Formulations including improved organoclay compositions

BACKGROUND OF THE INVENTION
This invention relates generally to organoclays, and, more specifically, to improved organoclays which are produced by the reaction of the organoclay with an alkoxylated quaternary ammonium compound.
Organoclays, representing the reaction product of a smectite clay with a quaternary ammonium compound, have long been known for use in gelling of organic liquids such as lubricating oils, linseed oil, toluene and the like. A large variety of highly useful products, such as lubricating greases, are producible through use of such gelling agents. The procedures and chemical reactions pursuant to which these organoclays are prepared, are well-known. Thus, under appropriate conditions, the organic compound which contains a cation, will react by ion exchange with the clay which contains a negative layer lattice and exchangeable cations to form the organoclay products.
Other uses for such modified organoclays are those such as are disclosed in U.S. Pat. No. 5,151,155, wherein organically modified smectite clays are utilized in a process for deinking wastepaper, and in U.S. Pat. No. 4,677,158, wherein smectite-type clays which have been reacted with quaternary ammonium compounds are utilized as thickeners for aqueous suspensions, particularly latex paints and caulks. These modified organoclays differ from those of the present invention in the type of quaternary ammonium compound with which they are reacted. This modification produces organoclays with markedly superior properties than those of the prior art.
OBJECTS OF THE INVENTION
It is an object of the present invention to prepare organoclay compositions having improved rheological properties, and thus useful as thixotropes in aqueous compositions.
It is further an object of the present invention to prepare improved aqueous compositions, especially paint formulations, which possess improved properties by virtue of their inclusion of the organoclay compositions of the present invention.
SUMMARY OF THE INVENTION
In accordance with the present invention, it has unexpectedly been discovered that the reaction of smectite clays with certain alkoxylated quaternary ammonium compounds can produce organoclay products having superior properties when utilized as water-based thixotropes.
Thus, the present invention is concerned with an organoclay composition comprising the reaction product of a smectite clay having an ion exchange capacity of at least 50 meq. wt. per 100 g. clay (active basis), and an alkoxylated quaternary ammonium compound having the following formula: ##STR1## wherein R.sub.1 and R.sub.2 are alike or different, and are selected from the group consisting of C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl groups; R.sub.3 is a C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl group, or an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles of an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide, and mixtures thereof; and R.sub.4 is an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles of an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide, and mixtures thereof; and X is the salt anion.

DESCRIPTION OF PREFERRED EMBODIMENTS
The smectite clays which are utilized as one of the starting materials of the present invention are those which have been conventionally utilized in the prior art. Suitable smectite clays are those which have a cation exchange capacity of at least 50 milliequivalents (meq.) weight (wt.) per 100 grams of clay (active basis). Useful clays for such purposes include the naturally occurring Wyoming variety of swelling bentonite and similar clays, and hectorite, which is a swelling magnesium-lithium silicate clay. The clays are preferably converted to the sodium form if they are not already in this form. This can be effected, again as in known in the art, by a cation exchange reaction, or the clay can be converted via an aqueous reaction with a soluble sodium compound.
Smectite clays prepared synthetically can also be utilized, such as montmorillonite, bentonite, beidelite, hectoritesaponite, and stevensite. Such clays, and processes for their preparation, are described in U.S. Pat. Nos. 4,695,402, 3,855,147, 3,852,405, 3,844,979, 3,844,978, 3,671,190, 3,666,407, 3,586,478, and 3,252,757, all of which are herein incorporated by reference.
The alkoxylated quaternary ammonium salts which are reacted with the smectite clay are of the formula ##STR2## wherein R.sub.1 and R.sub.2 are alike or different, and are selected from the group consisting of C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl groups; R.sub.3 is a C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl group, or an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide and mixtures thereof; and R.sub.4 is an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles of an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide and mixtures thereof; and X is the salt anion.
The salt anion X is methosulfate, ethosulfate, methylcarbonate, ethylcarbonate, chloride, bromide, or mixtures thereof, and is most preferably a methosulfate ion. The salt anion may also, however, be nitrate, hydroxide, acetate, or mixtures of these.
The alkoxylated chains present in the alkoxylated quaternary ammonium compounds of the present invention determine the particularly advantageous properties of the resultant organoclays of the present invention. Thus, the prior art organoclays which contain saturated alkyl groups in the quaternary ammonium compound provide modified organoclays which are too hydrophobic to be useful in aqueous systems. Likewise, the use of the prior art polyethoxylated chain quaternary ammonium compounds provide modified organoclays which are too hydrophilic and which provide organoclays which are difficult to de-water during processing steps. It is thus critical to the present invention to provide quaternary ammonium compounds which, upon reaction with the smectite clay, will afford an organoclay composition having the desired hydrophobic/hydrophilic balance, resulting in desirable properties in the end-products.
Preferred embodiments of the present invention will utilize quaternary ammonium compounds having one or two alkoxylated chains each containing 1-5 moles ethylene oxide and 4-10 moles propylene oxide and/or butylene oxide moieties.
Highly preferred embodiments of the present invention are organoclays which comprise the reaction product of smectite clays with alkoxylated quaternary ammonium compounds wherein the R.sub.3 and R.sub.4 chains each contain the moiety of 5 moles ethylene oxide and 5 moles propylene oxide, and are thus represented by the following formula:
(CH.sub.3).sub.2 N�(CH.sub.2 CH.sub.2 O).sub.x (CH.sub.2 CH(CH.sub.3)O.sub.y !.sub.2 H
wherein x and y=5
or wherein R.sub.3 and R.sub.4 each contain the moiety of 1 mole of ethylene oxide and 4 moles of propylene oxide, represented by the formula:
(CH.sub.3)2N�(CH.sub.2 CH.sub.2 O).sub.x (CH.sub.2 CH(CH.sub.3)(O).sub.y !.sub.2 H
wherein x and y=4
or wherein R.sub.3 and R.sub.4 each contain the moiety of 1 mole ethylene oxide and 5 moles each of propylene oxide and butylene oxide, represented by the formula:
(CH.sub.3).sub.2 N�(CH.sub.2 CH.sub.2 O).sub.x (CH.sub.2 CH(CH.sub.3)O).sub.y (CH.sub.2 CH(CH.sub.2 CH.sub.3)O).sub.z !.sub.2 H
wherein x=1, y=5 and z=2
Other preferred embodiments of the invention involve the reaction product of a smectite clay with an alkoxylated quaternary ammonium compound wherein R.sub.1, R.sub.2 and R.sub.3 are each a methyl group and R.sub.4 is an alkoxylated chain containing 1 mole ethylene oxide and 9 moles propylene oxide represented by the formula:
(CH.sub.3).sub.3 N�(CH.sub.2 CH.sub.2 O).sub.x (CH.sub.2 CH(CH.sub.3)O).sub.y !H
wherein x=1 and y=9
or when R.sub.4 is an alkoxylated chain containing 1 mole ethylene oxide, 5 moles propylene oxide and 5 moles of butylene oxide represented by the formula:
(CH.sub.3).sub.3 N�(CH.sub.2 CH.sub.2 O).sub.x (CH.sub.2 CH(CH.sub.3)O).sub.y (CH.sub.2 CH(CH.sub.2 CH.sub.3)O).sub.z !H
wherein x=1, y=5 and z=5.
x, y and z when employed herein denote relative reactive molar ratios and the reaction products generally represent a product distribution centered around these ratios. Other quaternary ammonium salts which are particularly useful in the present invention are described in the U.S. Pat. Nos. 3,123,641, 4,144,122, 4,432,833 and 5,296,627, which are incorporated herein by reference.
The alkoxylated quaternary ammonium compounds useful in the present invention of the present invention can be prepared by various methods known by those of ordinary skill in the art. In a preferred method, the quaternary ammonium compound is prepared by the reaction of a tertiary amine and an alkylating agent. Some alkylating agents, well known to those practicing the art, include organic halides such as methyl chloride, diorganosulfates such as dimethyl sulfate, or diorgano carbonates, such as dimethyl carbonate. This method of preparation is described in ENCYCLOPEDIA OF CHEMICAL TECHNOLOGY edited by Kirk/Othmer (Third Edition, Vol 19, page 521-531) which is incorporated herein by reference.
The tertiary amine, useful in preparing the quaternary ammonium salt, is preferably a polyalkoxylated amine produced by reacting ammonia, a primary amine, or a secondary amine with an alkoxylating agent. Suitable alkoxylating agents include alkyl epoxides such as ethylene oxide, propylene oxide, and butylene oxide. Tertiary polyalkoxylated amines which can also be employed in the present invention are prepared by reacting ammonia, a primary amine, or a secondary amine with a polyalkoxylated alcohol or polyalkoxylated glycol. Especially useful tertiary amines may also be made by alkylating a primary, or secondary alkoxylated amine, such as the available JEFFAMINE.RTM. series of alkoxylated amines available from Huntsman Chemicals (JEFFAMINE.RTM. is a registered mark of Huntsman Chemicals Inc.) or the available TECTRONIC.RTM. series of alkoxylated amines available form BASF Corporation (TECTRONIC.RTM. is a registered trademark of BASF Corporation). Examples of other tertiary amines useful in the present invention can be found in U.S. Pat. Nos. 3,654,370, 4,739,094, 4,960,942, 4,967,005, 5,344,984 and 5,347,051, which are incorporated herein by reference.
The amount of the alkoxylated quaternary ammonium compound reacted with the smectite clay depends upon the specific clay and the desired degree of hydrophobicity. Typically, the amount of cation ranges from about 0.1 to about 150%, preferably from about 100 to about 130% of the cation exchange capacity of the clay. Thus, for example, when bentonite is used, the amount of cation reacted with the clay will range from about 85 to about 143 milliequivalents, preferably from about 95 to about 124 milliequivalents per 100 grams of clay, 100% active basis.
A further embodiment of the present invention is the process for preparing the organoclay composition comprising the reaction product of a smectite clay having an ion exchange capacity of at least 50 meq. wt. per 100 g. clay (active basis), and an alkoxylated ammonium compound of the formula: ##STR3## wherein R.sub.1 and R.sub.2 are alike or different, and are selected from the group consisting of C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl groups; R.sub.3 is a C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl group, or an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles of an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide and mixtures thereof; and R.sub.4 is an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles of an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide and mixtures thereof; and X is the salt anion; which comprises:
a) dispersing of a smectite clay having an ion exchange capacity of at least 50 meq. wt. per 100 g. clay in an aqueous media;
b) heating the dispersion of step (a) to a temperature in excess of 30.degree. C;
c) adding the heated dispersion of step (b) of a quaternary ammonium salt of the formula ##STR4## wherein R.sub.1 and R.sub.2 are alike or different, and are selected from the group consisting of C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl groups; R.sub.3 is a C.sub.1 -C.sub.8 alkyl, benzyl or 2-hydroxyethyl group, or an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide and mixtures thereof; and R.sub.4 is an alkoxylated chain containing 0-10 moles ethylene oxide and 3-15 moles of an alkylene oxide moiety selected from the group consisting of propylene oxide, butylene oxide and mixtures thereof; and X is the salt anion, in the desired milliequivalent ratio; and
d) agitating of the mixture of step (c) to effect completion of the reaction.
The organoclay composition of the present invention is thus prepared by admixing an aqueous dispersion of the smectite clay, warmed to a temperature in excess of 30.degree. C., with an alkoxylated quaternary ammonium compound of formula I to exchange the metal counterions that are naturally present in the smectite clay. The reaction is typically conducted at a temperature within the range of from about 40.degree. C. to about 100.degree. C. for a period of time sufficient for the alkoxylated quaternary ammonium compound to react with the clay particles. Preferably, the clay is dispersed in the water at a concentration from about 3% to about 15% by weight and the slurry is centrifuged to remove non-clay impurities. The slurry is then agitated and heated to the desired temperature, and the quaternary ammonium salt added in the desired milliequivalent ratio. The alkoxylated quaternary ammonium compounds are typically liquids, but they can be dispersed in water to facilitate the reaction. Agitation is continued to effect completion of the reaction.
The amount of the alkoxylated quaternary ammonium compound added to the smectite clay for the purposes of this invention must be sufficient to impart to the clay the enhanced characteristics desired. The milliequivalent ratio is defined as the number of milliequivalents of the alkoxylated quaternary ammonium compound, per 100 grams of clay, 100% active basis. The typical smectite clays of this invention have a milliequivalent ratio of from about 10 to about 150. The preferred milliequivalent ratio will vary depending on the characteristics of the particular alkoxylated quaternary ammonium compound utilized and the end use for the resultant product.
When the organoclay composition of the present invention is utilized for its rheological properties for application as to control sagging of fluid films and prevent settling and hard packing of pigments present in paint compositions, particularly latex paint compositions, it is typically employed in an amount of about 5 lb. to about 95 lb./100 gallons paint composition.
The present invention thus contemplates the preparation of latex paint formulations having improved properties which comprise the addition of the improved organoclay composition which is the reaction product of a smectite clay having an ion exchange capacity of at least 50 meq. wt. per 100 g. clay and an alkoxylated quaternary ammonium compound of the general formula I. Typically, the latex paint formulation will contain the improved organoclay composition in an amount of about 2 to about 10% by weight of the finished latex paint formulation. Preferred formulations contain the organoclay thixotrope in an amount of about 3 to about 6% by weight of the finished latex paint formulation.
Latex paint formulations containing the organoclay composition of the instant invention exhibit superior characteristics when brush out, roll out and spray out applications were compared with standard commercially available latex paint formulations. The latex paints formulated using the organoclay compositions exhibited a high low-shear viscosity and a low high-shear viscosity in contrast to the commercial paints which exhibited lower low-shear values and higher high-shear values. When sheared, theses latex paint formulations thinned out to a flowable and workable viscosity. The low high-shear viscosity of the these latex paints results in excellent atomization in airless spray application. In addition, the presence of the organoclay in the latex paint formulations improved the sag characteristics of these paints to such a degree that sprayouts of thirty mils or higher were common.
The invention will now be illustrated by a series of Examples, which are intended to set forth typical and preferred procedures to be utilized in the practice of the invention.
EXAMPLE 1
The preparation of a smectite clay composition comprising the reaction product of a smectite clay and a quaternary ammonium compound of the formula I wherein the R.sub.1 and R.sub.2 are each a methyl group and the R.sub.3 and R.sub.4 chains each contain the moiety of 5 moles ethylene oxide and 5 moles propylene oxide is prepared as follows:
5000 Grams of an aqueous three pass slurry of montmorillonite SCPX 818 containing 3.72 % solids in a 5 gallon tank is heated on a lightening mixer to 60.degree. C. (140.degree. F).d To this heated slurry is then added 87.19 grams of the alkoxylated quaternary ammonium compound of formula I wherein the R.sub.1 and R.sub.2 are each a methyl group and the R.sub.3 and R.sub.4 chains each contain the moieties of 5 moles ethylene oxide and 5 moles propylene oxide (AKR 94005 Lot #94016RS-T) at 30 MER, which mixture is then stirred for fifteen minutes until the clay swells and mixing is no longer possible. After transfer to a quart jar, no separation was observed after twenty-four hours, indicating completion of the reaction.
This was calculated 5.03% solids
255.89 grams dry clay
EXAMPLE 2
The preparation of a smectite clay composition comprising the reaction product of a smectite clay and a quaternary ammonium compound of the formula I wherein the R.sub.1 and R.sub.2 are each a methyl group and the R.sub.3 and R.sub.4 chains each contain the moiety of 1 mole ethylene oxide and 5 moles propylene oxide is prepared as follows:
5000 Grams of an aqueous three pass slurry of montmorillonite SCPX 818 containing 3.72 % solids in a 5 gallon tank is heated on a lightening mixer to 60.degree. C. (140.degree. F). To this heated slurry is then added 43.6 grams of the alkoxylated quaternary ammonium of formula I wherein the R.sub.1 and R.sub.2 are each a methyl group and the R.sub.3 and R.sub.4 chains each contain the moiety of 1 mole ethylene oxide and 5 moles propylene oxide (ARK 94006 Lot #94016RS-T) at 20 MER, which mixture is then stirred for fifteen minutes until the clay swells and mixing is no longer possible. After transfer to a quart jar, no separation was observed after twenty-four hours, indicating completion of the reaction.
This was calculated 4.38% solids
220.91 grams dry clay
EXAMPLE 3
A latex paint formulation consisting of:
______________________________________Volume Material Weight______________________________________5.85 SM/OC CEP/HRD Thixotrope prepared as in 49.70 Example 114.42 Water 120.300.09 Troysan 142-Bacteriostat 1.000.65 Tamol 731 6.000.05 Potassium Tripolyphosphte 1.000.34 Triton N-101 3.000.13 AMP-95 1.002.55 Propylene Glycol 22.000.27 Bubble Breaker 748 2.00Procedure for preparation: Add together the following and mix:5.09 TIO2 CR-800 175.004.42 No. 1 White 100.003.56 Snowflake White 80.007.99 ECCA Tex 90 175.00 Disperse to 5+ Hegman 3400 RPM, 15 m. Dispermat16.61 Water 138.500.27 Bubble Breaker 748 2.005.85 SM/OC CEP/HRD Thixotrope prepared as in 49.70 Example 11.14 Texanol 9.00Then, mix and add:31.27 UCAR 376 Latex 283.00Check the following specs:Viscosity, KU 95ICI, Poise 0.8BF 1 66,800 10 10,520100 1,904Leneta Sag 12Leneta Leveling 3Final pH 8.16Weight/Gallon 11.95Syneresis 120/10D 1-2%Syneresis Ambient --______________________________________
EXAMPLE 4
A latex paint formulation consisting of:
______________________________________Volume Material Weight______________________________________8.19 SM/OC CEP/HRD Thixotrope prepared as in 69.58 Example 112.04 Water 100.420.09 Troysan 142-Bacteriostat 1.000.65 Tamol 731 6.000.05 Potassium Tripolyphosphte 1.000.34 Triton N-101 3.000.13 AMP-95 1.002.55 Propylene Glycol 22.000.27 Bubble Breaker 748 2.00Procedure for preparation: Add together and mix the following:5.09 TIO2 CR-800 175.004.42 No. 1 White 100.003.56 Snowflake White 80.007.99 ECCA Tex 90 175.00 Disperse to 5+ Hegman 3400 RPM, 15 m. Dispermat14.22 Water 118.620.27 Bubble Breaker 748 2.008.19 SM/OC CEP/HRD Thixotrope prepared as in 69.58 Example 11.14 Texanol 9.00Then, mix and add:31.27 UCAR 376 Latex 283.00Check the following specs:Viscosity, KU 126ICI, Poise 1.0BF 1 82,000 10 28,100100 5,710Leneta Sag 724Leneta Leveling 1Final pH 8.14Weight/Gallon 11.96Syneresis 120/10D 1-2%Syneresis Ambient --______________________________________
EXAMPLE 5
A latex paint formulation consisting of:
______________________________________Volume Material Weight______________________________________5.40 SM/OC CEP/HRD Thixotrope prepared as in Ex. 2 45.6614.91 Water 124.340.09 Troysan 142-Bacteriostat 1.000.65 Tamol 731 6.000.05 Potassium Tripolyphosphte 1.000.34 Triton N-101 3.000.13 AMP-95 1.002.55 Propylene Glycol 22.000.27 Bubble Breaker 748 2.00Procedure for preparation: Add the following ingredients together andmix:5.09 TIO2 CR-800 175.004.42 No. 1 White 100.003.56 Snowflake White 80.007.99 ECCA Tex 90 175.00 Disperse to 5+ Hegman 3400 RPM, 15 m. Dispermat17.09 Water 142.540.27 Bubble Breaker 748 2.005.40 SM/OC CEP/HRD Thixotrope prepared as in Ex. 2 45.661.14 Texanol 9.00Then, mix and add:31.27 UCAR 376 Latex 283.00Check the following specs:Viscosity, KU 94ICI, Poise 0.8BF 1 68,800 10 11,560100 2,028Leneta Sag 12Leneta Leveling 3-4Final pH 8.19Weight/Gallon 11.96Syneresis 120/10D 1-2%Syneresis Ambient --______________________________________
EXAMPLE 6
A latex paint formulation consisting of the following:
______________________________________Volume Material Weight______________________________________8.11 SM/OC CEP/HRD Thixotrope prepared in Ex. 2 68.4912.17 Water 101.510.09 Troysan 142-Bacteriostat 1.000.65 Tamol 731 6.000.05 Potassium Tripolyphosphte 1.000.34 Triton N-101 3.000.13 AMP-95 1.002.55 Propylene Glycol 22.000.27 Bubble Breaker 748 2.00Procedure for preparation: Add the following together and mix:5.09 TIO2 CR-800 175.004.42 No. 1 White 100.003.56 Snowflake White 80.007.99 ECCA Tex 90 175.00 Disperse to 5+ Hegman 3400 RPM, 15 m. Dispermat14.35 Water 119.710.27 Bubble Breaker 748 2.008.11 SM/OC CEP/HRD Thixotrope prepared in Ex. 2 68.491.14 Texanol 9.00Then, mix and add:31.27 UCAR 376 Latex 283.00Check the following specs:Viscosity, KU 102ICI, Poise 0.9BF 1 72,400 10 16,400100 3,076Leneta Sag 16Leneta Leveling 2Final pH 8.17Weight/Gallon 11.95Syneresis 120/10D 1-2%Syneresis Ambient --______________________________________
EXAMPLE 7
A latex paint formulation consisting of:
______________________________________Volume Material Weight______________________________________20.00 SM/OC CEP/HRD Thixotrope prepared as in 170.00 Example 20.09 Troysan 142-Bacteriostat 1.000.65 Tamol 731 6.000.05 Potassium Tripolyphosphte 1.000.23 Triton N-101 2.000.13 AMP-95 1.002.55 Propylene Glycol 22.000.27 Bubble Breaker 748 2.00Procedure for preparation: Add together the following and mix:5.47 TIO2 CR-813 175.004.42 No. 1 White 100.007.99 Satintone white 175003.46 Minex 7 75.00 Disperse to 5+ Hegman 3400 RPM, 15 m. Dispermat1.73 Water 14.400.27 Bubble Breaker 748 2.0020.00 SM/OC CEP/HRD Thixotrope prepared as in 170.00 Ex. 21.14 Texanol 9.00Then, mix and add:31.27 UCAR 376 Latex 283.00______________________________________
EXAMPLE 8
A latex paint formulation consisting of:
______________________________________Volume Material Weight______________________________________40.00 SM/OC CEP/HRD Thixotrope prepared as in 340.00 Example 2 Thixotrope load adjusted on a dry solids basis (Thix. + water = 170.0 grams)0.09 Troysan 142-Bacteriostat 1.000.65 Tamol 731 6.000.05 Potassium Tripolysphosphte 1.000.34 Triton N-101 3.000.13 AMP-95 1.002.55 Propylene Glycol 22.000.27 Bubble Breaker 748 2.00Procedure for preparation: Add together the following and mix:5.09 TIO2 CR-800 175.004.42 No. 1 White 100.003.56 Snowflake white 80.007.99 ECCA TEX 90 175.00 Disperse to 5+ Hegman 3400 RPM, 15 m. Dispermat2.18 Water 18.200.27 Bubble Breaker 748 2.001.14 Texanol 9.00Then, mix and add:31.27 UCAR 376 Latex 283.00______________________________________
EXAMPLE 9
Comparison of Paint Formulations
A. An aqueous slurry of non-exchanged montmorillonite added to paint at a rate of 6 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity 1 RPM (rotations per minute) 94,400 cps. 10 RPM 17,880 cps.100 RPM 2,884 cps.Krebs Stormer Viscosity 99 KUICI Cone and Plate Viscosity 0.9Leneta ChartSag Reading 10Leveling Reading 30pH 8.55Temp. C..degree. 23.6Pounds/Gallons 11.90 weight/gallonSyneresis Settling Rating 1.63120/10D %Scrub rating 94/152 106/152Brush Drag Rating 2.5-3Brush Out Rating Good Loading Poor LevelingRoller Splatter Rating 6Spray Out Rating Good Atomization at 12-14 mil.Roll Out Rating 2 Splatter Fine Texture______________________________________
B. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94005 (prepared as in Example 1, at 30 milliequivalence/100 grams montmorillonite) added to the same paint as A at 7 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity 1 RPM (rotations per minute) 80,000 cps. 10 RPM 14,400 cps.100 RPM 2,628 cps.Krebs Stormer Viscosity 97 KUICI Cone and Plate Viscosity 0.8Leneta ChartSag Reading 8Leveling Reading 4pH 8.57Temp. C..degree. 23.7Pounds/Gallons 11.92 weight/gallonSyneresis Settling Rating 1.2120/10D %Scrub Rating 115/188 148/211Brush Drag Rating 2Brush Out Rating Good Loading Poor LevelingRoller Splatter Rating 6-7Spray Out Rating Good Atomization at 20 mils.Roll Out Rating 5 Splatter Med Texture______________________________________
C. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94006 (prepared as in Example 2 at 20 milliequivalence/100 grams montmorillonite added to the same paint as A at 6 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity 1 RPM (rotations per minute) 92,000 cps. 10 RPM 19,400 cps.100 RPM 3,648 cps.Krebs Stormer Viscosity 109 KUICI Cone and Plate Viscosity 0.9Leneta ChartSag Reading 10Leveling Reading 4pH 8.61Temp. C..degree. 23.5Pounds/Gallons 11.95 weight/gallonSyneresis Settling Rating 1.65120/1OD %Scrub Rating 101/136 101/152Brush Drag Rating 3Brush Out Rating OK Loading Poor LevelingRoller Splatter Rating 8Spray Out Rating Good Atomization at 18 mils.Roll Out Rating 5 Splatter Coarse Texture______________________________________
D. An aqueous slurry of non-exchanged montmorillonite added to paint at a rate of 6 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 104,000 cps.10 RPM 28,400 cps.100 RPM 4.470 cps.Krebs Stormer Viscosity 115 KUICI Cone and Plate Viscosity 0.9Leneta ChartSag Reading 14Leveling Reading 1-2pH 8.17Temp. C.degree. 22.6Pounds/Gallons 11.77 weight/gallonSyneresis Settling Rating120/10 D % 1.85Scrub Rating 166/200 137/216Brush Drag Rating 2.5Brush Out Rating Good LoadingRoller Splatter Rating 7-8Spray Out Rating Good Atomization at 16 mils.Roll Out Rating 4 Splatter Fine Texture______________________________________
E. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94005 (prepared as in Example 1, at 30 milliequivalence/100 grams montmorillonite) added to the same paint as D at 7 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 81,600 cps.10 RPM 16,360 cps.100 RPM 2,840 cps.Krebs Stormer Viscosity 101 KUICI Cone and Plate Viscosity 0.8Leneta ChartSag Reading 8-9Leveling Reading 3pH 8.24Temp. C.degree. 22.6Pounds/Gallons 11.95 weight/gallonSyneresis Settling Rating120/10 D % 1.79Scrub Rating 154/183 122/159Brush Drag Rating 2.5-3Brush Out Rating Good LoadingRoller Splatter Rating 8Spray Out Rating Good Atomization at 17 mils.Roll Out Rating 2 Splatter Fine Texture______________________________________
F. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94005 (prepared as in Example 1, at 30 milliequivalence/100 grams montmorillonite) added to the same paint as D at 8 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 127,000 cps.10 RPM 34,260 cps.100 RPM 6,280 cps.Krebs Stormer Viscosity 132 KUICI Cone and Plate Viscosity 1.1Leneta ChartSag Reading 16Leveling Reading 1pH 8.21Temp. C.degree. 22.8Pounds/Gallons 11.84 weight/gallonSyneresis Settling Rating120/10 D % 1.32Scrub Rating 137/154 103/167Brush Drag Rating 2.5-3Brush Out Rating Good LoadingRoller Splatter Rating 9Spray Out Rating Good Atomization at 18 mils.Roll Out Rating 5 Splatter Fine Texture______________________________________
G. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94006 (prepared as in Example 2 at 20 milliequivalence/100 grams montmorillonite) added to the paint at 6 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 130,000 cps.10 RPM 27,000 cps.100 RPM 4,640 cps.Krebs Stormer Viscosity 118 KUICI Cone and Plate Viscosity 0.9Leneta ChartSag Reading 12-13Leveling Reading 2pH 8.18Temp. C.degree. 22.7Pounds/Gallons 11.90 weight/gallonSyneresis Settling Rating120/10 D % 1.67Scrub Rating 165/197 177/208Brush Drag Rating 2.5-3Brush Out Rating Good LoadingRoller Splatter Rating 8-9Spray Out Rating Good Atomization at 20 mils.Roll Out Rating 2 Splatter Medium Texture______________________________________
H. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94006 (prepared as in Example 2 at 20 milliequivalence/100 grams montmorillonite) added to the paint at 6 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 81,000 cps.10 RPM 23,100 cps.100 RPM 4,290 cps.Krebs Stormer Viscosity 114 KUICI Cone and Plate Viscosity 0.9Leneta ChartSag Reading 12Leveling Reading 2-3pH 8.30Temp. C.degree. 22.6Pounds/Gallons 11.88 weight/gallonSyneresis Settling Rating120/10 D % 1.72Scrub Rating 182/236 170/220Brush Drag Rating 3Brush Out Rating OK LoadingRoller Splatter Rating 7-8Spray Out Rating Good Atomization at 25-30 mils.Roll Out Rating 3 Splatter Medium Texture______________________________________
I. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94006 (prepared as in Example 2 at 20 milliequivalence/100 grams montmorillonite) added to the paint at 7 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 121,000 cps.10 RPM 37,400 cps.100 RPM 6,900 cps.Krebs Stormer Viscosity 136 KUICI Cone and Plate Viscosity 1.1Leneta ChartSag Reading 18Leveling Reading 1pH 8.23Temp. C.degree. 22.5Pounds/Gallons 11.81 weight/gallonSyneresis Settling Rating120/10 D % 1.61Scrub Rating 145/196 157/196Brush Drag Rating 3.5Brush Out Rating Ex. LoadingRoller Splatter Rating 8-9Spray Out Rating Good Atomization at 18 mils.Roll Out Rating 5 Splatter Medium Texture______________________________________
J. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94005 (prepared as in Example 1 at 30 milliequivalence/100 grams montmorillonite) added to the paint at 7 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 86,800 cps.10 RPM 17,880 cps.100 RPM 3,192 cps.Krebs Stormer Viscosity 100 KUICI Cone and Plate Viscosity 0.8Leneta ChartSag Reading 10Leveling Reading 3pH 8.48Temp. C.degree. 23.0Pounds/Gallons 11.90 weight/gallonSyneresis Settling Rating120/10 D % 1.61Scrub Rating 145/190 163/194Brush Drag Rating 2Brush Out Rating OK Loading EasyRoller Splatter Rating 9Spray Out Rating Good Atomization at 16 mils.Roll Out Rating 5 Splatter Rough Texture______________________________________
K. An aqueous slurry of montmorillonite exchanged with the quat ACAR 94006 (prepared as in Example 2 at 20 milliequivalence/100 grams montmorillonite) added to the paint at 5 dry lbs/100 gallons paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 76,000 cps.10 RPM 15,520 cps.100 RPM 2,680 cps.Krebs Stormer Viscosity 95 KUICI Cone and Plate Viscosity 0.8Leneta ChartSag Reading 10Leveling Reading 4pH 8.32Temp. C.degree. 22.7Pounds/Gallons 11.89 weight/gallonSyneresis Settling Rating120/10 D % 2.42Scrub Rating 131/197 160/200Brush Drag Rating 2Brush Out Rating Ex. Loading EasyRoller Splatter Rating 8Spray Out Rating Good Atomization at 19 mils.Roll Out Rating 2 Splatter Medium Splatter______________________________________
L. Benjamin Moore Contractor Flat Enhance Vinyl Latex paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 22,000 cps.10 RPM 6,960 cps.100 RPM 2,548 cps.Krebs Stormer Viscosity 102 KUICI Cone and Plate Viscosity 1.1Leneta ChartSag Reading 8Leveling Reading 5pH 8.50Temp. C.degree. 23.6Pounds/Gallons 12.14 weight/gallonSyneresis Settling Rating120/10 D % <1Scrub Rating 30/70 30/70Brush Drag Rating 4Brush Out Rating Good Loading Leveling OKRoller Splatter Rating 9Spray Out Rating Fair Atomization at 12 mils.Roll Out Rating 5 Splatter Leveling OK______________________________________
M. Benjamin Moore Regal Wall Satin paint was found to have the following characteristics:
______________________________________Brookfield Viscosity1 RPM (rotations per minute) 20,800 cps.10 RPM 4,500 cps.100 RPM 1,420 cps.Krebs Stormer Viscosity 87 KUICI Cone and Plate Viscosity 1.4Leneta ChartSag Reading 15Leveling Reading 7pH 7.54Temp. C.degree. 23.3Pounds/Gallons 10.82 weight/gallonSyneresis Settling Rating120/10 D % <1Scrub Rating 130/180 120/200Brush Drag Rating 2Brush Out Rating Good Loading Leveling OKRoller Splatter Rating 7Spray Out Rating Fair Atomization at 12 mils.Roll Out Rating 5 Splatter Leveling OK______________________________________
N. Benjamin Moore Contractor Flat with added paint was found to have the following characteristics:
______________________________________Krebs Stormer Viscosity 97 KUICI Cone and Plate Viscosity 1.5Leneta Chart 10Sag Reading______________________________________ Slight color change when comparing sealed leneta chart drawdown versus unsealed leneta chart drawdown.
O. Benjamin Moore paint with added tint was found to have the following characteristics:
______________________________________Krebs Stormer Viscosity 100 KUICI Cone and Plate Viscosity 1.4Leneta Chart 18Sag Reading______________________________________ Slight color change when comparing sealed leneta chart drawdown versus unsealed leneta chart drawdown.
P. Product of Example 2 with commercial antisplattering Associative Thickener (Rohm & Haas) agent added.
______________________________________ICI Cone and Plate Viscosity 1.2Roller Splatter Rating 8______________________________________
TEST METHODS
Sag and leveling were conducted on Leneta antisag bar and leneta leveling bar on leneta form 7B.

Number	Name	Date
3123641	Longley	Mar 1964
3252757	Granquist	May 1966
3586478	Neumann	Jun 1971
3654370	Yeakey	Apr 1972
3666407	Orlemann	May 1972
3671190	Neumann et al.	Jun 1972
3844978	Hickson	Oct 1974
3844979	Hickson	Oct 1974
3852405	Granquist	Dec 1974
3855147	Granquist	Dec 1974
4144122	Emanuelsson et al.	Mar 1979
4432833	Breese	Feb 1984
4677158	Tso et al.	Jun 1987
4695402	Finlayson et al.	Sep 1987
4739094	Mazanek et al.	Apr 1988
4960942	Gerkin et al.	Oct 1990
4967005	Smith	Oct 1990
5151155	Cody et al.	Sep 1992
5296627	Tang et al.	Mar 1994
5344984	Knifton et al.	Sep 1994
5347051	Sheehan et al.	Sep 1994

Formulations including improved organoclay compositions

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