Patent Application
20120183479
The present application relates to liquid or gel-like compositions comprising microencapsulated colorant granules.
Dyes have been included in detergent products either to provide product aesthetics, coloring of wash water or to increase perceived cleaning of white fabrics. Furthermore attempts have been made to incorporate particles comprising a dye into cleansing compositions which change color during use in order to indicate that sufficient time has elapsed and that a sufficient treatment with the cleansing composition has been achieved.
The choice of dye and the way to incorporate it in a composition should be carefully monitored to avoid spotting or staining of fabrics, skin, hair or hard surfaces after the treatment and/or to avoid the migration or the bleeding of the dye across the composition which may lead to a rather unattractive composition.
WO 2008/132616 discloses a composition comprising at least one thermo chromic dye, changing the color of the cleansing composition when the composition reaches a temperature of from about 21° C. to about 40° C. These color changing cleansing compositions are limited to thermo chromic dyes but do not indicate when a sufficient treatment with the cleansing compositions has been achieved.
Therefore, it was an object of the present invention to provide liquid or gel-like compositions such as cleansing products or personal care products which comprise an indicator for determining how long washing processes or applications should continue with the product in order to achieve a satisfying result. More particularly, a need currently exists for cleansing compositions that change color during use in order to indicate that a sufficient treatment with the cleansing compositions has been achieved.
Surprisingly it has now been found that this object is solved using pigments, which are converted to particular microencapsulated colorant granules. These pigments are suited to induce color to liquid or gel-like compositions during their application and in particular to the foam built-up during the washing process.
The present invention relates to liquid or gel-like compositions comprising one or more microencapsulated colorant granules consisting of a core (A) and a shell (B), whereby the core (A) has a diameter of between 1 and 1000 micrometer, preferably between 10 and 500 micrometer, more preferably between 100 and 400 micrometer, even more preferably between 200 and 300 micrometer, and comprises
a) a colorant (I),
b) microcrystalline cellulose,
c) a polyol;
and whereby the shell (B) has a thickness of between 1 to 500 micrometer, preferably between 10 and 400 micrometer, more preferably between 50 and 300 micrometer, even more preferably between 100 and 300 micrometer, and comprises
d) a polymer selected from the group consisting of polycarboxylic acids, copolymers of polycarboxylic acids, vinyl polymers, cellulose and cellulose derivatives.
Within the meaning of the present invention the term “liquid” means liquid at ambient conditions, i.e. at a temperature of 20° C. and a pressure of 1 atm (=1.013·105 Pa or 1013 hPa). Preferably, the liquid compositions according to the present invention have a viscosity of from 1 to 10 000 mPa·s. The viscosity is measured using the inventive liquid composition as such under the following conditions:
for measuring the viscosity in the range of from 1 to 250 mPa·s: temperature: 20° C.; apparatus: Brookfield RV 1; Spindle No. 1; 20 r.p.m. (rounds per minutes);
for measuring the viscosity in the range of from >250 to 500 mPa·s: temperature: 20° C.; apparatus: Brookfield RV 2; Spindle No. 2; 20 r.p.m. (rounds per minutes);
for measuring the viscosity in the range of from >500 to 5000 mPa·s: temperature: 20° C.; apparatus: Brookfield RV 3; Spindle No. 3; 20 r.p.m. (rounds per minutes);
for measuring the viscosity in the range of from >5000 to 10000 mPa·s: temperature: 20° C.; apparatus: Brookfield RV 4; Spindle No. 4; 20 r.p.m. (rounds per minutes).
Within the meaning of the present invention the term “gel-like” means gel-like at ambient conditions, i.e. at a temperature of 20° C. and a pressure of 1 atm (=1.013·105 Pa or 1013 hPa). Preferably, the gel-like compositions according to the present invention have a viscosity of from >10 000 to 200 000 mPa·s and particularly preferably of from 20 000 to 150 000 mPa·s. The viscosity is measured using the inventive gel-like composition as such under the following conditions: temperature: 20° C.; apparatus: Brookfield Viscosimeter RV; Spindle No. 7; 20 r.p.m. (rounds per minutes).
In one preferred embodiment of the invention the inventive compositions are liquid. In another preferred embodiment of the invention the inventive compositions are gel-like.
In a preferred embodiment of the invention, a white pigment (e), such as titanium dioxide (C.I. Pigment White 6), barium sulfate or zinc oxide, is incorporated into the shell. In this case the color of the core colorant (I) is hidden and the foam is to change from white to the color of colorant (I).
In a further preferred embodiment of the invention, the shell contains a colorant (II) (f) which color is different from the color of colorant (I). In this case, it is expedient to apply colorant (II) as a top-coat onto the shell containing components (d) and (e). Then, the color of the foam is to change from the color of colorant (II) to the color of colorant (I). It is preferred that the color of colorant (II) is equal or at least similar to the color of the cleansing base, so that the microencapsulated colorant granules are invisible or at least hardly visible in the inventive compositions.
In any embodiment of the invention, the core and the shell may contain some water not exceeding an amount for sustaining granular form, e.g. 0 to 50%, preferably 1 to 30%, more preferably 5 to 20%, by weight, based on the total weight of the granules.
In a preferred embodiment of the invention, the microencapsulated colorant granules contained in the inventive compositions contain
a) 5 to 60% by weight, preferably 10 to 40% by weight, of colorant (I),
b) 10 to 40% by weight, preferably 15 to 30% by weight, of microcrystalline cellulose,
c) 10 to 40% by weight, preferably 15 to 30% by weight, of polyol,
d) 0.1 to 20% by weight, preferably 1 to 10% by weight, of the polymer, relating to the total weight of the granules.
The amount of the white pigment (e) if any, may vary between 0 and 50%, preferably between 0.1 and 30%, by weight, relating to the total weight of the microencapsulated colorant granules.
The amount of colorant (II) (f), if any, may vary between 0 and 25%, preferably between 0.1 and 20% by weight, relating to the total weight of the microencapsulated colorant granules.
In a further preferred embodiment of the invention, the microencapsulated colorant granules contained in the inventive compositions contain
a) 5 to 60% by weight, preferably 10 to 40% by weight, of colorant (I),
b) 10 to 40% by weight, preferably 15 to 30% by weight, of microcrystalline cellulose,
c) 10 to 40% by weight, preferably 15 to 30% by weight, of polyol,
d) 0.1 to 20% by weight, preferably 1 to 10% by weight, of the polymer,
e) 0.1 to 30% by weight, preferably 1 to 20% by weight, of white pigment; and 1 to 30%, preferably 5 to 20%, by weight of water,
relating to the total weight of the granules.
In a further preferred embodiment of the invention, the microencapsulated colorant granules contained in the inventive compositions contain
a) 5 to 60% by weight, preferably 10 to 40% by weight, of colorant (I),
b) 10 to 40% by weight, preferably 15 to 30% by weight, of microcrystalline cellulose,
c) 10 to 40% by weight, preferably 15 to 30% by weight, of polyol,
d) 0.1 to 20% by weight, preferably 1 to 10% by weight, of the polymer,
e) 0.1 to 30% by weight, preferably 1 to 20% by weight, of white pigment;
f) 0.1 to 20% by weight, preferably 1 to 15% by weight, of colorant (II); and 1 to 30%, preferably 5 to 20%, by weight of water,
relating to the total weight of the granules.
The inventive compositions may be colored or upon application may result in a coloring (in case the compositions were colorless before their application) or may result in a color change of the composition itself. A similar coloring or color change may occur with respect to the foam resulting from the application of the inventive compositions. The coloring or color change of the inventive compositions and/or foam occurs independently of the temperature of the inventive compositions so that there is no need to use thermo chromic dyes as colorants. Therefore, it is preferred that colorant (I) and colorant (II) are not thermo chromic.
All color pigments from the group consisting of inorganic pigments, organic pigments and effect pigments come into consideration for use as colorant (I) and (II). By definition, pigments—in contradistinction to dyes—are virtually insoluble in the application medium.
Preferred organic pigments are monoazo, disazo, laked azo, β-naphthol, Naphthol AS, benzimidazolone, disazo condensation, azo metal complex pigments and polycyclic pigments such as, for example, phthalocyanine, quinacridone, perylene, perinone, thioindigo, anthanthrone, anthraquinone, flavanthrone, indanthrone, isoviolanthrone, pyranthrone, dioxazine, quinophthalone, isoindolinone, isoindoline and diketopyrrolopyrrole pigments.
Of the organic pigments mentioned, particularly suitable ones are in a very fine state of subdivision wherein preferably at least 95% by weight and more preferably at least 99% by weight of the pigment particles have a particle size ≦500 nm.
Advantageously, the pigment particles have a d50 value between 50 and 500 nm, preferably between 70 and 350 nm.
As an illustrative selection of particularly preferred organic pigments there may be mentioned monoazo and disazo pigments, more particularly the Colour Index pigments Pigment Yellow 1, Pigment Yellow 3, Pigment Yellow 12, Pigment Yellow 13, Pigment Yellow 14, Pigment Yellow 16, Pigment Yellow 17, Pigment Yellow 73, Pigment Yellow 74, Pigment Yellow 81, Pigment Yellow 83, Pigment Yellow 87, Pigment Yellow 97, Pigment Yellow 111, Pigment Yellow 126, Pigment Yellow 127, Pigment Yellow 128, Pigment Yellow 155, Pigment Yellow 174, Pigment Yellow 176, Pigment Yellow 191, Pigment Yellow 213, Pigment Yellow 214, Pigment Yellow 219, Pigment Red 38, Pigment Red 144, Pigment Red 214, Pigment Red 242, Pigment Red 262, Pigment Red 266, Pigment Red 269, Pigment Red 274, Pigment Orange 13, Pigment Orange 34 or Pigment Brown 41; β-naphthol and Naphthol AS pigments, more particularly the Colour Index pigments Pigment Red 2, Pigment Red 3, Pigment Red 4, Pigment Red 5, Pigment Red 9, Pigment Red 12, Pigment Red 14, Pigment Red 53:1, Pigment Red 112, Pigment Red 146, Pigment Red 147, Pigment Red 170, Pigment Red 184, Pigment Red 187, Pigment Red 188, Pigment Red 210, Pigment Red 247, Pigment Red 253, Pigment Red 256, Pigment Orange 5, Pigment Orange 38 or Pigment Brown 1; laked azo and metal complex pigments, more particularly the Colour Index pigments Pigment Red 48:2, Pigment Red 48:3, Pigment Red 48:4, Pigment Red 57:1, Pigment Red 257, Pigment Orange 68 or Pigment Orange 70; benzimidazoline pigments, more particularly the Colour Index pigments Pigment Yellow 120, Pigment Yellow 151, Pigment Yellow 154, Pigment Yellow 175, Pigment Yellow 180, Pigment Yellow 181, Pigment Yellow 194, Pigment Red 175, Pigment Red 176, Pigment Red 185, Pigment Red 208, Pigment Violet 32, Pigment Orange 36, Pigment Orange 62, Pigment Orange 72, Pigment Blue 80 or Pigment Brown 25; isoindolinone and isoindoline pigments, more particularly the Colour Index pigments Pigment Yellow 139 or Pigment Yellow 173; phthalocyanine pigments, more particularly the Colour Index pigments Pigment Blue 15, Pigment Blue 15:1, Pigment Blue 15:2, Pigment Blue 15:3, Pigment Blue 15:4, Pigment Blue 15:6, Pigment Blue 16, Pigment Green 7 or Pigment Green 36; anthanthrone, anthraquinone, quinacridone, dioxazine, indanthrone, perylene, perinone and thioindigo pigments, more particularly the Colour Index pigments Pigment Yellow 196, Pigment Red 122, Pigment Red 149, Pigment Red 168, Pigment Red 177, Pigment Red 179, Pigment Red 181, Pigment Red 207, Pigment Red 209, Pigment Red 263, Pigment Blue 60, Pigment Violet 19, Pigment Violet 23 or Pigment Orange 43; triarylcarbonium pigments, more particularly the Colour Index pigments Pigment Red 169, Pigment Blue 56 or Pigment Blue 61; diketopyrrolopyrrole pigments, more particularly the Colour Index pigments Pigment Red 254, Pigment Red 255, Pigment Red 264, Pigment Red 270, Pigment Red 272, Pigment Orange 71, Pigment Orange 73, Pigment Orange 81.
Preferred inorganic pigments are for example titanium dioxides, zinc sulfides, zinc oxides, iron oxides, magnetites, manganese iron oxides, chromium oxides, ultramarine, nickel or chromium antimony titanium oxides, manganese titanium rutiles, cobalt oxides, mixed oxides of cobalt and of aluminum, rutile mixed phase pigments, sulfides of the rare earths, spinels of cobalt with nickel and zinc, spinels based on iron and chromium with copper zinc and also manganese, bismuth vanadates and also blend pigments, more particularly the Colour Index pigments Pigment Yellow 184, Pigment Yellow 53, Pigment Yellow 42, Pigment Yellow Brown 24, Pigment Red 101, Pigment Blue 28, Pigment Blue 36, Pigment Green 50, Pigment Green 17. Preference is also given to mixtures of inorganic pigments and also mixtures of organic pigments with inorganic pigments.
Colorant (I) and colorant (II) can be used for example as powder pigment, as presscake, as dispersion, as solid pigment preparation or as liquid pigment formulation in the manufacture of the microencapsulated colorant granules. Preference is given to aqueous glycol-containing pigment dispersions or formulations.
More preferably, colorant (I) and colorant (II) are selected from colorants allowed for cosmetic use and from colorants allowed for detergents.
Even more preferably colorant (I) and colorant (II) are selected from the group consisting of C.I. Pigment Black 7 (C.I. 77266), C.I. Pigment Blue 15 (C.I. 74160), C.I. Pigment Blue 15:1 (C.I. 74160), C.I. Pigment Blue 15:3 (C.I. 74160), C.I. Pigment Blue 15:6 (C.I. 74160), C.I. Pigment Blue 80 (C.I. 77007), C.I. Pigment Red 4 (C.I. 12085), C.I. Pigment Red 5 (C.I. 12490), C.I. Pigment Red 112 (C.I. 12370), C.I. Pigment Red 122 (C.I. 73915), C.I. Pigment Red 181 (C.I. 73360), C.I. Pigment Red 254 (C.I. 56110), C.I. Vat Red 1, C.I. Pigment Green 7 (C.I. 74260), C.I. Pigment Green 36 (C.I. 74265), C.I. Pigment Violet 23 (C.I. 51319), C.I. Pigment Yellow 1 (C.I. 11680), C.I. Pigment Yellow 3 (C.I. 11710) and C.I. Pigment Yellow 122 (C.I. 21090).
Preferred polyols (c) are glycerine, glycols, polyglycols, pentaerythrite, sugar alcohols, especially mannitol, sorbitol, xylitol, maltitol, lactitol, lactose and monosaccharides, especially lactose.
Microcrystalline cellulose (E460i) and powdered cellulose (E460ii) are commercially available as inactive fillers, thickeners or stabilizers in processed foods and pharmaceuticals. While microcrystalline cellulose is used in the core as component b), powdered cellulose can be used in the shell as component d). Instead of or in addition to powdered cellulose, cellulose derivatives can be used, such as ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl methyl cellulose, hydroxyethyl cellulose.
Preferred polycarboxylic acids used as component d) are polyacrylic acid, polymethacrylic acid, acrylate-methacrylate copolymers, such as methacrylic acid-ethylacrylate copolymers, poly(ethylacrylate-methylmethacrylate-hydroxyethylmethacrylate), styrene-(meth)acrylates, and maleic acid copolymers, such as acrylic acid-maleic acid copolymers.
Preferred vinyl polymers used as component d) are polyvinyl acetates and vinyl (meth)acrylic copolymers.
In a preferred embodiment of the invention the polymer used as component d) and contained in the one or more microencapsulated colorant granules is selected from the group consisting of polyacrylic acid, polymethacrylic acid, copolymers of polyacrylic and polymethacrylic acid, styrene-(meth)acrylates, maleic acid copolymers, polyvinylacetates, vinyl acrylic copolymers, vinyl methacrylic copolymers, cellulose, ethyl cellulose, hydroxypropyl cellulose, carboxymethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl methyl cellulose, and hydroxyethyl cellulose.
The molecular weight of polymers (d) is preferably between 500 and 500 000 g/mol, more preferably between 1 000 and 300 000 g/mol.
In a preferred embodiment of the invention the inventive compositions comprise microencapsulated colorant granules as characterized before, wherein the particle size distribution of the granules is between 100 and 1500 μm, more preferred between 200 and 1000 μm, most preferred between 300 and 600 μm.
The microencapsulated colorant granules contained in the inventive compositions can preferably be prepared by a process with the following steps:
For example, colorant (I) in powderous form is homogenized with microcrystalline cellulose, the polyol and water in a planetary mixer until a homogeneous gel-like mass is obtained. This mass is then subjected to a screw extruder to get small noodles which are further charged into a spherodizer to get microbeads. These microbeads are treated as core. For coating, the core microbeads are subjected to a fluidized bed processing unit, wherein a solution or suspension of components (d) and optionally (e) and optionally (f) in water is sprayed onto the microbeads.
In one embodiment, a suspension of white pigment (e) and polymer (d) in water is sprayed onto the microbeads.
In another embodiment, in a first spraying operation, a suspension of white pigment (e) and polymer (d) in water is sprayed onto the microbeads, followed by a second spraying operation, wherein a suspension of colorant (II) and polymer (d) in water is sprayed onto the microbeads to get a colored coating.
The preferred processing temperature during spraying is between 20 and 80° C., especially between 30 and 60° C.
The coated microbeads obtained are dried to obtain microencapsulated colorant granules.
The microencapsulated colorant granules can be incorporated in colorless or colored liquid or gel-like cleansing compositions suitable for cleaning hard surfaces, washing clothes and dishes, and softening fabrics thereby producing inventive compositions. These inventive liquid or gel-like compositions can be employed for household, institutional and/or industrial applications. The microencapsulated colorant granules can furthermore be incorporated in colorless or colored liquid or gel-like personal cleansing compositions or personal care products thereby also producing inventive compositions. During the application, particularly during the washing process, the shell decomposes and the fine colorant particles are released into the inventive compositions and/or disperse into the foam resulting from the inventive compositions inducing a coloring or color change of the inventive composition and/or the foam.
Preferred inventive compositions are compositions suitable for cleaning hard surfaces such as general or all-purpose cleaners, window cleaners, sanitary cleaners, disinfectants or vehicle cleaners, compositions suitable for washing clothes such as detergents or high density liquids (HDL), dish washing compositions such as hand dishwash compositions, compositions suitable for softening fabrics or any other suitable cleaning products.
Further preferred inventive compositions are personal cleansing compositions such as personal cleansing compositions for skin, hair and teeth, e.g. shower baths, body washes, shampoos, hand soaps, facial soaps or facial cleansing compositions, baby washes or toothpastes or personal care products such as body lotions or sunscreens.
Further preferred inventive compositions are pet detergents or washes.
In general, the microencapsulated colorant granules are present in the inventive compositions in an amount of from 0.1 to 10% by weight, preferably in an amount of from 0.2 to 7% by weight, more preferably in an amount of from 0.5 to 5% by weight, relative to the total weight of the inventive composition.
The compositions according to the invention, in particular the inventive cleansing compositions, personal cleansing compositions and personal care compositions may contain components which are common in the respective art, such as nonionic, anionic, cationic, and amphoteric surfactants, dispersing agents such as suspending agents, emollients, preservatives, fragrances, pH modifiers, anti-microbial agents, colorants, water, and non-aqueous solvents.
In a preferred embodiment of the invention the inventive compositions comprise at least 40% by weight of water, relative to the total weight of the inventive composition. Preferably, these inventive compositions comprise not more than 99% by weight of water, relative to the total weight of the inventive composition. In a more preferred embodiment of the invention the inventive compositions comprise of from 50 to 98% by weight and more preferably of from 55 to 97% by weight of water, relative to the total weight of the inventive composition.
The amount of surfactants contained in the inventive compositions can vary greatly depending upon various factors. In some embodiments of the invention, the inventive compositions may contain surfactants in an amount of from 1 to 60% by weight and preferably of from 5 to 40% by weight, relative to the total weight of the inventive composition.
The inventive compositions may also contain various emollients. In fact, some of the above described surfactants may be considered emollients. Particular emollients that may be used include ethoxylated and propoxylated alcohols, such as cetyl alcohols and ethoxylated lanolin.
In some instances, the inventive compositions may also include one or more non-aqueous solvents. Although not required, non-aqueous solvents can sometimes aid in dissolving certain components, e.g. preservatives or anti-microbial agents. Examples of some suitable non-aqueous solvents include, but are not limited to:
glycerine; glycols, such as propylene glycol, butylene glycol, triethylene glycol, hexylene glycol, polyethylene glycols, ethoxydiglycol, and dipropyleneglycol; alcohols, such as ethanol, n-propanol, and isopropanol; triglycerides; ethyl acetate; acetone; triacetin; and combinations thereof. Preferred solvent combinations include a glycol, particularly hexylene and/or propylene glycol, and one or more lower alcohols, particularly isopropanol, n-propanol, and/or ethanol.
The inventive compositions may also contain various preservatives to increase the shelf life of the composition. Preferably, the preservative is present in an amount of from 0.001 to 5% by weight, more preferably of from 0.001 to about 1% by weight, and even more preferably, of from 0.1 to 0.15% by weight, relative to the total weight of the inventive composition.
If necessary, various pH modifiers may be utilized in the inventive compositions to achieve the desired pH level. For instance, some examples of basic pH modifiers that may be used in the inventive compositions include, but are not limited to ammonia, mono-, di-, and tri-alkylamines, mono-, di-, and tri-alkanolamines, alkali metal and alkaline earth metal hydroxides, alkali metal and alkaline earth metal silicates, mineral acids, carboxylic acids, and polymeric acids.
In a preferred embodiment of the invention the inventive compositions possess a pH value of from 1 to 12, preferably of from 2 to 10 and more preferably of from 2.5 to 8.5.
In a further preferred embodiment of the invention the inventive compositions comprise one or more dispersing agents.
As dispersing agent any known dispersing agent may be used. For example, the dispersing agent may be a clay, a starch including starch derivatives, a modified cellulose, a natural gum, a wax, a fatty acid, a fatty alcohol, a multifunctional alcohol, a colloidal or a fumed particle, a fatty acid ester, a polyoxyethylene glycol ether, or a mixture thereof.
However, in one preferred embodiment of the invention the inventive compositions comprise one or more polymers containing one or more structure units derived from acryloyldimethyltaurine and/or salts thereof (acryloyldimethyltaurates) as dispersing agent/s.
Preferred polymers containing one or more structure units derived from acryloyldimethyltaurine and/or salts thereof are polymers containing
Such polymers are commercially available from Clariant (e.g. Aristoflex® AVC and Aristoflex® TAC)
In a further preferred embodiment of the invention the inventive compositions comprise one or more polymers containing structure units derived from terephthalic acid and/or salts or esters thereof as dispersing agent/s.
Preferred polymers containing structure units derived from terephthalic acid and/or salts or esters thereof are polymers containing
Such polymers are commercially available from Clariant (e.g. Texcare® SRN 100, Texcare® SRN 170, Texcare® SRN 240, Texcare® SRN 300, Texcare® SRN 325 or Texcare® SRA 300).
The dispersing agent may be present in the inventive compositions in an amount sufficient to prevent the microencapsulated colorant granules from settling. The dispersing agent may be present in the inventive compositions in an amount of from 0.1 to 15% by weight, preferably of from 0.1 to 10% by weight and more preferably of from 0.5 to 3% by weight, relative to the total weight of the inventive composition.
The inventive compositions possess the advantage that they may change color upon application. Therefore, the inventive compositions preferably are color changing compositions.
In a further preferred embodiment of the invention the inventive compositions are personal care or cleansing compositions.
In the following examples “parts” refer to parts by weight and percentages refer to weight percent (wt.-%) if not expressly stated otherwise.
33 parts of powdered C.I. Pigment Red 181 were homogenized with 33 parts of microcrystalline cellulose and 33 parts of lactose and 30 parts of water in a planetary mixer until a homogeneous gel-like mass was obtained. This mass was subjected to a screw extruder to get small noodles which were further charged into a spherodizer to get microbeads of about 200 to 300 micrometer in diameter. The microbeads were subjected to a fluidized bed processing unit. A dispersion of 5 parts of methacrylic acid-ethylacrylate copolymer (1:1; mw approximately 250 000 g/mol) in 5 parts of water was sprayed with the microbeads at a temperature of about 50° C. to get a colorless polyacrylate coating onto the beads. The final beads were removed from the fluidized bed unit and dried.
33 parts of powdered C.I. Pigment Blue 15:1 were homogenized with 33 parts of microcrystalline cellulose and 33 parts of xylitol and 30 parts of water in a planetary mixer until a homogeneous gel-like mass was obtained. This mass was subjected to a screw extruder to get small noodles which were further charged into a spherodizer to get microbeads of about 200 to 250 micrometer in diameter. These microbeads were treated as core.
The microbeads were subjected to a fluidized bed processing unit. A dispersion of 15 parts of titanium dioxide in 5 parts of water and 5 parts of sodium polyacrylate (Mowilith® DM 6400) was sprayed with the microbeads at a temperature of about 50° C. to get a TiO2-polyacrylate coating onto the beads. The final beads were removed from the fluidized bed unit and dried to give microencapsulated colorant granules of about 400 to 450 micrometer in diameter.
33 parts of powdered C.I. Pigment Green 7 were homogenized with 33 parts of microcrystalline cellulose and 33 parts of sorbitol and 30 parts of water in a planetary mixer until a homogeneous gel-like mass was obtained. This mass was subjected to a screw extruder to get small noodles which were further charged into a spherodizer to get microbeads of about 200 to 250 micrometer in diameter. These microbeads were treated as core.
The microbeads were subjected to a fluidized bed processing unit. A dispersion of 15 parts of titanium dioxide in 5 parts of water and 5 parts of sodium polyacrylate (Mowilith® DM 6400) was sprayed with the microbeads at a temperature of about 50° C. to get a TiO2-polyacrylate coating onto the beads.
Further, a suspension of 15 parts of C.I. Pigment Red 5, 5 parts of water and 5 parts of sodium polyacrylate (Mowilith® DM 6400) was sprayed with the coated microbeads at a temperature of about 50° C. to get a red-colored coating on these beads.
The final beads were removed from the fluidized bed unit and dried to give microencapsulated colorant granules of about 400 to 450 micrometer in diameter.
Composition:
Preparation:
I. Mix C and D at room temperature
II. Add A to I and mix
III. Add B to II and mix
IV. Add E, F, G and H to III and mix
Composition:
Preparation:
I. Mix A and C at room temperature
II. Add B to I and mix
III. Add D, E, F and G to II and mix
Composition:
Preparation:
I. Mix A and C at room temperature
II. Heat B at 34 to 40° C.
III. add II to I
IV. heat III and homogenize at 80 to 85° C. with stirring
V. cool to room temperature
VI. add D and E to V and mix
Composition:
Preparation:
I. Mix A and B at room temperature
II. Add C to I and mix
III. Add D to II and mix
IV. Add E to III an mix
Composition
Preparation:
I. Stir B into A.
II. Add components from C successively to I.
III. Adjust pH to 5.5.
IV. Adjust the viscosity by stirring D into II.
Preparation:
I. Mix A with B.
II. Stir C into I until a clear solution is obtained.
III. Add components from D successively to II.
IV. Stir E into F with heating and then stir mixture into III.
V. Add components from G successively to IV.
VI. Adjust pH if appropriate.
VII. Adjust the viscosity by stirring H into V or VI.
Composition
Preparation:
I. Mix A and B.
II. Mix the components C.
III Add II to I.
IV. Stir D into III.
V. Homogenize emulsion, pH 3.5.
Composition
Preparation:
I. Heat A to about 80° C.
II. Dissolve B in I
III cool II to 25° C. without stirring
IV. add C to III under gentle stirring
V. add D to IV under gentle stirring
| Number | Date | Country | Kind |
|---|---|---|---|
| 09009318.8 | Jul 2009 | EP | regional |
| Filing Document | Filing Date | Country | Kind | 371c Date |
|---|---|---|---|---|
| PCT/EP10/04311 | 7/15/2010 | WO | 00 | 4/2/2012 |
