursor that generates foam having improved structural properties, e.g., foam having a flexural strength about 20 to 100% greater than many conventional materials such as wooden particle board. By employing a substantially water free acid as a foam precursor, the resultant foam has a lower expansion and water absorption, and greater structural strength and adhesion, e.g., to a painted or primed metal surface, wood, particle board, corrugated paper such as honeycomb, ABS, Formica®, Masonite®, thermoplastics such as polystyrene, among other surfaces. Substantially water free acids can also permit using a wider range of precursors, e.g., non-polyol carriers.




The adhesion of the foam to certain substrates, e.g., ABS, can be improved by pre-treating or priming the substrate surface. An example of a suitable primer comprises applying a silane coating (e.g., Z6040 supplied by Dow Chemical) onto the surface. The silane forms a coating to which the foam can adhere. Adhesion can also be improved by embossing or roughening the surface of the substrate.




A mechanical fastener can be attached to or incorporated within the substrate such that the foam embeds the fastener. The fastener can comprise a plurality of protrusions, studs or mechanical fastening means having any desirable shape can be located within a cavity to be filled with foam and/or attached to the substrate that contacts the foam. When studs are employed, the studs can be welded, e.g., sonically welded to a thermoplastic, within a cavity to be filled with foam. Protrusions can also be affixed within the cavity or upon the surface by a suitable adhesive, or by mechanical attachment. The height and specific configuration of the protrusions depends upon the application. These protrusions can be fabricated from any suitable material such as thermoplastics such as nylon, metal, among other materials. When introduced into the cavity, the inventive foam composition or precursors thereof embeds the protrusions, fills the cavity and embeds the protrusions thereby affixing the foam within the cavity or onto a substrate.




In another aspect of the invention, the hydrogen donor comprises a photo-initiator that becomes active when exposed to a source of energy. While any photoinitiator capable of becoming a hydrogen donor upon activation can be employed, specific examples of a suitable photoinitiators include a UV catalyst such as UVI 6974 (Union Carbide) that is described in greater detail in the aforementioned copending and commonly assigned U.S. non-provisional patent application Ser. Nos. 09/081,966, filed on May 20, 1998 and Ser. No. 09/197,107, filed Nov. 20, 1999, both filed in the name of Jeffrey Pachl et al., and entitled “Curable Sealant Composition”. Alternatively, free radical photoinitiators can be employed. An example of a free radical photo-iniator comprises 2-hydroxy-2-methyl-1-phenyl-propan-1-one, e.g., DAROCUR® 1173 (Ciba-Giegy). Free radical photoinitiators can be employed in systems comprising at least one of monomers and oligomers such as acrylated oligomers, urethane acrylates, acrylated epoxies, acrylated acrylics, acrylated polyesters, acrylated polybutadiene, methacrylated counterparts thereof, among others. When such initiators are employed, the foam precursors can be utilized in a single or multi-phase system.




For example, such a single phase system can be dispensed, exposed to a UV light source or other suitable source of energy that causes the UV catalyst to generate an acid thereby permitting the epoxy or free-radical reaction to occur. The heat released by the exothermic reaction in turn activates an expansion or blowing agent, e.g., a hydrocarbon encapsulated within a thermoplastic, thereby producing a foam. While any suitable single or two phase system can be employed, normally a single phase system produces a foam that is thin relative to a two phase system. Similar to other foam precursors, the radiation activated precursors can be modified for controlling the properties of the precursors or resultant foam, e.g., about 1 to about 20 wt. % polystyrene is added to the epoxy component.




The blowing agent can comprise one or more of the blowing agents recognized in the foam-forming field. Example of suitable blowing agents include water, hydrazide, diphenyloxide-4,4-disulphohydrazide, carbonamide, azocarbonamide, hexamethylene diamine carbamate, sodium bicarbonate, dimethyl ether, methylene chloride, carbon dioxide, fluorocarbons such as difluoroethane, tetrafluoroethane, HFC-4310, azeotropes and isomers thereof, among others; and hydrocarbons such as isobutane, butane, propane, pentane, isopentane, alcohol, isomers thereof; mixtures thereof, among other known blowing agents. Normally, the expansion or blowing agent comprises about 1 to about 40 wt. % of the foam precursor(s). The blowing agent can be present in either the A or B side of a two component system, although the B-side precursor is preferred.




The foam precursor(s) can also include at least one carrier component, e.g., a polyol, and optional components such as thermoplastics. A carrier usually comprises about 1 to about 40 wt. % of the precursor, e.g., preferably about 10-30 wt. %. The carrier typically serves to deliver a component, e.g., an acid, expanding agent, catalyst, mixtures thereof, among others for contact with the epoxy. Examples of suitable carriers comprise at least one member selected from the group of polyols including polyester, polyether, polycarbonate and caprolactone; alcohol, polyvinyl alcohol, synthetic or natural oils such as castor, soy, linseed, glycerin and glycols; water, among other carriers that are preferably miscible with the epoxy and mixtures thereof. When a two component precursor system is employed, these carrier materials are typically added to the acid side or “B side” component of the foam precursors




In addition to the aforementioned epoxy modifiers, the components of the precursor can be tailored by adding one or more modifiers in order to control viscosity, improve stability, physical properties, reaction rates, color, odor, among other characteristics. For best results, the modifier is solublized by the carrier or miscible with a carrier. Examples of suitable modifiers can comprise at least one member selected from the group consisting of natural and synthetic oils such as at least one of castor, soy, canola, linseed, polybutene, epoxidized counterparts thereof, among other oils. Epoxized natural oils such as epoxized castor oil can be employed as a Part A component. The addition of castor oil can also produce a foam having an exterior glaze or skin. Normally, the carrier modifier is used about 2 wt. % to about 50 wt. % of the composition prior to foaming.




Moreover, the density, moisture and temperature resistance among other physical properties of the final foam product can be modified or tailored by adding a thermoplastic, theromset, plastic or resinous material to the epoxy-containing precursor. While any suitable modifying material can be employed, examples of such modifying materials include dicyandiamide (Dicy (Amicure CG 1400)), ethylene vinyl acetate, polypropylene, polyethylene, rubber, phenoxy resin, phenolics, powdered wax, solid epoxy such as bis-A epoxy or modified epoxy, novalac compound, mixtures thereof, among others. For example, depending upon the relative concentration of the components of the precursor, polyvinyl alcohol, hydroscopic polyolefin such as modified polypropylene (as well as other suitable materials) can be employed as modifiers and for absorbing steam or water generated by or during the exothermic reaction. About 1 to about 60 wt. % of modifying material can be added relative to the epoxy, e.g., about 2 wt. % of the precursor(s). The modifying material will normally comprise a powder having a particle size less than about 20 microns and a melting point from about 150 to about 400 F. The modifying material will become fluid and normally melt when exposed to the exothermic reaction temperature. When a two component precursor system is employed, these materials are normally, but not necessarily, combined with the epoxy or “A side”.




The foam precursors can also include a thermoplastic component that can function to modify the properties of the resultant foam, reduce material cost, increase precursor shelf life, among other desirable results. The thermoplastic component of the foam precursor(s) can comprise at least one member selected from the group consisting of acrylonitrile, polyethylene, phenolic, wax, EVA, polypropylene, GMA, acid modified polyethylene, polybutadiene, modified polyethylene blend (such as Bynel® supplied by DuPont Company), SIS or SBS or SEBS blocked copolymers (such Kraton® supplied by Shell Chemical), oligomers, polyolefin, hydroxyl or epoxy functional compounds, among other thermoplastic materials that can be dispersed in a foam precursor and have a melting point less than about the aforementioned exothermic reaction and mixtures thereof. Normally, the thermoplastic component of the precursor will comprise about 1% to about 60 wt. % of the precursor. The thermoplastic component can possess any desirable configuration or particle size. In some cases, the thermoplastic component can form a film or skin upon an exterior surface of the foam thereby improving the resistance of the foam to fluids, e.g., water, gasoline, among other fluids.




In an aspect of the invention, the flame resistance of the foam can be improved by adding an effective amount of at least one member selected from the group consisting of halogenated epoxy as a component of the epoxy (brominated epoxy Erisys® GE-29), aluminum trihydrates, zinc borate, among other commercially available flame retardants. If desired, a halogenated epoxy can replace a portion of the Part A epoxy. Normally, the flame retardant comprises about 0.5 to about 15 wt. % of the unexpanded foam composition.




In one particularly useful aspect of the invention, a liquid or gaseous blowing agent is combined with or encapsulated within a thermoplastic particle or powder, e.g., a hydrocarbon encapsulated within an acrylonitrile shell as in Expancel® that is supplied by Expancel Inc., a division of Akzo Nobel Industries. When a two component precursor system is employed, the shells are normally combined on the B side along with the carrier. These shells can, however, be combined with the A side or in a single phase system so long as the composition of the shells is not substantially affected by the epoxy, e.g, the acrylonitrile or vinylidene chloride shells may be soluble within the epoxy. For example, the shells can be fabricated from polyolefins such polyethylene and polypropylene; vinyls, EVA, nylon, acrylics, among other materials not soluble in the epoxy component, and mixtures thereof could be present in the epoxy component of a two phase precursor system. The shells are selected to melt, soften, expand, rupture or retain their physical configuration depending upon whether or not an open or closed cell foam is desired. The shells can also comprise a distribution of differing particle sizes, composition and activation temperatures, e.g., a foam precursor comprising at least two different particle sizes and activation temperatures. A foam comprising particles having a range of sizes and compositions is especially desirable when producing an acoustical foam. The acoustical properties of a foam can also be improved by employing particles encapsulating blowing agents of more than one composition, e.g., employing shells encapsulating differing blowing agents. Specific examples of suitable encapsulated blowing agents comprise at least one member selected from the group of hydrocarbons such as isobutane and isopentane; fluorocarbons such as 1-1dichloroethene, HFC-134a, HFC-152a; and nitrogen releasing chemical blowing agents such as those supplied as Celogen® by UniRoyal that are encapsulated within any suitable thermoplastic, e.g., 2-methyl 2-propenioc acid methyl ester polymer with 2-propenenitrile and vinylidene chloride polymer and polyvinylidene fluoride. These materials are supplied commercially by Expancel, Inc., a division of Akzo Nobel as Expancels® 051WU, 051DU, 091DU80, 820WU, 820DU, 642WU, 551WU, 551WU80, 461DU or Micropearl® F30D supplied by Pierce and Stevens. These materials can be supplied in either dry or wet form. These materials can also be coated with any suitable material for controlling the activation temperature of the encapsulated blowing agents. An example of a coating comprises an acrylated materials, waxes, among other materials. When the A and B sides are contacted (or in the case of a single phase system exposed to an energy source), the epoxy reacts with the hydrogen or acid thereby releasing heat and causing the expansion agent within the shells to foam. The foam can be characterized by a composite wherein the epoxy reaction product (including of the aforementioned modifying materials) forms a matrix that embeds the expanded shells. Depending upon the physical characteristics desired in the foam, the shells can be open or closed cells.




In a further aspect of the invention, the encapsulated foam precursor can comprise at least one member selected from the group consisting of an acid source, a curing agent, surfactants, epoxy accelerators, among other foam precursors. By curing agent it is intended to mean one or more compositions, other than an acid source, that causes an epoxy functional material to react, exotherm, and cross-link. Examples of curing agents comprise at least one member selected from the group consisting of imidazoles, amines, amides, derivatives thereof, among others. If desired an encapsulated or unencapsulated acid source can be employed in conjunction with an encapsulated curing agent. An example of an encapsulated or polymer bound curing agent comprises those supplied by Landec as Intelimer® 7001, 7002, 7004, 7024 and mixtures thereof. By employing one or more encapsulated or polymer bound foam precursors, it is possible to produce a foam by a multiple stage reaction method wherein the resultant foam has enhanced physical properties, e.g., density, water absorption, hardness and strength.




The foam characteristics can also be modified by adding one or more filler materials to the precursor(s). Conventionally used filler materials comprise at least one of talc, mica, magnesium silicate, oxidized polyethylene, sodium silicate, alcohols, petroleum jelly, aromatic acid methacrylate-mixed half esters, methacrylated polybutadiene, concrete mix (supplied commercially as Quickrete®), arylalkoxy silane, hollow ceramic spheres, inorganic microspheres, dispersants, conventional blowing/expansion agents, flame retardants such as phosphates, borates and halogenated compounds; plasticizers, diluents, pigments, colorants, metal or ceramic powders, soybean hulls, pecan hulls, rice hull, antimicrobial agents such as fungicides, fumed silica, abrasive materials, magnetic materials, anti-static or conductive materials, mixtures thereof, among others. If desired calcium carbonate can be added to the foam precursor for increasing the hardness and density of the resultant foam. When included the filler comprises about 1 to about 60 wt. % of the foam precursors.




The inventive foam can be matrix that embeds or contacts other materials in order to obtain a composite structure. The compositing materials can comprise the aforementioned filler materials, previously formed preform or structures, e.g., honeycomb, fibrous mat, shaped particulate member, honeycomb structures, syntactic materials such as described in U.S. Pat. No. 4,568,603 hereby incorporated by reference; among others. The compositing material can be added to a foam precursor and/or introduced when foaming the precursors. In one aspect, the compositing material comprises styrene pellets, e.g., recycled packaging material, that is ground and added to the previously described carrier. These pellets function to reduce weight and cost of the resultant foam. In another aspect, the compositing material comprises a material for improving the compressive strength of the foam and/or spacers for limiting the degree to which the foam can be compressed, e.g., nylon, polyolefins, polyethylene, among other materials. The compressive strength improving materials can be of any suitable form such as cubes, beads, mixtures thereof, among other shapes.




In one aspect of the invention, one or more foam precursors interact to form an intermediate foam precursor. The intermediate foam precursor can correspond to a Part A and/or Part B. The intermediate foam precursor can be contacted with another precursor or another intermediate foam precursor in order to obtain a foam. A carrier such as a polyol, e.g., a polyester polyol, can interact with at least one member selected from the group of an acid source, e.g, phosphoric acid; a modifier, e.g., styrene; among other precursor components. An epoxy can interact with at least one member selected from the group of an acid source, e.g., phosphoric acid; a modifier, e.g., styrene; among other precursors that are miscible with the epoxy. If desired the aforementioned carrier containing intermediate product is contacted with the aforementioned epoxy containing intermediate product to obtain a foam. The intermediate precursor can be self-supporting. The combined intermediate products can produce a gel-like product that in turn is converted to a foam, e.g, the intermediate product can comprise a gel that can be shaped prior to onset of foam formation.




The precursor(s) and/or intermediate products thereof can be pre-blended and stored in separate containers prior to use. To this end, an A-side or first precursor mixture is typically obtained by combining the epoxy and modifying material, e.g, polyvinyl alcohol and polypropylene, and a B-side or second precursor mixture can be obtained by combining the carrier, e.g., a polyol, hydrogen donor/acid and thermoplastic, e.g., encapsulated blowing agent.




The precursor(s) can be produced using any suitable apparatus that imparts an amount of shear sufficient to obtain a substantially homogenous precursor. Examples of suitable apparatus comprise hand mixing, static tube mixtures, the structures described illustrated by

FIGS. 2A and 2B

(described below in greater detail), impingement spraying precursors, extrusion, e.g., a twin screw extruder, among other conventional apparatus. Normally, the samples are mixed for about 1 to about 40 seconds depending upon the composition and mixing environment, e.g., a 1:1 A:B composition can be mixed for about 1 to about 10 seconds in a static tube mixer.




The inventive method involves contacting the epoxy compound and acid or hydrogen donor under conditions effective to provide an exothermic reaction. The heat produced from the reaction can then cause the blowing agent(s) to expand in forming the desired foam. For example, where two precursors, A and B are employed, the two compositions can be combined—to obtain a foam by using conventional foam manufacturing equipment. For example, A-side and B-side can be contacted as two high pressure streams within a mixing chamber of an external mix-head. While heat can be added to the precursors, the reaction between “A” and “B” can occur at ambient conditions, e.g., to control viscosity, adjust reaction rate, etc. The ratio of A-side to B-side normally ranges from about 1:1 to about 10:1 or 1:10.




An example of a combined A and B side precursor composition is set forth in the following Table.
















TABLE









Chemical Name




Trade Name




Supplier




Wt. %




Equivalent











Cycloaliphatic




Uvacure 1500




UCB




1-80




Sartomer-






Epoxy





Radcure





SARCAT ®










K126






Caparolactone




Tone 0301




Union




0-70













Carbide






Phosphoric Acid




Phos. Acid




J. T.




1-20




commodity








Baker






Themoplastic




Expancel




Nobel




1-50




Pierce &








Industries





Stevens-










Micropearls ®














The pH of the A-side component (containing the epoxy compound(s)) is normally about 6 to at least about 8. The pH of the B side of the foam precursor comprising an acid and a carrier is normally about 0.5 to about 4, e.g., the pH of phosphoric acid when mixed with polyol. Normally, the pH prior to reaction with A-side precursors is about 1.6. The composition and concentration of the foam precursors can be modified to achieve a predetermined reaction rate e.g., by tailoring the concentration of the acid. The affects of the pH or acid concentration of the B side are better understood by reference to

FIG. 1

which illustrates the affects upon the composition demonstrated in Example 9.




Referring now to

FIG. 1

,

FIG. 1

is a graphical representation of % acid in the precursor versus foam reaction time and temperature.

FIG. 1

illustrates that as the acid concentration increases the reaction temperature increases and the reaction time decreases.

FIG. 1

also illustrates that the precursor can be selected to a predetermined reaction time/temperature. For example, by selecting a higher reaction temperature (higher acid concentration) a wider range of modifying materials can be employed whereas by selecting a slower reaction time (lower acid concentration) the foam has easier handling characteristics.




The viscosity of a foam precursor can be tailored to enhance the resultant foam characteristics. The viscosity of the “A-side” or epoxy component of the foam precursor is normally controlled, for example, so that a modifying material, e.g., a plastic powder, becomes or remains dispersed within the “A-side” precursor. While any suitable viscosity control agent can be employed desirable results can be achieved by using a solid polymer (in particulate form) to produce a foam precursor gel.




Examples of suitable solid polymers comprise at least one member selected from the group consisting of waxes, polyethylene, EVOH, PVOH, fluoropolymers and dispersions thereof such as polytetrafluoroethylene (supplied as Teflon® by the DuPont Company), among others. The viscosity control agent can range in particle size of about 20 to 50 microns, e.g,. less than 325 mesh. An example of a controlled viscosity composition comprises about 5 to about 10 wt. % solid epoxy, about 5 to about 15 wt. %, powdered polyethylene and about 25 to about 30 wt. % blowing agent. In addition to viscosity, the characteristics of the foam can be tailored by varying the temperature, pressure, foam pH, foam density, among other parameters known to those skilled in this art. Also, the “A-side” of the system can be thickened into a gel by the addition of a surfactant such as any commercially available liquid detergent or titanate such as Kenrich KRTTS, e.g., about 0.1 to about 10 wt. % surfactant. This enables a more complete Theological control, included insuring the homogeneity of the system.




As discussed above, the foam can be produced from a single-phase system, e.g., only an “A-side” mixture. An example of such a system comprises an epoxy, a polyol, thermoplastic spheres, modifying materials, phenoxy, polypropylene, mixtures thereof, among other components. This one component system can be heat activated. In other words the system expands by being exposed to elevated temperature, e.g., about 125C. If desired the single phase foam system can be initiated by employing a photo-initiator instead of, or in conjunction with, an elevated temperature. Examples of such initiators comprise at least one member selected from the group consisting of Union Carbide UVI 6974 among others. Normally, the amount of such an initiator corresponds from 0.5 to about 5 wt % of the foam precursor. More details regarding photoinitiators can be found in “Photopolymerization Behavior of Several Cationic Photoiniators in Catatonically Cured Resin Systems” by Edward Jurczak; that is hereby incorporated by reference.




Single phase systems are especially useful when applied upon a substrate by being sprayed. For example, the single phase system can be sprayed upon an automotive subassembly for reducing the amount of sound transmission to the interior of the car. In a further example, the single phase system can be sprayed upon a first component, e.g., a plastic fascia, exposed to UV to cause foaming and affixed upon a second component, e.g, metal support member, wherein the foam functions to reduce vibrations between the components.




A composite foam structure can be obtained in accordance with the instant invention. A structural modifier such as fibers, particles, rods, tubes, powders, mixtures thereof, among others, can be incorporated as a component of the foam precursor. The structural modifier can be employed for tailoring the chemical and/or physical properties of the resultant foam. Examples of suitable structural modifiers, normally as chopped fibers, ceramic or glass spheres or powders, can comprise at least one of nylon, carbon, carbonates, polymers such as polyethylene and polypropylene, graphite, Kevlar®, Dyneon, ceramic, fiberglass, mineral fillers, e.g., mica, metals, among other materials. The amount of such structural modifiers normally comprises about 1 to about 60 wt. % of the uncured foam precursor.




Any suitable commercially available foam production equipment can be employed for mixing and dispensing the inventive foam precursors to obtain the inventive foam. Examples of such equipment comprises DoPag (ECONO-MIX) supplied by Kirkco Corporation, Monroe, N.C.; as well as equipment supplied commercially by Jesco Products Company, Inc, Sterling Heights, Mich. Another example comprises using an Econo-Mix pump in combination with an Albion static mix head. The foam precursors can also be mixed by employing a power mix gun such as supplied by Sealant and Equipment Company, Oak Park, Mich. If desired, the inventive foam can be expanded within a cavity, e.g., an automotive A pillar, by employing a dispensing apparatus having a replaceable/disposable static mix head. That is, the static mix head can comprise a replaceable plastic tubing having a center piece with a helix or vortex configuration, that is connected to a pump discharge flange and inserted into the cavity for foaming the precursors.




In one aspect of the invention, the inventive foam is dispensed through a commercially available dual tube dispenser (e.g., a 4:1 dual tube dispenser supplied by Tah Industries). That is, one of dual tubes is loaded with an inventive Part A composition and the other tube contains an inventive Part B. The Part A and B are dispensed by the dual tube dispenser and pass through a static tube mixer (also known as a motionless mixer). The Part A and B are contacted by the static tube mixer thereby causing the Parts A and B to react and produce a foam. When dispensing the inventive compositions via a dual tube dispenser, the inventive compositions can be employed as replacement for conventional caulks as well as commercial cavity filling foams, e.g., polyurethane foams.




Another static mix head design has a valve type of arrangement that is illustrated in

FIGS. 2A and 2B

. Referring now to

FIG. 2A

,

FIG. 2A

illustrates a one-way value type of arrangement wherein the foam or precursors thereof are introduced or injected via a one-way valve


1


(commonly known as a zerk) that is positioned within a cap


2


. Valve


1


can also include a flap or secondary valve


1


A that prevents foam from escaping by reverse flow through valve


1


. The cap


2


seals or defines one end of a cavity being filled with foam. The cap


2


can include hooks or locking tabs


3


for securing the position of cap


2


, e.g, within the so-called A pillar of an automobile thereby permitting foam to be dispensed within the automotive cavity in a controlled manner. Normally, one end of the valve


1


is connected to a mixing zone


4


such as the aforementioned static mixers having helical vanes


5


. After traveling through the valve


1


and static mixer


4


, the foam is released into the cavity to be filled with foam. The area and direction into which the foam expands can be control and/or defined by using a containment means such as a polymeric bag


6


(the containment means is described below in greater detail).




Referring now to

FIG. 2B

, this type of arrangement provides a longer mixing time for the foam precursors before the foam is released into the cavity to be filled. The arrangement illustrated in

FIG. 2B

can also be employed as a cap


10


to seal or define one end of the cavity to be sealed. After delivering the foam precursors, a mix head


11


or previously described valves (


4


and


5


of FIG.


2


A). The foam precursors travel through mix head


11


and are released at the opening defined at


12


as foam. The opening


12


can also be within the aforementioned containment means. The caps


1


and


10


can remain associated with the foam product within the cavity. By using such a replaceable mix head, any problems associated with clogged mix heads are avoided. Two pressure streams can also be employed, to converge in a mix chamber or cavity to be foamed and mix action occurs without use of additional mixing apparatus. In addition to the foregoing, the inventive foam composition and precursors thereof can be injected, extruded, shaped, sprayed, cast, molded, among other conventional processes in order to obtain a desirable foam article. The configuration of the foam article can be virtually any shape including continuous shapes such as films or webs, discrete forms, among other shapes.




While the above description emphasizes particular foam compositions, the inventive compositions (and precursors thereof) can include additives such as dyes, fillers, surfactants, pigments, nucleating agents, among other conventional employed foam additives. If desired a pH indicator can be added to the precursor in order to provide a visual detection means for a reaction product. An example of a suitable pH indicator comprises at least one member selected from the group consisting of methyl red, methyl blue, chlorophenol red, bromothymol blue. That is, as the foam precursor react, e.g, acid-epoxy, the acid is consumed thereby changing the pH and causing the pH indicator to change color.




If desired, the inventive composition can be laminated or joined with other articles, e.g., laminated onto metal foil, Mylar, fiberboard, veneer, Formica® etc. In one aspect of the invention, the inventive foam precursors can be applied between two such laminating materials in order to form components that are useful in fabricating furniture. For example, the inventive foam is expanded between two laminating materials, one of which comprises the upper surface (e.g., a wood veneer) and the second the lower surface of a table top. Any excess foam can be removed by conventional methods such as sawing, scraping, etc. The foam imparts structural integrity to the article while reducing weight and fabrication time.




The inventive composition can also be expanded within a control or containment device or bag having a predetermined shape thereby forming a foamed article that replicates the bag, e.g, refer to U.S. Pat. Nos. 4,269,890 (Breitling), 4,232,788 (Roth), 4,390,333 (Dubois); the disclosure of each of which is hereby incorporated by reference. When expanding the foam into a bag, the previously described valves illustrated in

FIGS. 2A and B

; those supplied commercially by Inflatable Packaging as part no. IP04, or any other suitable delivery means can be employed at the opening in the bag in order to control introduction of the foam into the bag.




For example, a bag replicating a cavity such as an automotive cavity or any other desirable configuration unrolls or expands into the cavity as foam is introduced into the bag via the valve. If desired, the bag may comprise or be coated with a heat sensitive adhesive wherein the heat generated by the exothermic foam reaction activates the adhesive. The adhesive can permanently affix the foam containing bag at any desirable location. The bag can also include predetermined areas having weakened seams or perforations that are designed to rupture as the foam expands thereby directing the expanding foam. Similarly, the bag composition can be selected such that the bag melts when exposed to the foam. The melting bag can direct the expanding foam, form a coating upon the foam, and function as an adhesive, among other utilities. Further, a plurality of bags can be employed wherein one bag is surrounded by another bag. The inner and/or outer bag can possess the aforementioned predetermined properties. Furthermore, the bag can comprise areas having distinct chemical and/or physical properties, e.g., a bag comprising one sheet of polyethylene heat sealed around its periphery to a sheet comprising polybutadiene. At least a portion of the bag can be fabricated from one or members selected from the group consisting of polyethylene, polyester, vinyl, nylon, Surlyn®, ethylene vinyl acetate, styrene-isoprene-styrene, styrene-butadiene-styrene or other blocked copolymers, polybutadiene, among other plastic materials with melt points corresponding to temperature range of reaction, polyamide, modified EVA's, modified polyethylene, modified polybutadiene, GMA, SBR, among other plastic materials suitable for bag or bladder construction and seaming capability. The bag or containment means can be utilized with a wide range of foam compositions in addition to the previously described epoxy containing foams. Examples of foams that can be expanded into the previously described containment bags or means comprise at least one of epoxy amine, acrylic, and phenolic among others.




The foam precursors can be removed from surfaces, equipment, among other articles by employing non-hazardous cleaning materials. An example of suitable cleaning material comprises water, isopropyl alcohol, 2-butoxyethanol and a chelating agent. The cleaning material can be dispensed as an aerosol by using a propellant such as DME, hydrocarbons and carbon dioxide.




Moreover, the inventive foam can be fabricated to possess a substantially uniform or varying density throughout one or more of its dimensions. The ability to tailor foam density in individual articles as well as throughout an article is a marked improvement in the art. Foams having varying densities can be employed for attenuating or focusing sound, various forms of electromagnetic radiation, radar, etc.




While the above description emphasizes a reaction between an epoxy containing compound and one or more acid or hydrogen donor, the inventive method can be achieved by employing other polymer systems such as silicones, urethanes, silanes, hydroxyl or caboxyl modified elastomers; hydroxyl, carboxyl or epoxy functional compounds, reactive liquid polymers such as Hycar®, among others. That is, a polymer system is contacted with an acid that generates an exothermic reaction which in turn activates an expansion or foaming agent.




The following Examples are provided to illustrate not limit the scope of the invention as defined in the appended claims. Unless indicated otherwise, commercially available apparatus and materials were employed in these Examples.




EXAMPLE 1




A foam product was produced by mixing a 2-part system (A-side precursor and B-side precursor) through a conventional foam production apparatus comprising a static mixer that was manufactured by Albion (Model No. 535-1 or equivalent). The constituents of the foam were maintained in two separate supplies of materials, an A-side precursor and B-side precursor.




The A-side precursor comprised a blend of the epoxy and the thermoplastic microspheres including a blowing agent, in ratio of 30 parts to 15 (100 parts total). The B-side precursor comprised a blend of the phosphoric acid and the polyol in a 30 part to 50 part ratio (also 100 parts). The feed ratio of A-side precursor to B-side precursor to the mixer head was 1:1. The pH of the B-side precursors was about 1.6 prior to reaction with A-side precursor.




A pressurized flow through the mixing chamber produced a polymer which rapidly expands and released an amount of exothermic heat sufficient to produce a foam.




EXAMPLE 2




The process of Example 1 was repeated with the exception that the ratio of epoxy to thermoplastic microspheres in A-side precursor was 2:1, and the ratio of phosphoric acid to polyol in B-side precursor was 3:5. The feed ratio of A-side precursor to B-side precursor to the mixer head was 3:1.




EXAMPLE 3




The process of Example 1 was repeated with the exception that the A-side precursor and B-side precursor components were mixed together by hand (instead of using the static mixer).




EXAMPLE 4




This example demonstrates the formation of a composite foam. The process of Example 1 was repeated with the exception that about 5 wt. % polytetrafluoroethylene powder (TEFLON® supplied by the DuPont Company) was added to the A-side precursor composition. The A-side precursor and B-side precursor were contacted in the manner described in Example 1. A composite foam was recovered wherein the composite foam had greater flexibility or pliability in comparison the foam obtained by the process of Example 1.




EXAMPLE 5




A two phase system was used to produce a foam. The A-side precursor was composed of epoxy and microspheres in a 2:1 ratio (67% epoxy, 33.3% microspheres) by weight. (It is noted that for best results, the mix should be used within in 4-8 hours of mixing since certain epoxies can dissolve certain spheres). The A-side precursor was hand-stirred to a smooth consistency.




The B-side precursor was composed of Polyol (Tone 0301) and Phosphoric acid (10%) by weight). The acid was blended into the polyol. A-side precursor to B-side precursor ratio of 1:1 was contacted in a static tube mixer and produced a foam. The ratio of A to B can be from 1:1 to 4:1 depending on acid concentration.




EXAMPLE 6




A two phase system was used to produce a foam. The A-side precursor comprised an of epoxy (UCB-Radcure UVACURE 1500). The B-side precursor was comprised of a polyol (50 wt. %—Tone 0301), phosphoric acid diluted with water (approximately 50% acid in a commercially available solution) at 20%, and 30% microspheres. The spheres were hand-stirred into the polyol to a smooth consistency. The acid mixture was blended by hand-stirred into the sphere-polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was contacted in a static tube mixer and produced a foam. The ratio of A to B can be from 1:1 to 4:1 depending on acid concentration.




EXAMPLE 7




A two phase system was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure1500) While the B-side precursor comprised polyol (Tone 0301), polyvinyl alcohol and water blend (PVOH:H20 3:1 blend that corresponded to 20% of the polyol) and microspheres 30% by weight of polyol and acid can be 10% of total ‘B’ mixture. The spheres were hand-stirred into the polyol to a smooth consistency. The PVOH and water are hand-stirred. The PVOH/water solution temperature was 140° F. The PVOH blend was added to the polyol by hand stirring. The acid was hand-stirred into the sphere-PVOH-polyol mix. The A-side precursor to B-side precursor ratio of 1:1 was contacted in a static tube mixer and produced a foam. The ratio of A to B can be from 1:1 to 4:1 depending upon acid concentration.




EXAMPLE 8




A two phase system was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure 1500) and a phenoxy resin (Paphen PKHP-200 that corresponded to 25% of A-side precursors, epoxy is 75% of A-side precursors). The B-side precursor comprised 45% polyol (Tone 0301), 23.5% polyvinyl alcohol (Airvol 203S) and 23.5% microspheres. Phosphoric acid was 10% by wt. of the B-side precursor. Spheres are hand-stirred into the polyol to a smooth consistency. The PVOH, microspheres, and polyol are blended by hand stirring. The phosphoric acid was hand-stirred into the sphere-PVOH-polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was used contacted in a static tube mixer to produce a foam. The A to B ratio can range from 1:1 to 4:1 depending on acid concentration.




EXAMPLE 9A




A two phase system, namely an A-side precursor and a B-side precursor, was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure 1500) 60 wt %, polypropylene powder (Equistar FP 800-00) 20 wt %, polyvinyl alcohol (Airvol 203S) 20 wt %. The B-side precursor comprised polyol (Tone 0301) 60 wt % and microspheres 30%. Phosphoric acid was 10%. Spheres are hand-stirred into the polyol until a smooth consistency was obtained. The microspheres and polyol are blended by hand stirring. The phosphoric acid was hand-stirred into the microspheres and polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was used and contacted in a static tube mixer to produce a foam. The A to B ratio can, however, range from 1:1 to 4:1 depending on acid concentration.




EXAMPLE 9B




This Example employed a two phase system wherein the A-side precursor comprised a gel. A two phase system, namely an A-side precursor and B-side precursor, was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure 1500) 59 wt %, polypropylene powder (Equistar FP 800-00) 20 wt %, polyvinyl alcohol (Airvol 203S) 20 wt % and surfactant (gelling agent) at 1 wt %. The B-side precursor comprised polyol (Tone 0301) 60 wt % and microspheres 30%. Phosphoric acid was 10%. Spheres are hand-stirred into the polyol until a smooth consistency was obtained. The microspheres and polyol are blended by hand stirring. The phosphoric acid was hand-stirred into the microspheres and polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was used and contacted in a static tube mixer to produce a foam. The A to B ratio can, however, range from 1:1 to 4:1 depending on acid concentration.




EXAMPLE 10




A bag or containment device approximately 8×8 inches in size and having a one-way valve located on one end of the bag was constructed from two sheets of high density polyethylene film. The seams of the bag were designed to rupture at specific locations, which directs foam expansion into cavity area adjacent to weak seams. The sheets were joined by heating on a TEW Electric Heating Company Ltd sealing apparatus. The seams were selectively reinforced by double sealing or weakened to provide multiple points for foam direction from the same bag. The foam composition demonstrated by Example 9 was introduced into this bag. As the foam expanded, the foam escaped from the bag through the relatively weak seams.




EXAMPLE 11




A bag or bladder composed of each of polyethylene, ethylene vinyl acetate, polybutadiene were fabricated by using the apparatus described in Example 10. The foam of Example 9 was introduced into these bags. The bags, having a melting point less than the exothermic reaction temperature of the foam, failed and released the foam.




EXAMPLE 12




A bag or bladder composed of each of modified EVA (Bynel®), modified polyethylene (Primacor® supplied by Dow Chemical Company), modified butadiene, glycidal methacrylate (GMA) were fabricated by using the apparatus of Example 10. The foam of Example 9 was introduced into these bags. The heat released from the exothermic reaction of the foam caused the bags to melt. The melting bag material adhered to the foam thereby modifying the surface of the foam. The melting bag also adhered the foam to any surrounding surfaces or articles.




EXAMPLE 13




A bag or bladder composed of each of polypropylene, polyethylene, woven nylon mesh, aluminized fiberglass mesh was fabricated by using the apparatus of Example 10. Each of the bags was further processed to possess multiple perforations (25-100 holes/in.). The foam of Example 9 was introduced into each of these bags. The perforations allowed the foam to escape in controlled quantities while also generally retaining the shape of the bag.




EXAMPLE 14




Two bags or bladders, namely an inner and outer bag were fabricated by using the apparatus of Example 10. The inner bag comprised modified butadiene and the outer bag comprised high density polyethylene. The inner bag was placed within the outer bag and the outer bag was sealed. The foam of Example 9 was introduced into the inner bag. Inner bag or bladder melted during the foam reaction. The inner bag was of sufficient size to contain the required amount of mixed foam precursors to fill the out bag. Outer bag construction was of material and size to contain reaction within the cavity.




EXAMPLE 15




The insertion loss or sound dampening characteristics of the foam produced in accordance with Example 9A was tested in accordance with Society of Automotive Engineers (SAE) J 1400. The sample size was 3×3×10 inches and placed within an E-coated metal channel. An increase in insertion loss corresponds to an increase in sound dampening properties that in turn corresponds to less noise within the passenger compartment of an automobile.



















FREQ. (Hz)




INSERTION LOSS (dB)













 125




12.5







 160




10.6







 200




11.4







 250




12.0







 315




24.5







 400




35.4







 500




46.8







 630




38.4







 800




40.1







1000




45.7







1250




45.1







1600




49.6







2000




49.2







2500




50.1







3150




50.9







4000




55.5







5000




58.7







6300




59.2







8000




64.2















These data illustrate the desirable sound absorbing characteristics of the inventive foam compositions.




EXAMPLE 16




The viscosity of the Part A foam precursor fabricated in accordance with Example 9A was tested in accordance with conventional methods and apparatus (Brookfield Viscometer, Spindle 27, Thermal-Cell). The viscosity as a function of temperature is listed below.





















RPM




Temp 75 F.




Temp 110 F.




Temp 150 F.





























0.5




13,000 




8,000




3,000







1




10,500 




5,500




2,500







2.5




8,160




3,400




1,600







5




6,680




2,300




1,100







10




5,700




1,800




  800







20




4,830




1,480




  600







50




3,900




1,250




  468







100




3,280




1,100




  404















The viscosity of the Part B foam precursor fabricated in accordance with Example 9A was tested in accordance with conventional methods and apparatus (Brookfield Viscometer, Spindle 27, Thermal-Cell). The viscosity as a function of temperature is listed below.





















RPM




Temp 75 F.




Temp 110 F.




Temp 150 F.





























0.5




22,000




13,000 




4,000







1




20,000




10,000 




2,500







2.5




18,600




7,000




1,600







5




17,800




5,320




1,300







10




17,300




4,500




1,100







20





4,000




  975







50





3,700




  880







100





3,580




  860















EXAMPLE 17




This Example illustrates foam formation as a result of being activated by exposure to an energy source, e.g, UV light. A radiation curable foam having the following components was prepared:


















COMPONENT




TRADE NAME




SUPPLIER




AMOUNT



























Cycloaliphatic epoxy




UVACURE 1500




Radcure




50




wt. %






Caprolactone polyol




Tone 0301




Union Carbide




40






Blowing agent




Expancel DU551




Expancel Inc.




9






Sulfonium salt




UVI-6974




Union Carbide




1














The above components were combined as follows. The Uvacure and polyol were added together in a mixing vessel and mixed until the solution was clear. The UVI 6974 was added to the mixture, and mixed until substantially completely dispersed (about 2 minutes). The Expancels spheres were added to the mixture and mixed until substantially lump free. For best results, the minimum amount of mixing time, and shear were employed.




The foam precursors were placed onto a conveyor and exposed to a source of UV light. The method for exposing the precursors to UV light is described in the previously identified U.S. patent application Ser. No. 09/197,107, filed Nov. 20, 1999, both filed in the name of Jeffrey Pachl et al., and entitled “Curable Sealant Composition”.




This UV activated foam was modified by adding an acrylic monomer or acrylated oligomer. This modified LTV activated foam was prepared as described above and comprised:


















COMPONENT




TRADE NAME




SUPPLIER




AMOUNT



























Acrylated




IRR 84




UCB RADCURE




93.5




wt. %






oligomer






Acid






functional






Oligomer




Ebecryl 170




UCB RADCURE




0.9






Photo-




Darocure 1173




Ciba-Giegy




0.9






initiator






Blowing




F30D-Micropearls




Pierce & Stevens




4.7






Agent














The resultant foam possessed a pressure sensitive adhesive characteristic. The tacky pressure sensitive characteristic was removed by adding an acrylate compound. A tack-free formulation comprised:


















COMPONENT




TRADE NAME




SUPPLIER




AMOUNT



























Acrylated




IRR 84




UCB RADCURE




92.6




wt. %






oligomer






Acid






functional






Oligomer




Ebecure 170




UCB RADCURE




0.9






Photo-




Darocure 1173




Ciba-Giegy




0.9






initiator






Blowing




F30D-Micropearls




Pierce & Stevens




4.7






Agent






Acrylate




Sartomer 444




Sartomer




0.9














The later two formulations were also activated by being exposed to natural light.




EXAMPLES 18-22 AND 25




The following Table lists the Components, Trade Names and Suppliers for the foam precursors that were employed in Examples 18 through 22 and 25. The foam in Examples 18-22 was prepared by contacting the Part A with the Part B listed in the tables below in a 2.75″ diameter by 1.92″ height ointment can and mixed by hand. Reaction Time and Temperature were determined in accordance with conventional methods. The percent vertical expansion as well as the shrinkage was determined visually. The Shore A test was conducted using a Type A-2 Shore Durometer Hardness test unit that meets ASTM D2240 requirements. The Shore A test was conducted about 4 hours after foam formation. The instantaneous peak reading was recorded.

















Trade Name




Component




Supplier


























Epon 862





Bis F/Epichlorohydrin Epoxy Resin




.Shell Chemical Co.






Expancel 091DU80




(244F)




Blowing Agent (thermal)




Expancel, Inc






Expancel 051DU




(223F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 2-








propenenitrile and isobutane is the blowing








agent






Expancel 054WU




(257F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 2-








propenenitrile and isopentane is the blowing








agent






Expancel 461DU




(208F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 1,1-








dichloroethene and 2-propenenitrile and








isobutane is the blowing agent






Expancel 551WU




(199F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 1,1-








dichloroethene and 2-propenenitrile and








isobutane is the blowing agent






Expancel 551WU80





Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 1,1-








dichloroethene and 2-propenenitrile and








isobutane is the blowing agent






Expancel 642WU




(183F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 1,1-








dichloroethene and 2-propenenitrile and








isobutane is the blowing agent






Expancel 820DU




(167F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.








propenoic acid methyl ester polymer with 1,1-








dichloroethene and 2-propenenitrile and








isobutane is the blowing agent






Expancel 820WU




(167F)




Blowing Agent (thermal): 2-methyl 2-




Expancel, Inc.














propenoic acid methyl ester polymer with 1,1-








dichloroethene and 2-propenenitrile and







isobutane is the blowing agent






Heloxy 505




Epichlorohydrin Castor Oil Based Epoxy




Shell Chemical Co.







Resin (aliphatic triglyceride triglycidyl ether)






SR 239




1,6 Hexanediol Dimethacrylate




Sartomer






SR 495




Caprolactone Acrylate




Sartomer






Vertrel XF




Blowing Agent: 2,3-Dihydroperfluoropentane




DuPont







(Pentane,1,1,1,2,3,4,4,5,5,5-decafluoro:







CF3CHFCHFCF2CF3)






Micropearls F30D




Blowing Agent (thermal): isobutane




HM Royal (Pierce &







encapsulated in polymer vinylidene chloride




Stevens)






Ebecryl 170




Adhesion Promoter: Acrylate modified acidic




UCB Radcure







adhesion promoting agent






Amicure CG1400




Dicyandiamide




Air Products






Glycolic Acid (70% Tech)




Technical grade (70%)




DuPont






H


3


PO


4


(>95% conc.)




concentrated grade via distillation of the 75%




DeNOVUS







technical grade from Harcros Chemical






HQ54




merchant grade (73%)




PCS






Amberphos-54 (AMMGA)




merchant grade (75%)




PCS






H


3


PO


4


(85% Reagent)




reagent grade (85%)




Fischer Scientific






H


3


PO


4


(75% technical)




technical grade (75%)




Harcros Chemicals






H


3


PO


4


(85% technical)




technical grade (85%)




FMC/Harcros








Chemicals






BTL 71001




Elastomer: EVA powder




BTLSR Toledo






MU 760-00




Elastomer: EVA powder: MI = 23: MP = 187 F:




Equistar







VA = 19: Particle Size = 35 mesh






Microthene FA 700-00




Elastomer: HDPE powder: MI = 10.5:




Millennium







MP = 273 F: Particle Size = 20 microns






Microthene FN 514-00




Elastomer: LDPE powder: MI = 70: MP = 216 F:




Millennium







Particle Size = 20 microns






Microthene FP 800-00




Elastomer: Polypropylene powder: MP = 325 F:




Equistar







Particle Size = 20 microns






LIR 403




Elastomer: Rubber: (polyisoprene liquid




Kuraray Co







rubber)






Kraton D1107




Elastomer: SIS rubber pellets




Shell Chemical Co






Q325




Calcium carbonate




JM Huber Corp






Quikrete




Concrete mix




Quikrete Co.






Dicaperl CS-10-200




Hollow ceramic spheres




Grefco Inc






Qcel 650-D




Inorganic microspheres




PQ Corporation






SynPro Li Stearate




Li stearate




Ferro






A-C 6702




Oxidized polyethylene




Allied Signal






Airvol 203S




Polyvinyl Alcohol (PVOH)




Air Products






G




Sodium silicate




PQ Corporation






BTL 74001




Versatic acid ester/polyvinyl acetate ester




BTLSR Toledo






AZO 77




Zinc oxide




Morton Meyer






Isopropyl Alcohol (70%)




Alcohol




Commercial






Ethanol




Alcohol: Pure Grain Alcohol




Commercial






Ircosperse 2174




Dispersant




Lubrizol






Carbopol EZ-1




Emulsion Thickener




BF Goodrich






#1 Castor Oil




Oil




Acme-Hardesty






Lucant HC-2000




Oil: Hydrocarbon based synthetic oil




Mitsui Chemical






Vasoline




Petroleum Jelly




Chesebrough-








Ponds






Indopol L100




Polybutene




Amoco






Unifilm 100HSM




Rheology Control Agent




Troy Chemical






Z6040




Silane




Dow Corning






Z6124




Silane: Arylalkoxy silane




Dow Corning






Dish Soap




Soap




Commercial






Boraxo




Soap: Sedium tetraborax decahydrate




Dial Corp






Triton X45




Surfactant




Union Carbide






Texaphor Special




Surfactant: Anionic Surfactant




Henkel






KRTTS




Titanate




Kenrich






Santolink XI-100




Allyl glycidyl ether alcohol resin




Solutia/Monsanto






SB 400




Aromatic acid methacrylate-mixed half ester




Sartomer






Pliolite AC




Copolymer: (styrene-acrylate: powder)




Goodyear






Pliolite S-5A




Copolymer: (styrene-butadiene: powder)




Goodyear






CMD 50859




Epoxy:




Shell Chemical Co






CMD 8750




Epoxy:




Shell Chemical Co






PEP 6180




Epoxy: (epoxy toughener: hydrogenated Bis




Pacific Epoxy







A:)






PEP 6210 PA




Epoxy: (epoxy toughener: polyether adduct,




Pacific Epoxy







epoxy functionality: EEW = 210: visc = 500 cps)






Erisys GE-60




Epoxy: (sorbitol glycidyl ether - aliphatic




CVC Specialty







polyfunctional epoxy): liquid: EEW = 170:




Chemicals







visc = 13,000 cps






Epalloy 5000




Epoxy: Bis A: (epoxidized hydrogenated Bis




CVC Specialty







A resin): EEW = 220: visc = 1900 cps




Chemicals






DER 317




Epoxy: Bis A: liquid




Dow Chemical






DER 331




Epoxy: Bis A: liquid




Dow Chemical






DER 736




Epoxy: Bis A: liquid




Dow Chemical






Epon 828




Epoxy: Bis A: liquid




Shell






Uvacure 1500




Epoxy: cycloaliphatic




UCB Radcure






Uvacure 1502




Epoxy: cycloaliphatic




UCB Radcure






Uvacure 1533




Epoxy: cycloaliphatic




UCB Radcure






Cryacure UVR 6128




Epoxy: cycloaliphatic




Union Carbide






K126




Epoxy: cycloaliphatic: (cycloaliphatic




Sartomer







diepoxide)






Eponex 1510




Epoxy: cycloaliphatic: (cycloaliphatic glycidyl




Shell Chemical Co







ether): (hydrogenated DGEBPA)






Erisys GE-22




Epoxy: cycloaliphatic: (difunctional




CVC Specialty







cycloaliphatic): (cyclohexanedimethanol




Chemicals







diglycidyl ether): EEW = 155: visc = 60 cps






Uvacure 1534




Epoxy: cycloaliphatic: cycloaliphatic epoxy-




UCB Radcure







polyol blend






Erisys GE-35




Epoxy: Glycidyl ether of castor oil




CVC Specialty








Chemicals






Epon SU2.5




Epoxy: Novolac




Shell






Epalloy 8240




Epoxy: Novolac: (epoxidized phenol novolac:




CVC Specialty







liquid): EEW = 170: visc = 6550 cps: fnc = 2.35




Chemicals






Epon 58005




Epoxy: rubber modified: (40% CTBN)




BF Goodrich






Erisys EMRM-22




Epoxy: rubber modified: (CTBN modified




CVC Specialty







epoxy)




Chemicals






Tone EC




Monomer: Lactone: 2-oxepanone (6-




Union Carbide







hydroxyhexanoic acid-e-lactone)






Santicizer 261




Plasticizer: Alkyl Benzyl Phthalate




Solutia






Santicizer 278




Plasticizer: Alkyl Benzyl Phthalate




Solutia






Santicizer 160




Plasticizer: Butyl Benzyl Phthalate




Solutia






Santicizer 97




Plasticizer: Dialkyl Adipate




Solutia






Santicizer 141




Plasticizer: Flame Retardant: 2-ethyl




Solutia







Diphenyl Phosphate






CAPA 316




Polyol




Solvay Interox Ltd






Tone 0201




Polyol: (caprolactone-based polyol: diol):




Union Carbide







Hydroxyl # = 212:






Tone 0301




Polyol: (caprolactone-based polyol: triol):




Union Carbide







Hydroxyl # = 560: visc-225 @ 55 C






Arcol E-351




Polyol: (polyether polyol: capped diol):




Arco Chemical Co







Hydroxyl # = 40: visc = 507 Cp






Arcol DP-1022




Polyol: (polyether polyol: diol): Hydroxyl




Arco Chemical Co







# = 1200: visc = 175 cP






PPG-425




Polyol: (polyether polyol: diol): Hydroxyl




Arco Chemical Co







# = 263: visc = 71 cps






Acclaim Polyol 4220




Polyol: (polyether polyol: monol diol):




Arco Chemical Co






Acclaim Polyol 6300




Polyol: (polyether polyol: monol triol):




Arco Chemical Co







Hydroxyl # = 28: visc = 1452 cP: fnc = 2.94: acid







value = 0.01






Arcol LG-650




Polyol: (polyether polyol: triol): Hydroxyl




Arco Chemical Co







# = 650: visc = 1059 cP






Ebecryl 81




Polyol: Modified polyester polyol




Radcure






K-Flex 188




Polyol: Polyester Polyol:




King Industries






Desmophen L-951




Polyol: Short chained polyol: Hydroxyl # = 265




Bayer






Hycar 1300x40




Rubber




BF Goodrich






Hycar 1300X13




Rubber: (CTBN acrylonitrile liquid rubber)




BF Goodrich






Nipol 1312




Rubber: (liquid nitrile rubber)




Zeon Chemical






CN 301




Rubber: (methacrylated polybutadiene)




Sartomer






R45HT




Rubber: (PBD hydroxyl terminated)




Elf Atochem






Actipol E-16




Rubber: Activated polybutene: (Epoxidized




Amoco







polybutene): Liquid






Trilene M-101




Rubber: Epoxidized EPDM




Uniroyal






PBD 605




Rubber: Hydroxyl terminated PBD




Elf Atochem






Kraton L-2203




Rubber: Hydroxyl terminated poly




Shell Chemical Co







(ethylene/butylene) polymer: Diol






Ricon 100




Rubber: Styrene PBD: Liquid




Ricon Resins






Ricon 184




Rubber: Styrene PBD: Liquid




Ricon Resins






SAT 010




Silyl




Kaneka






SAT 030




Silyl




Kaneka






SAT 200




Silyl




Kaneka






Vertrel XF




2,3-Dyhydroperfluoropentane (Pentane,




DuPont







1,1,1,2,3,4,4,5,5,5-decafluoro:







CF3CHFCJFCF2CF3)






Micropearls F30D




Thermal Blowing Agent: isobutane




HM Royal (Pierce &







encapsulated in polymer vinylidene chloride




Stevens)














The following terms and definitions are referenced in Examples 18-22.




Tin Ointment Can: Dimensions 2.75″ d×1.92″ h




Initial Rxn Time: Time that initial expansion is observed (includes mix time, does not include time to pour part A into part B




Final Rxn Time: Time for reaction to go to completion (includes “Initial Rxn Time”)




Rxn Temp: The peak temperature observed during the reaction




% Ht Expansion: % HE=[(h


f


−h


i


)/h


i


]×100




Density: Weight of 1 in


3


block of expanded material (g/in


3


)




H


2


O Absorption 1: 100×(W


3


−W


2


)/(W


2


−W


C


): W


C


=weight of aluminum coupon only W


2


=weight of coupon+material before submerging in water W


3


=weight of coupon+material after submerging in water: Mix material, apply to a 3″×3″ aluminum coupon, allow to cool to room temperature, submerge in water for 24 hrs, wipe off excess and immediately calculate water absorption.




H


2


O Absorption 2: Take a 1.5 inner diameter×h Polyvinyl chloride (PVC) pipe: use Daubert #2-76GSM paper as the release liner inside the PVC pipe (use some means to cap the bottom so that material does not exude out): mix part A & B and pour into the pipe and allow to expand and cure: cool to room temperature: cut 1.5″ lengths so that the sample size is ≈1.5″d×1.5″h: sand the edges: submerge in water for 24 hrs: remove the sample, wipe off excess water and immediately calculate % water absorption. % Water Absorption=100×(W


F


−W


1


)/W


1






H


2


O Absorption 3: “Open Chunk”: Mix part A & B in a polystyrene plastic cup: allow to expand and cure: cool to room temperature: Cut a “chunk” of foam from the top surface: submerge in water for 24 hrs: remove the sample, wipe off excess water and immediately calculate % water absorption: % Water Absorption=100×(W


F


W


1


)/W


1






Hardness: Shore A: The foam surface may be irregular: Take highest instantaneous reading from top surface after conditioning at room temperature for 4 hrs minimum




Shrinkage: Rating: 0=none 1=<1 mm from edge 2=1-2 mm from edge 3=2-3 mm from edge 4=3-4 mm from edge 5=4-5 mm from edge 6=5-6 mm from edge (shrinkage is usually not symmetrical: take the largest gap and divide by 2 if it did not shrink equally from the outer perimeter. Other values listed will be visually results: Rating 1=very slight, Rating 2=noticeable, Rating 3 & 4=significant, Rating 5 & 6=very significant




EXAMPLE18


















Components




SAMPLE NO




















Wt. %




1




2




3




4




5




6




7




8




9









Part A






Uvacure 1500




30




30




30




30




30




30




20




30




30






Microthene




10




10




10




10





10




10




10






FP800-00






Airvol 203 S




10




10




10




10




10




10




10




10




10






(PVOH)






Dicaperl CS-








10






10-200






Hycar 1300x13









10






PEP 6180










10




5






Part B






Tone 0301




29.65




29.65




29.65




29.65




29.65




29.65




29.65




29.65




29.65






(Polyol)






Micropearls




14.85




10




12




16




14.85




14.85




14.85




14.85




14.85






F30D






H


3


PO


4






5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5






(Reagent: 85%)






Rxn Time




59 sec




57 sec




56




57 sec




53 sec




65 sec




64 sec




58 sec




61 sec






Rxn Temp




288 F.




291 F.




289 F.




265 F.




292 F.




265 F.




238 F.




289 F.




270 F.






% Vertical




487%




413%




434%




468%




482%




385%




205%




404%




528%






Expansion






Hardness -




20




19




20




21




17




22




23




26




18






Shore A






Shrinkage




None




None




None




None




Very Slight




Noticeable




Noticeable




Very Slight




Very Slight















Components




SAMPLE NO




















Wt. %




10




11




12




13




14




15




16




17




18









Part A






Uvacure 1500




30




30




20




30




30




30




30




30




15






Microthene






10




10








10






FP800-00






Airvol 203 S




20




10




10




10




10




10




10




10




10






(PVOH)






Microthene





10






10






FN514-00






DER 317






10






Microthene








10






FA700-00






Equistar MU









10






76000






AC 6702










10






BTL 71001











10






Cryacure UVR












15






6128






Part B






Tone 0301




29.65




29.65




29.65




20




29.65




29.65




29.65




29.65




29.65






(Polyol)






Micropearls




14.85




14.85




14.85




14.85




14.85




14.85




14.85




14.85




14.85






F30D






H


3


PO


4






5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5






(Reagent: 85%)






CN 301







9.65






Rxn Time




55 sec




50 sec




56




40 sec




51 sec




55 sec




50 sec




49 sec




56 sec






Rxn Temp




276 F.




274 F.




242 F.




268 F.




277 F.




271 F.




280 F.




292 F.




259 F.






% Vertical




494%




396%




226%




361%




388%




406%




415%




519%




326%






Expansion






Hardness -




16




23




22




42




22




19





19




15






Shore A






Shrinkage




None




Very Slight




Very Slight




Very Slight




Very Slight




Very Slight




Very Slight




None




Very Slight















Components




SAMPLE NO




















Wt. %




19




20




21




22




23




24




25




26




27









Part A






Uvacure 1500




30




30




30




30




30




30




20




30




30






Microthene




10




10




10




10




10




10




10




10






FP800-00






Airvol 203 S




10





10




10




10




10




10




10




10






(PVOH)






Quickrete





20






Concrete Mix






DER 331








10






Epalloy 8240










10






Q325












10






Part B






Tone 0301




29.65




29.65




29.65




29.65




29.65





29.65




29.65




29.65






(Polyol)






Micropearls





14.85






14.85




14.85




14.85





14.85






F30D






H


3


PO


4






8




5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5






(Reagent: 85%)






Acclaim 6300









29.65






Expancel




14.85






091DU80






Expancel






14.85




14.85






642WU






Expancel











7.5






051DU






Rxn Time





52 sec




55 sec




52 sec




54 sec




46 sec




55 sec




72 sec




50 sec






Rxn Temp




298 F.




282 F.




289 F.




285 F.




270 F.





278 F.




323 F.




274 F.






% Vertical




183%




282%




460%




450%




378%




206%




388%




219%




570%






Expansion






Hardness -




75




18




10




12




43




23




39




53




21






Shore A






Shrinkage




None




Very Slight




Very Slight




None




Noticeable




None




Noticeable




Very Slight




Noticeable















Components




SAMPLE NO




















Wt. %




28




29




30




31




32




33




34




35




36









Part A






Uvacure 1500





30




30




30




30




30




30




30




30






Microthene




10




10




10




10






10




10




10






FP800-00






Airvol 203 S




10




10




10




10




10




10




10




10




10






(PVOH)






Sartomer K126




30






Epon 58005






10






DER 736







10






Sodium








10






Silicate






Q Cel 650-D









10






Texaphor










4






Special






Blue Dish











2






Wish Soap






Part B






Tone 0301




29.65




29.65




29.65




29.65




29.65




29.65




29.65




29.65






(Polyol)






Micropearls




14.85





14.85




14.85




14.85




14.85




14.85




14.85




14.85






F30D






H


3


PO


4






5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5




5.5






(Reagent: 85%)






Expancel





14.85






820DU






E-351 Polyol












29.65






Rxn Time




50 sec




50 sec




54 sec




61 sec




58 sec




49 sec




68 sec




71 sec




40 sec






Rxn Temp




285 F.




296 F.




273%




271 F.





294 F.





281 F.




295 F.






% Vertical




483%




410%




396%




374%




410%




445%




530%




502%




302%






Expansion






Hardness -




20




32




34




30




10




18




13




23




38






Shore A






Shrinkage




None




Noticeable




Noticeable




Significant




Significant




None




Very Slight




None




None















Components




SAMPLE NO




















Wt. %




37




38




39




40




41




42




43




44




45









Part A






Uvacure 1500




30




30




30




30




30





30




30




25






Microthene




10




10




10




10




10




10




10




10




10






FP800-00






Airvol 203 S




10




10




10





10




10




10




10




10






(PVOH)






Shell CMD






5






50809






Z6124







2






Uvacure 1502









30






Expancel











14.85






461DU






Epon 1510












5






Part B






Tone 0301






29.65




29.65




29.65




29.65




14.65




29.65




29.65






(Polyol)






Micropearls




14.85




14.85




14.85




14.85




14.85




14.85




14.85





14.85






F30D






H


3


PO


4






5.5




5.5




5.5




5.5




5.5




5.5






(Reagent: 85%)






Sartomer SB




29.65






400






LIR 403





14.65






Santolink XI-





15








15






100






75% Isopropyl








9.65






Alcohol






Amberphos-54










6.5




6.5




6.5






Rxn Time




37 sec




32 sec




55 sec






67 sec




45 sec




51 sec




82 sec






Rxn Temp




292 F.





305 F.






282 F.





291 F.






% Vertical




345%




188%




462%




561%




638%




450%




440%




340%




334%






Expansion






Hardness -




39




45




32




15




3




25




43




35




43






Shore A






Shrinkage




Noticeable




None




Very Slight




None




Very Slight




None




Very Slight




None




Noticeable

















Components




SAMPLE NO

















Wt. %




46




47




48




49











Part A







Uvacure 1500




30




30




30




30







Microthene FP800-00




10




10







Airvol 203 S (PVOH)




10




10







Erisys GE-60





10







SAT 200 (silyl)






20







Kraton D1107







5







Part B







Tone 0301 (Polyol)




20







Micropearls F30D




14.85




14.85




14.85




14.85







Amberphos-54




6.5







#1 Castor Oil




9.65







Arcol LG-650





29.65







HQ54 (73% H


3


PO


4


)





6.5




6.5







Arcol DP-1022






29.65




29.65







H


3


PO


4


(75% technical grade)







6.5







Rxn Time




47 sec




110 sec




101 sec




83 sec







Rxn Temp




287 F.





289 F.







% Vertical Expansion




364%




350%




458%




620%







Hardness - Shore A




32




25




9




7







Shrinkage




Very Slight




Very slight




Noticeable




Significant















EXAMPLE 19



















Components wt. %




Sample No. 1




Sample No. 2




Sample No. 3




Sample No. 4



























Part A










Uvacure 1500




30




30




30




30






Microthene FP800-00




10




10




10




10






Airvol 203 S (PVOH)




10




10




10




10






Part B






Tone 0301 (Polyol)






Micropearls F30D




14.85




14.85




14.85




14.85






Amberphos-54 (AMMGA)




6.5




6.5




6.5




6.5






Tone 0201




14.65




20




9.65






Santolink XI-100




15




9.65




20






Arcol DP-1022







29.65






Initial Rxn Time




27 sec




24 sec









63 sec






Initial Rxn Temp




204 F.














201 F.






Rxn Time




42 sec




35 sec









99 sec






Rxn Temp


























% Vertical Expansion




293%




277%




249%




550%






Hardness - Shore A




55




59




53




4






Shrinkage




Significant




Significant




Noticeable shrinkage




Noticeable







(>2 mm < 4 mm from




(>2 mm < 4 mm from




(>1 mm < 2 mm from




shrinkage







edge of tin cup) after




edge of tin cup) after




edge of tin cup) after




(>1 mm < 2 mm







cooling to RT




cooling to RT




cooling to RT




from edge of tin










cup) after cooling










to RT














EXAMPLE 20























Component wt %




Sample No. 1




Sample No. 2




Sample No. 3




Sample No. 4




Sample No. 5




Sample No. 6









Part A






Uvacure 1500




30




30




30




30




40




34.46






Nipol 1312






15




15






Lucant HC-2000




15






Carbopol EZ-1





5






Microthene FP800-00





10






Microthene FN-514-00








20




12.75






Kraton D1107









3.79






Part B






Arcol PPG-425




20





15




10




20






Micropearls F30D




14.85





14.85




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5





6.5




6.5




6.5




6.5






Jeff P. Control Part B





50






Arcol DP-1022






5




10






Tone 0301









14.65






Santolink XI-100









15






Initial Rxn Time




40 sec




34 sec




51 sec




50 sec




51 sec




29 sec 31 sec






Final Rxn Time




50 sec




52 sec




65 sec




65 sec




73 sec




70 sec 65 sec






% Ht Expansion




390%




423%




387%




310%




292%




374%






Water Absorption




81% 75%




31% 33%




73% 98%




46% 58%




19% 28%




18% (matl chunk)






Shore A Hardness




27




28




32




33




62




38






Shrinkage




0




0




≈5.5 mm




≈7 mm




2 mm




2 mm









Component wt %




Sample No. 7




Sample No. 8




Sample No. 9




Sample No. 10




Sample No. 11




Sample No. 12









Part A






Uvacure 1500




30.4




34.46




34.46




50.7




50.7




27.9






Kraton D1107




3.34




3.79




3.79




5.6




5.6




3.1






Microthene FN514-00




11.26




12.75




12.75




18.8




18.8




10.3






Part B






Tone 0301




14.65






Santolink XI-100




15






Micropearls F30D




14.85




14.85




11.6




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5




6.5




5.1




6.5




12.5




6.5






Arcol PPG-425









20






Arcol DP-1022





29.65




23.3




29.65




29.65






Initial Rxn Time





83 sec




96 sec




101 sec




28 sec




41 sec






Final Rxn Time





107 sec




132 sec




136 sec




42 sec




58 sec






% Ht Expansion




432%




398%




368%




252%




313%




402%






Density (g/in


3


)






Water Absorption






Shore A Hardness




36




13




18




28




24




46






Shrinkage




1 mm




1 mm




3 mm




5 mm




1 mm




0.5 mm









Component wt %




Sample No. 13




Sample No. 14




Sample No. 15




Sample No. 16




Sample No. 17




Sample No. 18









Part A






Uvacure 1500




40.5




40.5




40.5




46.29




46.29




40






Microthene FN-514-00




4.5




4.5




4.5




8.57




8.57






Kraton D1107




15




15




15




5.14




5.14






Nipol 1312









15






Part B






Arcol PPG-425




20




20




20




20




20




20






Micropearls F30D




14.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




6.5




8.5




8.5




8.5




8.5




8.5






Glycolic Acid (70% tech)






6





6






Initial Rxn Time




46 sec




34 sec




33 sec




27 sec




27 sec




32 sec






Final Rxn Time




58 sec




48 sec




49 sec




40 sec




39 sec




46 sec






% Ht Expansion




317%




377%




480%




405%




395%




508%






Density (g/in


3


)






1.99






Water Absorption





115% 142%




116% 174%




59% 131%




443% 409%




131% 160%






Shore A Hardness




63




42




13




29




13




25






Shrinkage




4 mm




0.5 mm




0.5 mm




1.5 mm




1 mm




1 mm









Component wt %




Sample No. 19




Sample No. 20




Sample No. 21




Sample No. 22




Sample No. 23




Sample No. 24









Part A






Uvacure 1500




40




40




40




40




40




35






Microthene FN-514-00






Kraton D1107






Nipol 1312




15




15




15




15




15




15






Carbopol EZ-1





5




5






Epon CMD 50859









5






Part B






Arcol PPG-425




20




20




20




20




20




20






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




8.5






Glycolic Acid (70% tech)




6





3






#1 Castor Oil







8






Z6040








1






Initial Rxn Time




30 sec




30 sec




25 sec




33 sec




36 sec




37 sec






Final Rxn Time




42 sec




41 sec




39 sec




59 sec




57 sec




52 sec






% Ht Expansion




382%




402%




417%




421%




455%




432%






Density (g/in


3


)






Water Absorption





144% 133%




152% 162%




66% 55%




105% 108%




99% 129%












(open chunk:












137%)






Shore A Hardness




18




24




17




23




29




23






Shrinkage




3 mm




0 mm




1.5 mm




0 mm




0.5 mm




0 mm









Component wt %




Sample No. 25




Sample No. 26




Sample No. 27




Sample No. 28




Sample No. 29




Sample No. 30









Part A






Uvacure 1500




40




40




40




40




40




40






Microthene FN-514-00






Kraton D1107






Nipol 1312




15






SAT 030





15




15




15




15






CN 301









15






Part B






Arcol PPG-425





20




20




20




20




20






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




8.5






Arcol Acclaim 6300




20






#1 Castor Oil






8




15





8






Tone EC Monomer








10






Initial Rxn Time




36 sec




38 sec




50 sec




61 sec




54 sec




42 sec






Final Rxn Time









56 sec




74 sec




95 sec




73 sec




60 sec






% Ht Expansion




150%




555%




492%




370%




467%




445%






Density (g/in


3


)






1.939






Water Absorption





67% 95%




48% 45%




44% 37%




50% 95%




62% 39%








(open chunk:




(open chunk:





(open chunk:




(open chunk:








260%)




49%)





75%)




143%)






Shore A Hardness





18




24




20




25




25






Shrinkage




1.5 mm




0 mm




0 mm




0.5 mm




3 mm




0 mm









Component wt %




Sample No. 31




Sample No. 32




Sample No. 33




Sample No. 34




Sample No. 35




Sample No. 36









Part A






Uvacure 1500




40




40




40




40




40






CN 301





15





15






Uvacure 1534









40






Part B






Arcol PPG-425




20





20




20




20




20






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




8.5






#1 Castor Oil




8




8




8




8




8




8






CN 301




15





22





15




15






Ebecryl 81





20






Z6040







1.5






KR TTS








1.5






Initial Rxn Time




41 sec




88 sec




38 sec




39 sec




37 sec




163 sec






Final Rxn Time




59 sec




120 sec




55 sec









54 sec




265+ sec






% Ht Expansion




461%




153%




386%




479%




433%






Density (g/in


3


)






Water Absorption




99% 66%





37% 45%




45% 34%




294% 243%







(open chunk:





(open chunk:




(open chunk:




(open chunk:







160%)





151%)




158%)




184%)






Shore A Hardness




22




72




22




22




22






Shrinkage




0 mm




1 mm




0 mm




0.5 mm




0 mm









Component wt %




Sample No. 37




Sample No. 38




Sample No. 39




Sample No. 40




Sample No. 41




Sample No. 42









Part A






Uvacure 1500




40




40




40




40




40




50.91






Ricon 100




15








19.09






SAT 030





25






Ricon 184






15




15






Expancel 461DU







10






Actipol E-16








15






Part B






Arcol PPG-425




20




20




20




20




20




20






Micropearls F30D




24.85




24.85




24.85




14.85




24.85




24.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




8.5






#1 Castor Oil




8




8




8




8




8




8






Initial Rxn Time




39 sec




66 sec




39 sec




31 sec




39 sec




43 sec






Final Rxn Time




64 sec




102 sec




63 sec




50 sec




68 sec




72 sec






% Ht Expansion




504%




348%




470%




345%




395%




432%






Density (g/in


3


)






Water Absorption




77% 79%




26% 43%




84% 93%




60% 63%




71% 90%




105% 72%







(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:







119%)




121%)




108%)




166%)




101%)




186%)






Shore A Hardness




26




22




27




30




32




31






Shrinkage




0 mm




0 mm




0 mm




0 mm




0 mm




0.5 mm









Component wt %




Sample No. 43




Sample No. 44




Sample No. 45




Sample No. 46




Sample No. 47




Sample No. 48









Part A






Uvacure 1500




40




40




40




40




40




40






SAT 030




15





15




15




15




15






Kraton L-2203





15






Erisys GE-35









10






Part B






Arcol PPG-425




20




20




20






20






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




8.5






#1 Castor Oil




8




8




8




8




8




8






CN 301




15






Santolink XI-100






10






Tone 0301







20




29.65






Initial Rxn Time




52 sec




39 sec




53 sec




31 sec




36 sec




48 sec






Final Rxn Time




84 sec




65 sec




83 sec




49 sec




53 sec




77 sec






% Ht Expansion




275%




431%




350%




480%




502%




395%






Density (g/in


3


)






Water Absorption




34% 36%




79% 61%




26% 40%




159% 220%




102% 102%




96% 75%







(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:







119%)




62%)




117%)




212%)




205%)




135%)






Shore A Hardness




30




26




27




17




16




25






Shrinkage




0 mm




0 mm




0.5 mm




0 mm




0 mm




0 mm









Component wt %




Sample No. 49




Sample No. 50




Sample No. 51




Sample No. 52




Sample No. 53




Sample No. 54









Part A






Uvacure 1500




40




40




40




40




40




40






SAT 030




15




15




15




15




15




15






Erisys GE-35




10






Part B






Arcol PPG-425




20




20





20




20




20






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




12




8.5




8.5




8.5




8.5




8.5






#1 Castor Oil




8




8




8




8





8






Kraton L-2203





15






Tone 0201






20






Santicizer 261







10




15






Z6124









2






Z6040









1






Initial Rxn Time




29 sec




59 sec




27 sec




51 sec




53 sec




45 sec






Final Rxn Time




50 sec




118 sec




36 sec




67 sec




63 sec




78 sec






% Ht Expansion




410%




317%




422%




263%




225%




458%






Density (g/in


3


)




1.826






Water Absorption




74%




29% 44%




104% 138%




19% 22%




41% 54%




22% 24%







(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:







53% & 64%)




86%)




133%)




75%)




137%)




180%)






Shore A Hardness




12




34




30




44




50




23






Shrinkage




0 mm




0.5 mm




2 mm




0 mm




0 mm




0.5 mm









Component wt %




Sample No. 55




Sample No. 56




Sample No. 57




Sample No. 58




Sample No. 59




Sample No. 60









Part A






Uvacure 1500




40




40




40




40




40




40






SAT 030







15






SAT 010




15






SAT 200





15






PBD 605






15





15




15






Part B






Arcol PPG-425




20




20




20




20




20




15






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




24.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




8.5






#1 Castor Oil




8




8




8




8




8




8






Santicizer 261







5




5




10






Z6124







2




2




2






Z6040







1




1




1






Initial Rxn Time




58 sec




50 sec




40 sec




51 sec




40 sec




29 sec






Final Rxn Time




83 sec




76 sec




80 sec




85 sec




69 sec




39 sec






% Ht Expansion




444%




435%




536%




388%




433%




320%






Density (g/in


3


)






Water Absorption




44% 60%




96% 105%




25% 27%




65% 53%




32% 33%




115% 105%







(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:







191%)




131%)




34%)




85%)




54%)




197%)






Shore A Hardness




25




20




24




22




23




19






Shrinkage




0 mm




0 mm




0 mm




0 mm




0.5 mm




0.5 mm









Component wt %




Sample No. 60




Sample No. 61




Sample No. 62




Sample No. 63




Sample No. 64




Sample No. 65









Part A






Uvacure 1500




40




40




40




40




40




40






PBD 605




15




20




25




15




15




15






Part B






Arcol PPG-425




20




20




20




20




25




20






Micropearls F30D




24.85




24.85




24.85




24.85




24.85




14.85






75% H


3


PO


4


(tech)




8.5




8.5




8.5




8.5




8.5




6.5






#1 Castor Oil




6




6




6




3




8






Santicizer 261




7




7




7




5






Z6124




2




2




2






Z6040




1




1




1






Initial Rxn Time




37 sec




43 sec




43 sec




42 sec




46 sec




48 sec 42 sec






Final Rxn Time




62 sec




74 sec




72 sec




71 sec




86 sec




77 sec 60 sec






% Ht Expansion




411%




357%




337%




493%




423%




475% 486%






Density (g/in


3


)









2.17






Water Absorption




28% 26%




17% 25%




56% 34%




43% 49%




29% 26%




17% 15%







(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:




(open chunk:







119%)




126%)




121%)




134%)




71%)




14%)






Shore A Hardness




23




22




18




20




20




29 30






Shrinkage




0.5 mm




0.5 mm




0.5 mm




0.5 mm




0.5 mm




0.8 mm



















Component wt %




Sample No. 66




Sample No. 67




Sample No. 68











Part A







Uvacure 1500




40




40




40







PBD 605




15




15




15







Z6040






1







Part B







Arcol PPG-425




20




20




20







Micropearls F30D




24.85




24.85




24.85







75% H


3


PO


4


(tech)




8.5




8.5




8.5







#1 Castor Oil




3




3




3







Santicizer 261




7




7




7







Z6124





2




2







Initial Rxn Time




39 sec




38 sec




41 sec







Final Rxn Time




65 sec




55 sec




56 sec







% Ht Expansion




455%




403%




439%







Density (g/in


3


)







Water Absorption




57% 72%




131% 130%




107% 88%








(open chunk =




(open chunk =




(open chunk =








153%)




160%)




156%)







Shore A Hardness




28




25




28







Shrinkage




0.5 mm




0.5 mm




1 mm















EXAMPLE 21























Component wt %




Sample No. 1




Sample No. 2




Sample No. 3




Sample No. 4




Sample No. 5




Sample No. 6









Part A






Uvacure 1500




32.7




36.4




43.6




40




40




40






PBD 605




12.3




13.6




16.4




20




25




15






Part B






Arcol PPG-425




20




20




20




20




20




20






Micropearls F30D




14.85




14.85




14.85




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5




6.5




6.5




6.5




6.5




6.5






Santicizer 160









4






Initial Rxn Time




47 sec




47 sec




50 sec




51 sec




54 sec




49 sec






Final Rxn Time




75 sec




70 sec




78 sec









104




67 sec






% Ht Expansion




564%




454%




430%




427%




387%




426%






Density (g/in


3


)






H


2


O Absorption 1






H


2


O Absorption 2






H


2


O Absorption 3




37%




31%




14%




28% 30%




42% 31%




74%






Shore A Hardness




28




31




32




33




33




38






Shrinkage




0 mm




0.3 mm




1.5 mm




0.8 mm




0.5 mm




3 mm









Component wt %




Sample No. 7




Sample No. 8




Sample No. 9




Sample No. 10




Sample No. 11




Sample No. 12









Part A






Uvacure 1500




40




40




40




40




40




40






PBD 605




15




15




15




10




15




15






Part B






Arcol PPG-425




20




20




20




20




20




20






Micropearls F30D




14.85




14.85




14.85




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5




6.5




6.5




6.5




8




9.5






Santicizer 160




8






Santicizer 278





4




8






Initial Rxn Time




51 sec




54 sec




55 sec




42 sec




32 sec




27 sec






Final Rxn Time




71 sec




80 sec




83 sec




57 sec









38 sec






% Ht Expansion




332%




395%




338%




529%




567%




500%






Density (g/in


3


)






H


2


O Absorption 1





44% 23%




26% 26%




61% 90%




25% 33%




56% 65%






H


2


O Absorption 2






H


2


O Absorption 3




106%




63%




87%




126%




34%




92% 83%






Shore A Hardness




43




24




32




30




29




28






Shrinkage




4 mm




2 mm




2 mm




0 mm (had




0.5 mm (had




0.75 mm (had










radial shrinkage)




radial shrinkage)




radial shrinkage)









Component wt %




Sample No. 13




Sample No. 14




Sample No. 15




Sample No. 16




Sample No. 17




Sample No. 18









Part A






Uvacure 1500




40




40




40




40




40




40






PBD 605




15




15




15




15




15




15






Epon SU2.5




10






Epon 828







5






Part B






Arcol PPG-425




20





29.98





20




20






Micropearls F30D




14.85




14.85




22.27




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5




6.5




9.75




6.5




6.5






CAPA 316





20






Tone 0301







20






Dicy 1400







2




0.26






85% H


3


PO


4


(tech)









6.5






Initial Rxn Time









20 sec




50 sec




74 sec




49 sec




36 sec






Final Rxn Time



















99 sec




70 sec




76 sec






% Ht Expansion




414%




430%




445%





451%




433%






Density (g/in


3


)






H


2


O Absorption 1






97% 106%






19% 14%






H


2


O Absorption 2






H


2


O Absorption 3




40% 56%




69% 65% 57%




128%






22% 13% 17%






Shore A Hardness




53




43




26





30




32






Shrinkage




3 mm




0 mm (had




2.8 mm




very significant




2.6 mm




0 mm








radial shrinkage)









Component wt %




Sample No. 19




Sample No. 20




Sample No. 21




Sample No. 22




Sample No. 23




Sample No. 24









Part A






Uvacure 1500




40




40




35




35




35




40






PBD 605




15




15




15




15




15




15






Epon 828









10






Part B






Arcol PPG-425




20








20






Micropearls F30D




14.85




14.85




14.85




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5




6.5




6.5




5




8




6.5






Ebecryl 170




5








15






Desmophen L-951





20




20




20




20






Initial Rxn Time




25 sec




44 sec 50 sec




48 sec 48 sec




72 sec




37 sec 34 sec




18 sec






Final Rxn Time




43 sec




64 sec 67 sec




79 sec 70 sec




100 sec




57 sec 51 sec




35 sec






% Ht Expansion




415%




467% 510%




505% 442%




420%




530% 535%




289%






Density (g/in


3


)




1.93




2.02






H


2


O Absorption 1




9% 15%




15% 18%




20% 22%





39% 19%






H


2


O Absorption 2








36%






H


2


O Absorption 3




39% 22%




32% 22% 37%




60% 49% 73%





66% 55% 61%




81% 48%






Shore A Hardness




35




38 31




29 32




31




30 27




52






Shrinkage




0.3 mm




1.5 mm 0.8 mm




0.5 mm 0.75 mm




3.3 mm




0.5 mm 0.75 mm




2 mm









Component wt %




Sample No. 25




Sample No. 26




Sample No. 27




Sample No. 28




Sample No. 29




Sample No. 30









Part A






Uvacure 1500




40




30




40




30




40




40






PBD 605




15





15




15




15




7.5






Epon 828







10






SAT 030









7.5






Part B






Arcol PPG-425









20






Micropearls F30D




14.85




14.85




14.85




14.85




14.85




14.85






75% H


3


PO


4


(tech)






6.5




6.5




6.5




6.5






Desmophen L-951




20





10




20






Ebecryl 170




20




30




5




5






Santicizer 261






10






K-Flex 188








20






Initial Rxn Time





<10 sec




21 sec




25 sec




27 sec




48 sec






Final Rxn Time






36 sec




41 sec









61 sec






% Ht Expansion





350%




358%




333%




456%






Density (g/in


3


)







3.45






H


2


O Absorption 1







28% 38%






H


2


O Absorption 2







89%






H


2


O Absorption 3






94% 95%




84% 83% 85%




32% 28% 30%




19% 22%






Shore A Hardness






39




37




47






Shrinkage





0.5 mm




2.5 mm




2.5 mm




0.9 mm









Component wt %




Sample No. 31




Sample No. 32




Sample No. 33




Sample No. 34




Sample No. 35




Sample No. 36









Part A






Uvacure 1500




40




40




40




40




40




20






PBD 605




7.5





15




15





15






Epon 828






SAT 030




7.5






Trilene M-101





15






Hycar 1300x40








15






Uvacure 1533









20






Part B






Arcol PPG-425




20




20




20




20




20




20






Micropearls F30D




14.85




14.85




14.85




14.85




14.85




14.85






75% H


3


PO


4


(tech)




6.5




6.5




6.5




6.5




6.5




6.5






Ebecryl 170




2






#1 Castor Oil






6






Santicizer 141







10






Initial Rxn Time




31 sec




46 sec




49 sec




56 sec




45 sec




47 sec






Final Rxn Time




49 sec




60 sec




68 sec




71 sec




55 sec




78 sec






% Ht Expansion





394%






Density (g/in


3


)






H


2


O Absorption 1






H


2


O Absorption 2






H


2


O Absorption 3




22% 23%




114% 81% 107%




17% 15%




51% 70%





30% 34%






Shore A Hardness





40






Shrinkage





2.75 mm









Component wt %




Sample No. 37




Sample No. 38




Sample No. 39




Sample No. 40




Sample No. 41




Sample No. 42









Part A






Uvacure 1500




25




40




40




40






PBD 605




15




15




15




15






Epon 828








45




45






Uvacure 1534




15






Part B






Arcol PPG-425




20




20




20




20






Micropearls F30D




14.85




14.85




14.85




14.85




15




15






75% H


3


PO


4


(tech)




6.5






H


3


PO


4


(conc: >95%)





6.5




4.9




4




10




10






Tone EC Monomer








20






#1 Castor Oil









20






Initial Rxn Time




58 sec




28 sec




33 sec




37 sec




58 sec




33 sec






Final Rxn Time




73 sec




37 sec




52 sec




50 sec




93 sec











% Ht Expansion





274%




261%




181%




510%




300%






Density (g/in


3


)








1.8






H


2


O Absorption 1






H


2


O Absorption 2






H


2


O Absorption 3




27% 33%





15% 20%





37% 38%









(72 hrs)





(72 hrs)






Shore A Hardness





62




60




62




48




68






Shrinkage








0 mm




0 mm




















Component wt %




Sample No. 43




Sample No. 44




Sample No. 45




Sample No. 46











Part A







Epon 828




45




45




50




50







Vertrel XF







5







Part B







Micropearls F30D




15




15




15




10







H


3


PO


4


(conc: >95%)




10




20




10




10







Santicizer 261




20







Pure Grain Alcohol





20







(EtOH)







Santicizer 97






20




20







Initial Rxn Time




24 sec




108 sec




27 sec




26 sec







Final Rxn Time




72 sec




130 sec

















% Ht Expansion




182%




575%




376%




297%







Density (g/in


3


)





1.37







H


2


O Absorption 1







H


2


O Absorption 2







H


2


O Absorption 3





843%









(after 15 mins)







Shore A Hardness




78




4





62







Shrinkage




0.5 mm




0.5 mm





0 mm




















EXAMPLE 22























Component wt %




Sample No. 1




Sample No. 2




Sample No. 3




Sample No. 4




Sample No. 5




Sample No. 6









Part A






Uvacure 1500




40






PBD 605




15






Epon 828





40




40




35




35




50






Santicizer 97







5




5






Part B






Desmophen L-951




20






H


3


PO


4


(75% tech)




6.5






Micropearls F30D




2




10




10




10




10




10






H


3


PO


4


(>95% conc)





10




10




10




10




10






Arcol PPG-425





20






Santicizer 97






20




20




15




20






#1 Castor Oil








5






Initial Rxn Time




43 sec




263 sec




20 sec




19 sec




24 sec




25 sec






Final Rxn Time




54 sec




299 sec


























% Ht Expansion




86%




308%




189%




118%




122%




184%






Density (g/in


3


)





2.50




6.20





6.93




6.13






H


2


O Absorption 1




3%






H


2


O Absorption 2






H


2


O Absorption 3




3%




27% 23%




8% 10%




18% 22% 18%




11% 12%




5% 6%






Shore A Hardness






88




90




88




88






Shore D Hardness




(32)





27 (30)




30 (32)




27 (30)




28 (30)






(##) = calculated






Shrinkage




2.2 mm




0 mm




0 mm




0 mm




0 mm




0 mm









Component wt %




Sample No. 7




Sample No. 8




Sample No. 9




Sample No. 10




Sample No. 11




Sample No. 12









Part A






Epon 828




40




20




40




40




40




60






CMD 50859





20






Tone EC








2




3






Part B






Santicizer 97





20




20




15




15




15






H


3


PO


4


(>95% conc)




10




10




10




10




10




10






Micropearls F30D




10




10




6




6




4




4






Santicizer 160




20






#1 Castor Oil







5




5




5






Initial Rxn Time




17 sec




22 sec




18 sec




22 sec




22 sec




30 sec






Final Rxn Time




































% Ht Expansion




260%




152%




120%




145%




99%




92%






Density (g/in


3


)





4.20




7.03




6.40




6.94




8.19






H


2


O Absorption 1






H


2


O Absorption 2






H


2


O Absorption 3




40% 32% 39%




50% 34%




13% 12%




13% 11%




15% 10%




3% 2%






Shore A Hardness





80




91




86




93




98






Shore D Hardness





23 (22)




32 (33)




26 (28)




34 (36)




46 (42)






(##) = calculated






Shrinkage




0 mm




0 mm




0 mm




0 mm




0 mm




0 mm









Component wt %




Sample No. 13




Sample No. 14




Sample No. 15




Sample No. 16




Sample No. 17




Sample No. 18









Part A






Epon 828




40




60




80




80




50




50






Santicizer 97




5




7.5




10




10






Vertrel XF







5




10






Part B






Santicizer 97




15




15




15




15




20




20






H


3


PO


4


(>95% conc)




10




10




10




10




10




10






Micropearls F30D




6




6




6




6




5




10






#1 Castor Oil




10




10




10




10





10






Initial Rxn Time














69 sec




66 sec




24 sec




41 sec






Final Rxn Time




































% Ht Expansion














60%




61%




238%




123%






Density (g/in


3


)





























4.64-8.38






H


2


O Absorption 1




































H


2


O Absorption 2




































H


2


O Absorption 3




14%




8% 8%




1% 1%














32% 35%






Shore A Hardness



















90









90






Shore D Hardness



















(32)









29 (32)






(##) = calculated






Shrinkage














0 mm




0 mm




0 mm




0 mm

















Component wt %




Sample No. 19











Part A







Epon 828




65







Santicizer 97




5







Part B







Santicizer 97




15







H


3


PO


4


(>95% conc)




10







Micropearls F30D




10







Initial Rxn Time




25 sec







Final Rxn Time












% Ht Expansion




176%







Density (g/in


3


)




6.55







H


2


O Absorption 1







H


2


O Absorption 2







H


2


O Absorption 3




4% 4%








(after 48 hrs)







Shore A Hardness




93







Shore D Hardness




(36)







(## = calculated)







Shrinkage




0 mm















EXAMPLE 23




This Example illustrates the ability to tailor the inventive foam compositions and obtain foams having a wide range of characteristics. A foam of relatively low density was produced by in accordance with Example 18. The foam was obtained by combining the following foam precursors:


















AMOUNT




COMPONENT




TRADE NAME




SUPPLIER























Part A:















18.2




g




cylcoaliphatic




Uvacure 1500




Radcure








epoxy






1.8




g




phenoxy resin




Phenoxy PKHP-200




Paphen






30




g




bis-A epoxy




D.E.R. 736




Dow Chemical











Part B:















29.65




g.




caprolactone




Tone 0301




Union Carbide








polyol






14.85




g.




vinylidene




Micropearls F30D




Pierce & Stevens








chloride








encapsulated








iso-butane






5.5




g.




phosphoric





ACROS








Acid (85%)














Each component (Part A & B) was individually mixed by hand using a hand driven paddle in a cup or ointment can. The two were brought together in a single vessel, again mixed by hand, and allowed to react. The foam produced was similar in appearance to other types listed above, but had a final specific gravity 0.16 g/ml.




EXAMPLE 24




The following Example demonstrates employing the inventive foam as a structural material between two laminates to fabricate furniture. The components listed in the following Table were combined in accordance with Examples 18-22.






















Sample




Sample






Components wt. %




Sample No. 1




Sample No. 2




No. 3




No. 4






























Part A













Epon 828




75
















50






Santicizer 97




5























Epon 813










50

















Epon 825















50












Part B






Santicizer 97




20





20




20





23






H


3


PO


4


(>95% conc)




10





10




10





10






Micropearls F30D




10





10




10





10






Initial Rxn Time




40




sec




    33 sec




28




sec




28




sec






Final Rxn Time




























% Ht Expansion




136%





   262% 




225%





170%






Density 1 (g/in


3


)




























Density 2 (g/in


3


)




8.77










5.70





5.52






H


2


O Absorption 1




1% 1%




2%






















H


2


O Absorption 2




























Shore A Hardness




95
















81






Shore D Hardness




40


















(##) = calculated




(38)








(23)






Shrinkage




0




mm




      0 mm




0




mm




0




mm









Had significant









radial









shrinkage














The following Table lists components employed in the above Table for making foam.

















Trade Name




Component




Supplier











#1 Castor Oil




#1 Castor Oil




Commercial






Epon 825




Bis A Epoxy




Shell Chemical Co.






Epon 828




Bis A Epoxy




Shell Chemical Co.






Epon 813




Bis A Epoxy Modified: (74% Bis-




Shell Chemical Co.







phenol A epichlorohydrin resin &







26% Cresyl glycidyl ether)






Santicizer 97




Dialkyl Adipate




Solutia






H


3


PO


4






Phosphoric acid: Took Harcros




DeNOVUS






(>95% conc)




75% Technical Grade & distilled







to > 90% acid concentration






Micropearls




Therma Blowing Agent: isobutane




HM Royal (Pierce






F30D




encapsulated in polymer vinylidene




& Stevens)







chloride














Sample No. 1 above was combined and introduced into a mold comprising standard 1″×4″×12″ boards and laminating materials comprising wood-grain Formica® and fiber-reinforced paper board that were maintained a defined distance about by wood spacers, i.e., a distance of about ½ inch. The boards and laminating materials were placed into “C” clamps and a vise. The foam composition was prepared and poured between the laminating materials. Once the foam reaction was completed and the foam had cooled to room temperature, the assembly was visually inspected. The foam had adhered to the laminating materials and provided structural support.




EXAMPLE 25





















Component




Sample No.




Sample No.




Sample No.




Sample No.




Sample No.




Sample No.






Wt. %




1




2




3




4




5




6











Part A












Epon 828




48




23




50




34.5




50




50






Santicizer 97




2






Epon 825





23





9.5






Part B






Santicizer 97




19.8




20




20




18






H


3


PO


4


(>95%




11




10




10




10




10




10






conc)






Micropearls F30D




13.7




12.5




2




12.5




12.5




12.5






Expancel 642DU






2






Expancel 820DU






2






Expancel 551DU






2






Expancel 461DU






2






SR 239








20






SR 495









20






Initial Rxn Time




28 sec 26




38 sec




38 sec




28 sec 34




41 sec




79 sec







sec






sec






% Ht Expansion




289%




320%




240%




306% 275%




269%




399%






Density 1 (g/in


3


)





2.41-2.75






Density 2 (g/in


3


)




3.35






H


2


O Absorption 1




16% 20%




13% 13%






Shore A




50




63






Hardness






Shrinkage




0 mm




0 mm




0 mm




0 mm




0.5 mm




1 mm (had











(had radial




radial shrinkage)











shrinkage)














EXAMPLE 26




The following Example demonstrates a composition of the instant invention that can be dispensed via a commercially available dual tube caulk gun.


















Product Name




Chemical Name




Supplier




% range























Part A














Epon 862




Bis F epoxy resin




Shell




5-75






Cardura E-10




glycidyl ester




Walsh & Assoc




1-30






Polybd ®




polybutadiene




Elf Atochem




1-60






605 E






Micropearls




Isobutane encapsulated in




HM Royal




10-75 






F30 D




Polymer vinylidene chloride











Part B














Phosphoric




phosphoric acid




Harcross




3-25






acid






CD513




methacrylate




Sartomer




1-10






SR495




caprolactone acrylate




Sartomer




1-10














Parts A and B were prepared separately by being mixed in lab scale beakers. Parts A and B were mixed and dispensed by using a 4:1 TAH Industries motionless mixer tube.




EXAMPLE 27




The following Table lists the Raw Materials that were employed in Example 27. The foam in Example 27 was prepared and tested in accordance with Examples 18-22 and 25. This Example illustrates foam having desirable flame resistant characteristics. Such foam can be employed in a wide range of applications including aerospace (e.g., aircraft insulation), automotive (e.g., sound abatement and structural support), among other end uses.



















Raw Material




Description




Supplier









Intelimer 7004




Polymer Bound Imidazole Catalyst: MP = 149F




Landec






Intelimer 7024




Encapsulated 2-Ethyl-4-Methyl Imidazole:




Landec







MP = 149F






Intelimer 7124




Polymer Bound Imidazole Catalyst




Landec






PEP 6137




Acrylic Monomer Modifier Epoxy: EEW = 150:




Pacific Epoxy







Visc = 950 cP






PEP 6138




Acrylic Monomer Modified Epoxy: EEW = 150:




Pacific Epoxy







Visc = 100 cP






PEP 6139




Acrylic Monomer Modified Epoxy: EEW = 130:




Pacific Epoxy







Visc = 3000 cP






PEP 6264




Urethane Modified Epoxy: EEW = 210:




Pacific Epoxy







Visc = 2000 cP






PEP 6431




Novolac: EEW = 170: visc = 25,000: fnc = 2.2




Pacific Epoxy






PEP 6433




Novolac: EEW = 170: visc = 8000: fnc = 2.2




Pacific Epoxy






NPEK-119




Bis A Epoxy: EEW = 180-195: Visc = 500-1200




Peninsula Polymers/Nan








Ya Corporation






Epon 824




Bis A/Epichlorohydrin Based Epoxy Resin (85-90%)




Walsh & Assoc/Shell







& Modified Base Epoxy Resin (10-15%)




Chemical






Epon 826




Bis A/Epichlorohydrin Based Epoxy Resin:




Walsh & Assoc/Shell







EEW = 182: Visc = 8000 cP




Chemical






SR 239




DiFunctional: 1,6 Hexanediol Dimethacrylate:




Sartomer







visc = 8: hydrophobic backbone






SR 9009




TriFunctional: Trifunctional Methacrylate:




Sartomer







visc = 35






CD 9050




Monofunctional Acid Ester: Adhesion




Walsh &







Promoting Monomer: visc = 20




Assoc/Sartomer






CD 9051




Trifunctional Acid Ester: Adhesion Promoting




Walsh &







Monomer: visc = 250




Assoc/Sartomer






SR 444




Trifunctional Monomer: Pentaerythritol




Walsh &







Triacrylate: Hydroxy Pendant Group:




Assoc/Sartomer







visc = 520 cP






CD 513




Methacrylate Ester (Propoxylated


2


Allyl




Sartomer







Methacrylate): Commercially available under







5E consent






Ebecryl 2047




Trifunctional Acrylated Diluting Oligomer:




UCB Radcure







visc = 400 cP: tensile = 1000 psi: elong = 8%:




UCB Radcure







Tg = 3F






Ebecryl 3200




Acrylated Epoxy: visc = 3000 cP:




UCB Radcure







tensile = 11,900 psi: elong = 6%: Tg = 118F






Kronitex TCP




Tricrecyl Phosphate: Flame Retardant




FMC Corp






Santicizer 143




Modified Triaryl Phosphate Ester




Solutia






Santicizer 148




Isodecyl Diphenyl Phosphate




Solutia






Santicizer 154




Triaryl Phosphate Ester: t-Butylphenyl




Solutia







Diphenyl Phosphate






NOVOC RGS-2020DV




Modified Vinyl Ester: WPE = 300-2800:




Composite







Visc = 800 cP: Acid Value = 14-20




Technology






Veova 10




Vinyl Ester Of Tertiary Carboxylic acid:




Walsh & Assoc/Shell







Neodecanoic acid, ethenyl ester: visc = 8 cP


















Components Wt. %




Sample No. 1




2




3




4









Part A






Epon 828




60




60




60




60






BK 5799 (carbon Black)




4 g




4 g




4 g




4 g






Part B






Santicizer 97




15




15




15




15






H


3


PO


4


(conc)




7.5




7.5




7.5




7.5






Micropearls F30D




8




8




8




8






Intelimer 7004





1.5






Intelimer 7024






1.5






Intelimer 7124







1.5






Initial Rxn Time (sec)




51 sec




64 sec




78 sec




81 sec






Shrinkage




0 mm




0 mm




0 mm




0 mm






% Height Expansion




221%




238%




257%




234%






Density 2 (g/in


3


)






Top




4.53




4.51




4.72




4.20






Bottom




4.87




4.93




5.25




4.76






Specific Gravity






% H


3


O Absorption 2




2.8% 2.0%




4.8% 3.0




6.8% 4.9%




7.5% 5.2%






Shore A: Initial




81 85




80 82




86 85




75 77






Shore A - After 24 hr Water Soak




82 84




79 79




80 78




72 71



















Components Wt. %




Sample No. 5




6




7




8




9









Part A






Epon 828




60






30




30






BK 5799




4 g






Epon 826





60




60




30




30






Z6040








1






Part B






Santicizer 97





15




28.46




28.46




28.46






H


3


PO


4


(conc)




7.5




7.5




13.34




13.34




13.34






Micropearls F30D




8




8




14.23




14.23




14.23






CD 513




15






Initial Rxn Time (sec)




92 sec




50 sec




32 sec




31 sec




32 sec






Shrinkage




0 mm




0 mm




0 mm




0 mm




0 mm






% Height Expansion




383%




278%




238%




209%




240%






Density 1 (g/in


3


)






Density 2 (g/in


3


)






Top





4.75




3.72




5.05




4.50






Bottom





4.78




4.15




4.62




4.45






% H


2


O Absorption 1






% H


2


O Absorption 2





54% 71%




74% 38%




11% 9%




15% 13%






Shore A: Initial





90 86




74 77




89 87




83 80






Shore A - After 24 hr





78 75




45 57




70 73




57 56






Water Soak






Shore A: % Drop





13%↓, 13%↓




39%↓, 39%↓




21%↓, 16%↓




31%↓, 30%↓






After 24 hr H


2


O Soak



















Components Wt. %




Sample No. 10




11




12




13




14









Part A






Epon 828




30




60




60




30




40






BK 5799







4 g)




4 g






Epon 826




30






30






Z6040




1




2.5




3.5




2






PEP 6264








20






Part B






Santicizer 97




28.46




28.46




28.46




25.14




15.5






H


3


PO


4


(conc)




11




13.34




13.34




11.79




7.5






Micropearls F30D




14.23




14.23




14.23




12.57




8






Initial Rxn Time (sec)




45 sec




38 sec




47 sec




44 sec




281 sec






Shrinkage




0 mm




0 mm




0.5 mm




0.5 mm




0.5 mm






% Height Expansion




178%




232%




227%




233%




50%






Density 1 (g/in


3


)






Density 2 (g/in


3


)






Top




6.11




4.53




5.14




4.13






Bottom




6.08




4.13




4.83




4.46






% H


2


O Absorption 1






% H


2


O Absorption 2




24% 26%




56% 41%




73% 86%




27% 20%






Shore A: Initial




84 86




72 67




81 79




83 80






Shore A - After 24 hr




67 68




30 31




44 38




50 48






Water Soak






Shore A: % Drop




20%↓, 21%↓




58%↓, 54%↓




46%↓, 52%↓




40%↓, 40%↓






After 24 hr H


2


O Soak


















Components Wt %




Sample No. 15




16




17




18









Part A






Epon 828




40




40




40




40






BK 5799




4 g




4 g




4 g




4 g






PEP 6264




20






PEP 6137





20






PEP 6138






20






PEP 6139







20






Part B






Santicizer 97 $1.22/lb




15.5




15.5




15.5




15.5






H


3


PO


4


(conc) $0.70/lb




10




7.5




7.5




7.5






Micropearls F30D $8/lb




8




8




8




8






Initial Rxn Time (sec)




116 sec




74 sec




81 sec




77 sec






Shrinkage




0.5 mm




0 mm




0 mm




0 mm






% Height Expansion




55%




210%




223%




204%






Density 1 (g/in


3


)






Density 2 (g/in


3


)






Top




11.88




4.64




4.27




4.44






Bottom





5.24




4.94




4.99






% H


2


O Absorption 1






% H


2


O Absorption 2




20%




4% 3%




6% 5%




5% 3%






Shore A: Initial




96




84 86




78 84




85 87






Shore A - After 24 hr




90




73 75




63 66




72 70






Water Soak






Shore A: % Drop




6%↓




13%↓, 13%↓




19%↓, 21%↓




15%↓, 20%↓






After 24 hr H


2


O Soak


















Components Wt %




Sample No. 19




20




21




22









Part A






Epon 828





40




45




50






BK 5799 (carbon black)






NPEK-119




60




10






DER 736






15






CD 513







10






Part B






Santicizer 97




15




24.73




24.73




28.8






H


3


PO


4


(>85% conc)




7.5




11.6




11.6




13.5






Micropearls F30D




8




12.37




12.37




14.4






Initial Rxn Time




68 sec




33 sec




instant




44 sec






% Ht Expansion




233%




241%





190%






Density (g/in


3


)






Top




4.50




4.18





4.01






Bot




4.28




4.72





4.44






H


2


O Absorption




25% 12%




25% 13%





151%






Shore A: Initial




85 81




75 82





67 68






Shore A: After Water Soak




67 58




52 60





10 16






Shore A % Drop After Water Soak




21%↓, 28%↓




27%↓,27%↓





85%↓, 77%↓






Shrinkage




0.2%




<2%

















Components Wt. %




Sample No. 23




24




25









Part A






Epon 828




50




30




30






BK 5799 (carbon black)





4 g




4 g






Z 6040




2.5




2






Epon 826





30




30






Part B






Santicizer 97




22.86




25.14




16.76






H


3


PO


4


(>85% conc)




11.9




11.79




7.86






Micropearls F30D




12.7




12.57




8.38






Kraton D1107




2.54






Initial Rxn Time




33 sec




44 sec 53 sec




49 sec






% Ht Expansion




228%




233% 204%




210%






Density (g/in


3


)






Top




4.12




4.13




4.53






Bot




4.47




4.46




5.09






H


2


O Absorption




(72 hrs: 118% 148%)




27% 20%




3% 2%






Shore A: Initial




78 71




83 80




85 89






Shore A: After Water Soak




(72 hrs: 25 26)




50 48




79 82






Shore A % Drop After Water Soak




72 hrs Soak 68%↓, 63%↓




40%↓, 40%↓




7%↓, 8%↓






Shrinkage




0.2%




0.9%




0.6%


















Components Wt %




Sample No. 26




27




28




29









Part A






Epon 828




30




30




30




60






BK 5799 (carbon black)




4 g




4 g




4 g




4 g






Epon 826




30




30




30






PEP 6210 PA




10






Cardura E-10






10




10






Part B






Santicizer 97




16.76




16.76




16.76




16.76






H


3


PO


4


(>85% conc)




7.86




7.86




7.86




7.86






Micropearls F30D




8.38




8.38




8.38




8.38






Initial Rxn Time




183 sec




44 sec




63 sec




57 sec ?






% Ht Expansion




<50%




197%




257%




250%






Density (g/in


3


)






Top





4.97




5.19




5.34






Bot





5.42




4.72




5.33






H


2


O Absorption





3% 3%




26% 17%




9% 4%






Shore A: Initial





87 89




88 82




88 84






Shore A: After Water Soak





82 84




62 57




63 56






Shore A % Drop After Water Soak





6%↓, 6%↓




30%↓, 31%↓




28%↓, 33%↓






Shrinkage





0.2%




2.1%




2.5%
















Components Wt %




Sample No. 30




31









Part A






Epon 828




65.5




65.5






BK 5799 (carbon black)




4 g




4 g






Cardura E-10




3.5




3.5






Part B






Santicizer 97




17




17






H


3


PO


4


(>85% conc)




7.5




7.5






Micropearls F30D




8.5






Initial Rxn Time




84




53






% Ht Expansion




205% 215%




0%






Density (g/in


3


)






Top




5.09











Bot




5.60




18.83






H


2


O Absorption




(72 hrs: 4% 3%)




0.22% (96 hrs)






Shore A: Initial




90 90




>100






Shore A: After Water Soak




(72 hrs: 87 86)




>100 (96 hrs)






Shore A % Drop After Water Soak




(72 hrs: 3%↓, 4%↓)




0% (96 hrs)






Shrinkage




0.4%




3%






Compression: 1″d (psi)




1483 1450






Compression: 2″d (psi)




1113


















Components Wt %




Sample No. 32




33




34




35









Part A






Epon 828




65.5




65.5




65.5




65.5






BK 5799 (carbon black)




4 g




4 g




4 g






Cardura E-10




3.5




3.5




3.5




3.5






Expancel 051DU




5






Part B






Santicizer 97




17




8.5






H


3


PO


4


(>85% conc)




7.5




7.5




7.5




7.5






Micropearls F30D





8.5




8.5




8.5






Expancel 051DU






Veova 10





8.5





7






Santolink XI-100






17






Cardura E-10







10






Initial Rxn Time




120+ sec




94 sec




232 sec




77 sec






% Ht Expansion




<25%




137%




258%




206%






Density (g/in


3


)






Top






4.16




4.68






Bot






4.19




5.27






H


2


O Absorption






2% 2%




1.3% 1%






Shore A: Initial






73 75




79 79






Shore A: After Water Soak






61 64




70 69






Shore A % Drop After Water Soak






16%↓, 15%↓




11%↓, 13%↓






Shrinkage






0.7%




1%



















Components Wt %




Sample No. 36




37




38




39




40









Part A






Epon 828




55.5





95




65.5




65.5






Cardura E-10




3.5




3.5




5




3.5




3.5






Erisys GE-60




10






Epalloy 8240





65.5






BK 5799 (carbon Black)






4 g




4 g






Micropearls F30D








8.5






Part B






H


3


PO


4


(>85% conc)




7.5




7.5




11




7.5




7.5






Micropearls F30D




8.5




8.5




8.5




8.5






Cardura E-10




12




12





12






Veova 10




5




5






Santicizer 97






17




5






Initial Rxn Time




69 sec




75 sec




63 sec




203 sec




17 sec






% Ht Expansion




130%




229%




166%




245%




335%






Density (g/in


3


)






Top





4.63




5.83




4.46






Bot





5.42




6.11




4.99






H


2


O Absorption





(72 hrs) 5% 3%




1% 1%




10% 6%










(72 hrs)






Shore A: Initial





74 74




94 95




76 76






Shore A: After





(72 hrs) 69 67




91 91




65 66






Water Soak







(72 hrs)






Shore A % Drop





(72 hrs)




3%↓, 4%↓




15%↓, 13%↓






After Water Soak





7%↓, 10%↓





(72 hrs)






Shrinkage




Slight




1%




0.4% 0.5%




1.1%






Compression: 1″d (psi)






2724 2504



















Components Wt %




Sample No. 41




42




43




44




45









Parts A






Epon 828




65.5




65.5




65.5




65.5




65.5






Cardura E-10




3.5




3.5




3.5




3.5




3.5






BK 5799 (carbon Black)




4 g




4 g




4 g




4 g




4 g






Part B






H


3


PO


4


(>85% conc)




7.5




7.5




7.5




7.5




7.5






Micropearls F30D




8.5




8.5




8.5




8.5




8.5






Ebecryl 2047




17






Ebecryl 3200





17






CD 9051






17






CD 9050







17






SR 444








17






Initial Rxn Time




81 sec




92 sec




63 sec




82 sec




71 sec






% Ht Expansion




275%




275%




285%




290%




300%






Density (g/in


3


)






Top




4.69




3.92




3.67




3.89




3.59






Bot




4.70




4.75




4.20




4.06




4.12






H


2


O Absorption




32%? 2%




3% 27%?




6% 3%




29% 42%




15% 10%











(see 1 below)






Shore A: Initial




88 83




83 83




81 82




78 80




78 78






Shore A: After




78 73




70 73




66 67




52 51




75 75






Water Soak






Shore A % Drop




11%↓, 12%↓




16%↓, 12%↓




19%↓, 18%↓




33%↓, 36%↓




4%↓, 4%↓






After Water Soak






Shrinkage




1.1%




0.2%




0.3%




2%




1.2%


















Components Wt %




Sample No. 46




47




48




49









Part A






Epon 828




65.5




65.5




65.5




55.5






Cardura E-10




3.5




3.5




3.5




3.5






BK 577 (carbon Black)




4 g




4 g




4 g




4 g






Epalloy 8240







10






Erisys GE-60






Part B






H


3


PO


4


(>85% conc)




7.5




7.5




7.5




7.5






Micropearls F30D




8.5




8.5




8.5




8.5






Santicizer 278




17






SR 9009





17






SR 239






17






Santicizer 97







17






Initial Rxn Time




54 sec




54 sec




79 sec




49 sec






% Ht Expansion




260%




268%




320%




214%






Density (g/in


3


)






Top




4.07




3.99




3.63




4.82






Bot




4.83




4.41




4.20




5.41






H


2


O Absorption




27% 4% (see 1)




53% 39% (see 1)




12% 9%




3% 2%






Shore A: Initial




80 82




85 85




69 71




86 87






Shore A After Water Soak




67 72




77 79




65 67




83 85






Shore A % Drop After Water Soak




16%↓, 12%↓




9%↓, 7%↓




6%↓, 6%↓




4%↓, 2%↓






Shrinkage




0.6%




2%




6%




0.3%


















Components Wt %




Sample No. 50




51




52




53









Part A






Epon 828




65.5




55.5




55.5




55.5






Cardura E-10




3.5




3.5




3.5




3.5






BK 5799 (carbon Black)




4 g




4 g




4 g




4 g






Micropearls F30D




8.5






PEP 6433





10






PEP 6431






10






Epalloy 8240







10






Part B






Santicizer 97




17




17




17




17






H


3


PO


4


(>85% conc)




7.5




7.5




7.5




7.5






Micropearls F30D





8.5




8.5




6.5






Initial Rxn Time




56 sec




88 sec




51 sec




52 sec






% Ht Expansion




165%




133%




157%




123%






Density (g/in


3


)






Top




5.39




8.98




5.72




7.15






Bot




5.82




9.59




6.30




7.63






H


2


O Absorption




2% 1%




36% 29%




0.7% 0.7%




0.5% 0.4%







(72 hrs)






Shore A: Initial




89 90




97 98




91 94




97 97






Shore A: After Water Soak




85 87




93 94




87 91




95 95






Shore A % Drop After Water Soak




5%↓, 3%↓




4%↓, 4%↓




4%↓, 3%↓




2%↓, 2%↓







(72 hrs)






Shrinkage




0.4%




0.2%




0.1%




0.3%






Compression: 1″d (psi)






1886 2090






Compression: 2″d (psi)







2190



















Components Wt %




Sample No. 54




55




56




57




58









Part A






Epon 828




50




65.5




55.5




65.5




55






Cardura E-10





3.5




3.5




3.5




3.5






BK 5799 (carbon Black)




4 g




4 g




4 g




4 g




4 g






Epalloy 8240




20






PEP 6431






10






PBD 605








10






Part B






Santicizer 97




17




12




17




20.4




20.4






H


3


PO


4


(>85% conc)




7.5




7.5




7.5




9




9






Micropearls F30D




8.5




3.5




5




2.5




4






Initial Rxn Time




57 sec




51 sec




56 sec




54 sec 51 sec




37 sec






% Ht Expansion




213%




45%




40%




23% 30%




21%






Density (g/in


3


)






Top




5.21




10.77









12.28






Bot




5.87




10.89




9.44




12.41






H


2


O Absorption




2% 0.9%




0.2%




0.6%




1.1% (5 days)









(72 hrs)






Shore A: Initial




88 92




100




99




100+






Shore A: After Water Soak




85 88




99




98




98 (5 days)









(72 hrs)






Shore A % Drop After Water Soak




3%↓, 5%↓




1%↓




1%↓




2%↓ (5 days)









(72 hrs)






Shrinkage




0.1%




1.4%




0.8%




1.9%






Compression: 1″d (psi)




1825 1939




4875 4768




3472 4070




5762 6141




5132 4874

















Components Wt %




Sample No. 59




60




61









Part A






Epon 828




150.65




65.5




65.5






Cardura E-10




8.05






BK 5799 (carbon Black)




4 g




4 g




4 g






Veova 10





10






Z 6040






2






Part B






Santicizer 97




17




17




17






H


3


PO


4


(>85% conc)




16




7.5




7.5






Micropearls F30D




5




6.5




6.5






Initial Rxn Time




42 sec 30 sec




54 sec




96 sec






% Ht Expansion




20%




20%




122%






Compression: 1″d (psi)




7212 7201





1955 1940

















Components Wt %




Sample No. 62




63




64









Part A






Epon 828




65.5




65.5




65.5






Cardura E-10




3.5





3.5






BK 5799 (carbon black)




4 g




4 g




4 g






Santicizer 97





3.5






Part B






Santicizer 97




20




20.4






H


3


PO


4


(>85% conc)




6.5




9




9






Micropearls F30D




4.5




2.5




2.5






RGS-2020 DV






20.4






Initial Rxn Time




81 sec




58 sec




175 sec






% Ht Expansion




32%




23%




67%






Density (g/in


3


)






Top





11.44




9.54






Bot




11.4




11.38




10.21






H


2


O Absorption




(72 hrs) 0.4%




0.9




1.3%






Shore A: Initial




100+




100+




98






Shore A: Water Soak




(72 hrs) 100




99




91






Shore A % Drop After Water Soak




(72 hrs) 0%+




1%+




7%






Salt: % Absorption




0.5%




1.5%






Salt: % Shore A Drop




1%+




16%+






Shrinkage




1.1




1.6%




2.2%






Compression: 1″d (psi)




4116 4452




4382 4933




3784 3786






Heat Age Rating




2




3
















Components Wt %




Sample No. 65




66









Part A






Epon 828




42.8




50.4






Erisys GE-29




12.8




4.2






Micropearls F30D




12.8




10.8






BK 5799 (carbon black)




4 g




4 g






Part B






Santicizer 97




17.6




18






Santicizer 154




4.4




4.5






H


3


PO


4


(>85% conc)




13.2




11.2






Initial Rxn Time




25 sec




30 sec






% Ht Expansion




287%




275%






Density (g/in


3


)






Top





3.72






Bot






H


2


O Absorption




34%






Shore A: Initial




45




71






Shore A: Water Soak




14






Shore A % Drop After Water Soak




69%






Shrinkage




0.5%




0.2%






Flammability (vert)




Torch




Torch






Flame Time




3 sec




7 sec






Burn Length




0.06-0.19 in




3.75-7 in






Flammability (horiz)




Torch




Torch






Flame Time




5 sec




6 sec






Burn Length




3.25-3.75 in



















A skilled person in this art would understand that these exemplary processes an be modified by manipulating process variables such as time and temperature of each aforementioned mixing step, mixing rate (RPM), time under vacuum, radiation source (e.g., UV light) and length of exposure and distance from source, and level of vacuum (mm Hg) as well as operating a continuous process. While the above Examples illustrate a batch process a skilled person in this art after having reviewed and understood the instant disclosure, would be capable of manipulating the aforementioned process variables to tailor the instant composition for a virtually unlimited array of product applications.




While the present invention has been described in certain preferred embodiments thereof, it will be apparent that various substitution, omissions, modifications, and other changes which may be made without departing from the spirit of the invention. Thus, the present invention should be limited only by the scope of the following claims including equivalents thereof.



Claims
  • 1. A foam precursor comprising:(a) an A-side foam precursor composition comprising at least halogenated epoxy functional compound, and a blowing agent, and; (b) a B-side foam precursor composition comprising an acid source and at least one dialkyl adipate; wherein at least one of said foam precursors is encapsulated.
  • 2. The foam precursor according to claim 1 wherein (a) further includes a modifying material.
  • 3. The foam precursor according to claim 1 wherein (b) further comprises a carrier material.
  • 4. The foam precursor of claim 1 wherein said blowing agent comprises an encapsulated blowing agent and the encapsulated blowing agent has at least two different activation temperatures.
  • 5. The foam precursor of claim 1 wherein the encapsulated blowing agent comprises a thermoplastic shell that contains at least one of isobutane and isopentane blowing agent.
  • 6. The foam precursor of claim 1 wherein at least one of the A-side precursor and the B-side precursor further comprises castor oil, at least one benzyl phthalate and at least one member selected from the group consisting of Bis A epoxy and Bis F epoxy.
  • 7. The foam precursor of claim 1 wherein said epoxy compound is a bis-A or bis-F epoxy compound; the blowing agent comprises at least one of isopentane and isobutane and the A-side precursor further comprises at least one member selected from the group consisting of polypropylene, polyethylene and polyvinyl alcohol.
  • 8. A method for producing a foam comprising:(a) combining an A-side foam precursor comprising at least one epoxy functional compound with a B-side foam precursor comprising at least one hydrogen donating Lewis acid and at least one dialkyl adipate, wherein at least one of said A-side and B-side comprise an encapsulated blowing agent, under conditions sufficient to provide an exothermic reaction within less than about 2 minutes from said combining; and (b) utilizing heat from the exothermic reaction so as to expand the combined components to form a foam.
  • 9. The method of claim 8 wherein said at least one hydrogen donating Lewis acid comprises phosphoric acid.
  • 10. The method of claim 9 wherein said phosphoric acid is substantially water free.
  • 11. The method of claim 8 wherein said combining comprises dispensing through a mixing device comprising a static mix head.
  • 12. The method of claim 8 wherein the combined A-side and B-side are dispensed into a containment device.
  • 13. The method of claim 11 wherein said static mix head is affixed in a manner to substantially seal a cavity into which the foam is dispensed.
CROSS REFERENCE TO RELATED PATENT APPLICATIONS

This is a continuation-in-part of U.S. patent application Ser. No. 09/344,198, filed on Jun. 24, 1999 as a continuation in part of U.S. Ser. No. 09/300,930, filed on Apr. 28, 1999, that is a continuation in part of Ser. No. 09/197,124, filed on Nov. 20, 1998, that is a continuation-in-part of Ser. No. 09/081,967, filed on May 20, 1998 and entitled “Novel Foaming Compositions and Methods For Making and Using the Composition”. The disclosure of these prior filed patent applications is hereby incorporated by reference. The subject matter herein claims benefit under 35 U.S.C. 111(a), 35 U.S.C. 119(e) and 35 U.S.C. 120 of U.S. Provisional Patent Application Ser. No. 60/047,273, filed on May 21, 1997, entitled “A Room Temperature Foaming Composition”; and U.S. Provisional Patent Application Ser. No. 60/079,205, filed on Mar. 24, 1998, entitled “Novel Foaming Compositions and Methods For Making and Using the Compositions”. The disclosure of the aforementioned Provisional Patent Applications is hereby incorporated by reference. The subject matter of the instant invention is also related to non-provisional patent application Ser. Nos. 09/081,966, filed on May 20, 1998 and Ser. No. 09/197,107, filed Nov. 20, 1999, both filed in the name of Jeffrey Pachl et al., and entitled “Curable Sealant Composition”. The disclosure of these Non-provisional patent applications is hereby incorporated by reference.

US Referenced Citations (3)
Number Name Date Kind
3154504 Carey et al. Oct 1964 A
4923902 Wycech May 1990 A
5274006 Kagoshima et al. Dec 1993 A
Provisional Applications (2)
Number Date Country
60/047273 May 1997 US
60/079205 Mar 1998 US
Continuation in Parts (4)
Number Date Country
Parent 09/344198 Jun 1999 US
Child 09/578206 US
Parent 09/300930 Apr 1999 US
Child 09/344198 US
Parent 09/197124 Nov 1998 US
Child 09/300930 US
Parent 09/081967 May 1998 US
Child 09/197124 US