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WO2000063341A1 - Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition - Google Patents

Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition Download PDF

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Publication number
WO2000063341A1
WO2000063341A1 PCT/US2000/010386 US0010386W WO0063341A1 WO 2000063341 A1 WO2000063341 A1 WO 2000063341A1 US 0010386 W US0010386 W US 0010386W WO 0063341 A1 WO0063341 A1 WO 0063341A1
Authority
WO
WIPO (PCT)
Prior art keywords
colored
liquid
particles
process according
polymeπc
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2000/010386
Other languages
French (fr)
Inventor
Jeffrey Donald Painter
Joseph Herbert Thien
Peter Robert Foley
Xiaoqing Song
Mary Ruth Leyendecker
Eugene Steven Sadlowski
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Procter and Gamble Co
Original Assignee
Procter and Gamble Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Priority to CA002368600A priority Critical patent/CA2368600C/en
Priority to EP00923464A priority patent/EP1171569A1/en
Priority to US09/937,356 priority patent/US6730652B1/en
Priority to AU43582/00A priority patent/AU4358200A/en
Priority to JP2000612420A priority patent/JP2002542383A/en
Publication of WO2000063341A1 publication Critical patent/WO2000063341A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B63/00—Lakes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
    • C11D17/0013—Liquid compositions with insoluble particles in suspension
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/22—Carbohydrates or derivatives thereof
    • C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • C11D3/225—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3753—Polyvinylalcohol; Ethers or esters thereof
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/40—Dyes ; Pigments

Definitions

  • the present invention generally relates to liquid automatic dishwashing detergent compositions. More particularly, the invention relates to a process for making colored particles that can be incorporated into a bleach-contammg or non-bleach-contammg liquid automatic dishwashing detergent composition for improving the aesthetics of the liquid composition wherein the colored particles do not stain the plastic surfaces of dishware or an automatic dishwasher.
  • liquid ADW products have a preference for such products having a certain color or appearance.
  • the addition of solid particles suspended into a liquid ADW composition can improve the aesthetics of the product by simply improving the physical appearance of the product. This is particularly true if the particles are colored and their color is matched effectively to the base color of the liquid ADW composition.
  • Previously used particles in liquid ADW products have had a major disadvantage of contributing negatively to unwanted filming, particularly on glass, stainless steel and plastic surfaces. This is because the previously used particles have been coated with water-msoluble coatings, such as waxes, which melt and are released into the wash solution due to the high temperature encountered during the automatic dishwashing process.
  • the particles cannot be colored by simply using a dye, because du ⁇ ng storage of the liquid ADW product, the dye gets bleached
  • the formulators have to use bleach-safe pigments to impart an aesthetically pleasing color
  • the incorporation of pigments posed a major problem: the color of the pigment is found to detrimentally stain plastic surfaces, such as plastic dishware and the internal plastic surfaces of a dishwasher.
  • the inventors of the present invention have discovered a process of coating the particles with a pigment in a manner such that the particles are non-stammg.
  • This invention is not limited to just bleach-contammg liquid ADWs and is also applicable to non-bleach-contammg liquid ADWs that are incorporated with prills or particles colored with pigments.
  • the present invention is thus directed to overcome one or more of the problems as set forth before.
  • the invention meets the needs above by providing a process for forming a non-stammg colored composite particle suitable for incorporation in a bleach-contammg or non-bleach- contaming liquid detergent composition, a non-stainmg colored composite particle and a liquid dishwashing detergent composition.
  • the process includes the steps of forming a colored liquid dispersion of pigment particles in a first liquid medium.
  • the size of the pigment particles in the colored liquid dispersion is no greater than about 5 ⁇ m.
  • the process includes the step of mixing the colored liquid dispersion with a polymeric material and a second liquid medium to form a sprayable colored polyme ⁇ c mate ⁇ al.
  • the polymeric mate ⁇ al being selected from the group consisting of alkyl cellulose ethers and polyvinyl alcohol.
  • the process also includes the step of spraying the colored polyme ⁇ c material on a composite particle and forming a colored polyme ⁇ c coating on the composite particle.
  • a non-staining colored composite particle suitable for incorporation in a bleach-contammg liquid detergent composition is disclosed.
  • the particle is made by the process as set forth above.
  • a liquid automatic dishwashing detergent product is disclosed.
  • the product includes a liquid dishwashing detergent composition containing chlo ⁇ ne bleach, and non-staming colored composite particles.
  • the particles are made by the process as set forth above. DETAILED DESCRIPTION OF THE INVENTION
  • the process includes the steps of forming a colored liquid dispersion of pigment particles in a first liquid medium.
  • the size of the pigment particles in the colored liquid dispersion is desirably no greater than about 5 ⁇ m, preferably no greater than about 1 ⁇ m, more preferably no greater than about 0J ⁇ m, and most preferably no greater than about 0.01 ⁇ m. It has been surp ⁇ smgly discovered that when the pigment particle size in the pigment-liquid dispersion is maintained withm the above size limitations, the resultant pigment, when deposited on a particle as a part of the sprayable polyme ⁇ c slurry, is essentially non-stammg. i.e., its color does not transfer onto plastic surfaces. The selection of the pigment particle size is the key to the present invention.
  • the first liquid medium is preferably water.
  • a minor amount of a nomonic surfactant is added to the water to improve the dispersion of the pigment. Typically, this surfactant is added in an amount no greater than about 10% by weight.
  • the process includes the step of maintaining the amount of surfactants used in the bleach-containing liquid detergent composition at a preselected value such that when the bleach-containing liquid detergent composition is diluted m a wash solution, the amount of surfactant delivered m the wash solution is less than c ⁇ tical micelle concentration
  • critical micelle concentration is well known to those skilled m the art and need not be explained any further for purposes of brevity.
  • Polvmenc coating In the preferred embodiment, the colored polyme ⁇ c coating is insoluble in the liquid automatic dishwashing detergent composition but soluble m automatic dishwashing wash solution. The coating is prepared from mate ⁇ als which are insoluble in the liquid automatic dishwashing detergent composition but soluble m automatic dishwashing wash solution.
  • the coaling is prepared from mate ⁇ als selected from the group consisting of alkyl cellulose ethers and polyvmyl alcohol.
  • the coating is prepared from algmate.
  • the alkyl cellulose ethers are selected from one of methyl cellulose and hydroxypropyl methyl cellulose (HPMC).
  • HPMC hydroxypropyl methyl cellulose
  • the coating is prepared from methyl cellulose having a number average molecular weight desirably in a range of from about 5000 to about 100,000, more preferably from about 10,000 to about 20,000, and most preferably, about 14,000.
  • the preferred methyl cellulose IS one sold under the trade name Methocel A15LV. and manufactured by Dow Chemicals.
  • the polymeric coating is polyvmyl alcohol (PVA) having a molecular weight, desirably m a range of from about 5000 to about 100,000, and preferably from about 13,000 to about 23,000
  • PVA polyvmyl alcohol
  • the preferred PVA is from about 87% to about 89% hydrolyzed, such as a commercially available product having a trade name Airvol 205.
  • the particles are insoluble in the liquid automatic dishwashing detergent composition and only soluble m the wash solution du ⁇ ng automatic dishwashing.
  • the process by which the colored polymeric coating is prepared and deposited upon the particle is critical in order for the particles to remain undissolved in the liquid automatic dishwashing detergent composition and only become soluble m the wash solution du ⁇ ng automatic dishwashing. It is desirable that the particles dispersed m the liquid ADW compositions do not break up or dissolve in the composition. It is also desirable that this be achieved without depositing an unduly thick coating of a polymeric mate ⁇ al on the particle. It has been surprisingly discovered that when the polyme ⁇ c mate ⁇ al, such as methyl cellulose is sufficiently hydrated before spraying on the particle or prill, the polymer coated particle or prill remains stable, unbroken and undissolved in the liquid ADW composition.
  • This hydration is achieved by forming a sprayable aqueous solution of the polymer (alkyl cellulose ether and/or polyvmyl alcohol) having a polymer concentration desirably in a range of from about 1% to about 30%) by weight, preferably in a range of about 3% to about 20 %, more preferably in a range of about 3% to about 10 %, and most preferably, about 5%.
  • the temperature of aqueous solution of the polymer is desirably maintained within a range of from about 30 °C to about 40 °C while spraying the polymer solution on the particle, and preferably m a range of from about 32 °C to about 38 °C, and most preferably at a temperature of about 35 °C.
  • the coating is desirably present m an amount in a range of from about 1% to about 25% by weight of the particle, preferably from about 4% to about 10% by weight of the particle, and most preferably, about 5% by weight of the particle.
  • the reduced coating weight levels are desirable so that the least effective coating amount is used in order to accomplish the objective to having a protective coating without unnecessary polymer that might det ⁇ mentally contribute to unwanted residue deposition in the washing machine.
  • the particles are colored and the automatic dishwashing liquid detergent composition is clear or translucent, so as to make the liquid automatic dishwashing product aesthetically pleasing.
  • the particles and the liquid automatic dishwashing detergent composition are both colored and the color of the particles is matched to the base color of the liquid composition.
  • the particles have a dark green color whereas the liquid composition has a light green color.
  • Other preferred color combinations for the polyme ⁇ c coating on the particles and the liquid automatic dishwashing composition are: blue:blue, blue:wh ⁇ te, gree green, greemwhite and green:yellow, respectively.
  • the particles comprise from about 0.1% to about 5.0% by weight of the liquid composition, and preferably, from about 0.2% to about 1.0% by weight of the liquid composition.
  • a non-stammg colored composite particle suitable for incorporation in a bleach-contammg liquid detergent composition is disclosed. The particle is made by the process as set forth above.
  • the particles can be formed from va ⁇ ous mate ⁇ als that do not cause any det ⁇ mental affect upon the performance of the liquid detergent.
  • the particles are in the form of p ⁇ lls.
  • the prills typically have a core which is coated with a polyme ⁇ c coating as desc ⁇ bed before.
  • the core can be made from sucrose, as an example.
  • the method of forming p ⁇ lls is well known to those skilled m the art and is disclosed m the literature, such as for example, in U.S. Patent No. 4,965,012, which is incorporated herein by reference.
  • the particles can be of va ⁇ ous sizes and shapes, such as sphe ⁇ cal, oval, cyhnd ⁇ cal or polygonal and desirably have a particle size in a range of from about 200 ⁇ m to about 5000 ⁇ m, preferably, from about 400 ⁇ m to about 2000 ⁇ m, and most preferably, from about 500 ⁇ m to about 850 ⁇ m.
  • a liquid automatic dishwashing detergent product in yet another embodiment, includes a liquid dishwashing detergent composition containing chlorine bleach, and non-stammg colored composite particles. The particles are made by the process as set forth above. Liquid automatic dishwashing composition components
  • the liquid automatic dishwashing detergent product is highly viscous in a quiescent state and has a relatively high yield stress values. When subjected to shear stresses, however, such as being shaken m a container or squeezed through an orifice, the product quickly fluidizes and upon cessation of the applied shear stress, quickly reverts to a high viscosity state.
  • the above liquid automatic dishwashing detergent product is preferably low foaming, readily soluble in the washing medium and most effective at pH values best conducive to improved cleaning performance, such as in a range of desirably from about pH 7.0 to about pH 13.0, and preferably from about pH 8.0 to about pH 12.0.
  • the physical stability of the liquid product may be improved and the thickness of the liquid product may be altered by the addition of a cross linking polyacrylate thickener to the liquid detergent product as a thixotropic thickener.
  • the pH adjusting components are desirably selected from sodium or potassium carbonate or sesquicarbonate, sodium or potassium silicate, cit ⁇ c acid, sodium or potassium bicarbonate, sodium or potassium borate, sodium or potassium hydroxide, and mixtures thereof.
  • KOH are the preferred ingredients for increasing the pH to withm the above ranges.
  • Other preferred pH adjusting ingredients are sodium carbonate, potassium carbonate, and mixtures thereof.
  • Chlo ⁇ ne bleach stable low foaming surfactants are preferred and such surfactants are present in a range of from about 0.1% to about 10% by weight of the liquid composition.
  • Such surfactants are generally known to one skilled m the art and need not be elaborated here, for purposes of brevity.
  • One example of such a surfactant is an aniomc surfactant commercially available under the trade name Dowfax.
  • the liquid automatic dishwashing detergent composition optionally also contains from about 0.5% to about 20% of a dispersant polymer selected from the group consisting of polyacrylates and polyacrylate copolymers, and from about 0.1% to about 5% of a chlo ⁇ ne bleach stable foam suppressant.
  • a dispersant polymer selected from the group consisting of polyacrylates and polyacrylate copolymers
  • foam suppressants are well known to those skilled in the art.
  • Sample A of the liquid automatic dishwashing detergent product composition is formulated using the below named ingredients, as set forth in Example A.
  • the non-staining colored particles having a sphencal shape, and a diameter of about 750 ⁇ m are formed from a sucrose core coated with a polyme ⁇ c coating formed from methyl cellulose (Methocel A15LV), and having a bluish-green color.
  • the bluish- green color is imparted by adding a pigment into the methyl cellulose coating before spraying it on the particle according to the process of the present invention.
  • the particles comp ⁇ se about 0.1% to about 5% by weight of the liquid composition.
  • the optimum methyl cellulose coating is about 5% by weight of the particle.
  • the coating is sprayed on the sucrose core particle by spraying a 5% by weight aqueous solution of methyl cellulose with pigment.
  • the aqueous solution temperature being carefully maintained at about 35 °C.
  • the size of the pigment particles in the aqueous solution is no greater than about 1 ⁇ m.
  • the resultant particles are insoluble in the liquid composition but are soluble m the wash solution du ⁇ ng automatic dishwashing.
  • the resultant colored particles are also non-stammg to plastic surfaces.

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  • Life Sciences & Earth Sciences (AREA)
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  • Engineering & Computer Science (AREA)
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Abstract

A process for forming a non-staining colored composite particle suitable for incorporation in a bleach-containing or a non-bleach-containing liquid detergent composition is disclosed. The process includes the steps of forming a colored liquid dispersion of pigment particles in a first liquid medium wherein the size of the pigment particles in the colored liquid dispersion is no greater than about 5 νm. The process includes the step of mixing the colored liquid dispersion with a polymeric material and a second liquid medium to form a sprayable colored polymeric material. The process also includes the step of spraying the colored polymeric material on a composite particle and forming a colored polymeric coating on the composite particle. A non-staining colored particle and a liquid ADW detergent composition are also disclosed.

Description

PROCESS FOR MAKING NON-STAINING COLORED PARTICLES FOR IMPROVING AESTHETICS OF A LIQUID AUTOMATIC DISHWASHING DETERGENT PRODUCT. THE
PARTICLES. AND A COMPOSITION
TECHNICAL FIELD The present invention generally relates to liquid automatic dishwashing detergent compositions. More particularly, the invention relates to a process for making colored particles that can be incorporated into a bleach-contammg or non-bleach-contammg liquid automatic dishwashing detergent composition for improving the aesthetics of the liquid composition wherein the colored particles do not stain the plastic surfaces of dishware or an automatic dishwasher.
BACKGROUND OF THE INVENTION Consumers of liquid ADW products have a preference for such products having a certain color or appearance. The addition of solid particles suspended into a liquid ADW composition can improve the aesthetics of the product by simply improving the physical appearance of the product. This is particularly true if the particles are colored and their color is matched effectively to the base color of the liquid ADW composition. Previously used particles in liquid ADW products have had a major disadvantage of contributing negatively to unwanted filming, particularly on glass, stainless steel and plastic surfaces. This is because the previously used particles have been coated with water-msoluble coatings, such as waxes, which melt and are released into the wash solution due to the high temperature encountered during the automatic dishwashing process. Further, in the arena of bleach containing liquid ADWs, the particles cannot be colored by simply using a dye, because duπng storage of the liquid ADW product, the dye gets bleached Thus, the formulators have to use bleach-safe pigments to impart an aesthetically pleasing color Before this invention, the incorporation of pigments posed a major problem: the color of the pigment is found to detrimentally stain plastic surfaces, such as plastic dishware and the internal plastic surfaces of a dishwasher.
It has been desirable to have a process by which colored pigment based particles can be made for incorporation m bleach-contammg or non-bleach-contaming liquid ADW product, such that the particles are non-stammg. It has also been desirable that the solid particles do not dissolve in the liquid ADW product, but dissolve rapidly in the wash solution duπng automatic dishwashing. It has been desirable to have a liquid ADW product having solid particles that do not cause a significant amount of unwanted filming on glass, stainless steel and plastic.
The inventors of the present invention have discovered a process of coating the particles with a pigment in a manner such that the particles are non-stammg. This invention is not limited to just bleach-contammg liquid ADWs and is also applicable to non-bleach-contammg liquid ADWs that are incorporated with prills or particles colored with pigments. The present invention is thus directed to overcome one or more of the problems as set forth before.
SUMMARY OF THE INVENTION The invention meets the needs above by providing a process for forming a non-stammg colored composite particle suitable for incorporation in a bleach-contammg or non-bleach- contaming liquid detergent composition, a non-stainmg colored composite particle and a liquid dishwashing detergent composition.
In one aspect of the present invention, the process includes the steps of forming a colored liquid dispersion of pigment particles in a first liquid medium. The size of the pigment particles in the colored liquid dispersion is no greater than about 5 μm. The process includes the step of mixing the colored liquid dispersion with a polymeric material and a second liquid medium to form a sprayable colored polymeπc mateπal. The polymeric mateπal being selected from the group consisting of alkyl cellulose ethers and polyvinyl alcohol. The process also includes the step of spraying the colored polymeπc material on a composite particle and forming a colored polymeπc coating on the composite particle.
In another aspect of the present invention, a non-staining colored composite particle suitable for incorporation in a bleach-contammg liquid detergent composition is disclosed. The particle is made by the process as set forth above. In yet another aspect of the present invention, a liquid automatic dishwashing detergent product is disclosed. The product includes a liquid dishwashing detergent composition containing chloπne bleach, and non-staming colored composite particles. The particles are made by the process as set forth above. DETAILED DESCRIPTION OF THE INVENTION In the preferred embodiment of the present invention, the process includes the steps of forming a colored liquid dispersion of pigment particles in a first liquid medium. Pigment processing
The size of the pigment particles in the colored liquid dispersion is desirably no greater than about 5 μm, preferably no greater than about 1 μm, more preferably no greater than about 0J μm, and most preferably no greater than about 0.01 μm. It has been surpπsmgly discovered that when the pigment particle size in the pigment-liquid dispersion is maintained withm the above size limitations, the resultant pigment, when deposited on a particle as a part of the sprayable polymeπc slurry, is essentially non-stammg. i.e., its color does not transfer onto plastic surfaces. The selection of the pigment particle size is the key to the present invention. One skilled m the art can apply other means for achieving a pigment particle size in the size limitation as disclosed above. In the preferred embodiment, the first liquid medium is preferably water. Optionally, a minor amount of a nomonic surfactant is added to the water to improve the dispersion of the pigment. Typically, this surfactant is added in an amount no greater than about 10% by weight. In the preferred embodiment, the process includes the step of maintaining the amount of surfactants used in the bleach-containing liquid detergent composition at a preselected value such that when the bleach-containing liquid detergent composition is diluted m a wash solution, the amount of surfactant delivered m the wash solution is less than cπtical micelle concentration The term "critical micelle concentration" is well known to those skilled m the art and need not be explained any further for purposes of brevity. Polvmenc coating In the preferred embodiment, the colored polymeπc coating is insoluble in the liquid automatic dishwashing detergent composition but soluble m automatic dishwashing wash solution. The coating is prepared from mateπals which are insoluble in the liquid automatic dishwashing detergent composition but soluble m automatic dishwashing wash solution. The coaling is prepared from mateπals selected from the group consisting of alkyl cellulose ethers and polyvmyl alcohol. Alternatively, the coating is prepared from algmate. Desirably, the alkyl cellulose ethers are selected from one of methyl cellulose and hydroxypropyl methyl cellulose (HPMC). Preferably, the coating is prepared from methyl cellulose having a number average molecular weight desirably in a range of from about 5000 to about 100,000, more preferably from about 10,000 to about 20,000, and most preferably, about 14,000. The preferred methyl cellulose IS one sold under the trade name Methocel A15LV. and manufactured by Dow Chemicals. Alternatively, the polymeric coating is polyvmyl alcohol (PVA) having a molecular weight, desirably m a range of from about 5000 to about 100,000, and preferably from about 13,000 to about 23,000 The preferred PVA is from about 87% to about 89% hydrolyzed, such as a commercially available product having a trade name Airvol 205. Further, the particles are insoluble in the liquid automatic dishwashing detergent composition and only soluble m the wash solution duπng automatic dishwashing.
Process for spraying colored polymeπc coating on particles
The process by which the colored polymeric coating is prepared and deposited upon the particle is critical in order for the particles to remain undissolved in the liquid automatic dishwashing detergent composition and only become soluble m the wash solution duπng automatic dishwashing. It is desirable that the particles dispersed m the liquid ADW compositions do not break up or dissolve in the composition. It is also desirable that this be achieved without depositing an unduly thick coating of a polymeric mateπal on the particle. It has been surprisingly discovered that when the polymeπc mateπal, such as methyl cellulose is sufficiently hydrated before spraying on the particle or prill, the polymer coated particle or prill remains stable, unbroken and undissolved in the liquid ADW composition. This hydration is achieved by forming a sprayable aqueous solution of the polymer (alkyl cellulose ether and/or polyvmyl alcohol) having a polymer concentration desirably in a range of from about 1% to about 30%) by weight, preferably in a range of about 3% to about 20 %, more preferably in a range of about 3% to about 10 %, and most preferably, about 5%. Further, the temperature of aqueous solution of the polymer is desirably maintained within a range of from about 30 °C to about 40 °C while spraying the polymer solution on the particle, and preferably m a range of from about 32 °C to about 38 °C, and most preferably at a temperature of about 35 °C. It has been surpπsingly found that by using a combination of the above process steps, i.e., the polymer solution being in a range of from about 1% to 30% by weight, and the spray temperature being m a range of from about 30 °C to about 40 °C, that a very stable, unbroken, continuous coating is formed on the particle or pπll which is undissolved in the liquid ADW composition but soluble m the wash solution, while at the same time, requiπng only about 5% polymer by weight of the particle. In the preferred embodiment, the coating is desirably present m an amount in a range of from about 1% to about 25% by weight of the particle, preferably from about 4% to about 10% by weight of the particle, and most preferably, about 5% by weight of the particle. The reduced coating weight levels are desirable so that the least effective coating amount is used in order to accomplish the objective to having a protective coating without unnecessary polymer that might detπmentally contribute to unwanted residue deposition in the washing machine.
Color
In one embodiment, the particles are colored and the automatic dishwashing liquid detergent composition is clear or translucent, so as to make the liquid automatic dishwashing product aesthetically pleasing. In another embodiment, the particles and the liquid automatic dishwashing detergent composition are both colored and the color of the particles is matched to the base color of the liquid composition. In one embodiment, the particles have a dark green color whereas the liquid composition has a light green color. Other preferred color combinations for the polymeπc coating on the particles and the liquid automatic dishwashing composition are: blue:blue, blue:whιte, gree green, greemwhite and green:yellow, respectively.
Desirably, the particles comprise from about 0.1% to about 5.0% by weight of the liquid composition, and preferably, from about 0.2% to about 1.0% by weight of the liquid composition. In another embodiment of the present invention, a non-stammg colored composite particle suitable for incorporation in a bleach-contammg liquid detergent composition is disclosed. The particle is made by the process as set forth above. Particles
The particles can be formed from vaπous mateπals that do not cause any detπmental affect upon the performance of the liquid detergent. Preferably, the particles are in the form of pπlls. The prills typically have a core which is coated with a polymeπc coating as descπbed before. The core can be made from sucrose, as an example. The method of forming pπlls is well known to those skilled m the art and is disclosed m the literature, such as for example, in U.S. Patent No. 4,965,012, which is incorporated herein by reference.
The particles can be of vaπous sizes and shapes, such as spheπcal, oval, cyhndπcal or polygonal and desirably have a particle size in a range of from about 200 μm to about 5000 μm, preferably, from about 400 μm to about 2000 μm, and most preferably, from about 500 μm to about 850 μm.
In yet another embodiment of the present invention, a liquid automatic dishwashing detergent product is disclosed. The product includes a liquid dishwashing detergent composition containing chlorine bleach, and non-stammg colored composite particles. The particles are made by the process as set forth above. Liquid automatic dishwashing composition components
The liquid automatic dishwashing detergent product is highly viscous in a quiescent state and has a relatively high yield stress values. When subjected to shear stresses, however, such as being shaken m a container or squeezed through an orifice, the product quickly fluidizes and upon cessation of the applied shear stress, quickly reverts to a high viscosity state. The above liquid automatic dishwashing detergent product is preferably low foaming, readily soluble in the washing medium and most effective at pH values best conducive to improved cleaning performance, such as in a range of desirably from about pH 7.0 to about pH 13.0, and preferably from about pH 8.0 to about pH 12.0.
The physical stability of the liquid product may be improved and the thickness of the liquid product may be altered by the addition of a cross linking polyacrylate thickener to the liquid detergent product as a thixotropic thickener. PH admstmg components
The pH adjusting components are desirably selected from sodium or potassium carbonate or sesquicarbonate, sodium or potassium silicate, citπc acid, sodium or potassium bicarbonate, sodium or potassium borate, sodium or potassium hydroxide, and mixtures thereof. NaOH or
KOH are the preferred ingredients for increasing the pH to withm the above ranges. Other preferred pH adjusting ingredients are sodium carbonate, potassium carbonate, and mixtures thereof.
Low Foaming Surfactant
Chloπne bleach stable low foaming surfactants are preferred and such surfactants are present in a range of from about 0.1% to about 10% by weight of the liquid composition. Such surfactants are generally known to one skilled m the art and need not be elaborated here, for purposes of brevity. One example of such a surfactant is an aniomc surfactant commercially available under the trade name Dowfax.
Other ingredients
The liquid automatic dishwashing detergent composition optionally also contains from about 0.5% to about 20% of a dispersant polymer selected from the group consisting of polyacrylates and polyacrylate copolymers, and from about 0.1% to about 5% of a chloπne bleach stable foam suppressant. Such foam suppressants are well known to those skilled in the art.
To exemplify vaπous embodiments of the present invention, Sample A of the liquid automatic dishwashing detergent product composition is formulated using the below named ingredients, as set forth in Example A.
EXAMPLE A Ingredient (weight % active) A Sodium Tπpolyphosphate 17.5
Potassium Tπpolyphosphate —
Sodium Silicate 6.0
Potassium hydroxide 3.6
Sodium hydroxide 2.0
Polyacrylate polymer 1.0
Nitric Acid 0.012
Perfume 0.03
Nomonic surfactant —
Sodium Benzoate 0.75
Sodium hypochloπte 1.15
Polyacrylate polymer thickener 1.5
Dye solution —
Solid Pπll 0.5
Water Bal.
TOTAL 100.0
In the above composition, the non-staining colored particles having a sphencal shape, and a diameter of about 750 μm, are formed from a sucrose core coated with a polymeπc coating formed from methyl cellulose (Methocel A15LV), and having a bluish-green color. The bluish- green color is imparted by adding a pigment into the methyl cellulose coating before spraying it on the particle according to the process of the present invention. The particles compπse about 0.1% to about 5% by weight of the liquid composition. The optimum methyl cellulose coating is about 5% by weight of the particle. The coating is sprayed on the sucrose core particle by spraying a 5% by weight aqueous solution of methyl cellulose with pigment. The aqueous solution temperature being carefully maintained at about 35 °C. The size of the pigment particles in the aqueous solution is no greater than about 1 μm.
The resultant particles are insoluble in the liquid composition but are soluble m the wash solution duπng automatic dishwashing. The resultant colored particles are also non-stammg to plastic surfaces.
Accordingly, having thus described the invention in detail, it will be obvious to those skilled in the art that vaπous changes may be made without departing from the scope of the invention and the invention is not to be considered limited to what is described in the specification.

Claims

WHAT IS CLAIMED IS:
1 A process for forming a non-stammg colored composite particle suitable for incorporation in a bleach-contammg liquid detergent composition, characterized by the steps of forming a colored liquid dispersion of pigment particles in a first liquid medium, wherein the size of said pigment particles in said colored liquid dispersion is no greater than 5 μm; mixing said colored liquid dispersion with a polymeπc mateπal and a second liquid medium to form a sprayable colored polymeπc mateπal, said polymeπc material being selected from the group consisting of alkyl cellulose ethers and polyvmyl alcohol; and spraying said colored polymeπc mateπal on a composite particle, and forming a colored polymeπc coating on said composite particle.
2. The process according to claim 1 , wherein the size of said pigment particles in said colored liquid dispersion is no greater than 1 μm.
3. The process according to any of claims 1-2, wherein the size of said pigment particles in said colored liquid dispersion is no greater than 0J μm.
4. The process according to any of claims 1-3, wherein the size of said pigment particles in said colored liquid dispersion is no greater than 0.01 μm.
5. The process according to any of claims 1 -4, wherein the first liquid medium is water
6. The process according to any of claims 1-5, wherein the first liquid medium is water mixed with up to about 10% by weight of a nomonic surfactant.
7 The process according to any of claims 1-6, further including the step of maintaining the amount of surfactants used in said bleach-contammg liquid detergent composition at a preselected value such that when the bleach-contammg liquid detergent composition is diluted in a wash solution, the amount of surfactant delivered in the wash solution is less than cπtical rnicell concentration.
8. The process according to any of claims 1-7, wherein said composite particle remains insoluble in said bleach-containing liquid detergent composition but soluble in automatic dishwashing wash solution.
9. The process according to any of claims 1-8, wherein said colored polymeπc coating is soluble in an automatic dishwashing wash solution and leaves no significant residue.
10. The process according to any of claims 1-9, wherein the step of spraying said colored polymeπc material on a composite particle includes the step of forming a sprayable aqueous solution of a polymeric mateπal, said polymeric mateπal being present in said sprayable aqueous solution in an amount in a range of from 1% to 20% by weight.
PCT/US2000/010386 1999-04-19 2000-04-18 Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition Ceased WO2000063341A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CA002368600A CA2368600C (en) 1999-04-19 2000-04-18 Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition
EP00923464A EP1171569A1 (en) 1999-04-19 2000-04-18 Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition
US09/937,356 US6730652B1 (en) 1999-04-19 2000-04-18 Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition
AU43582/00A AU4358200A (en) 1999-04-19 2000-04-18 Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition
JP2000612420A JP2002542383A (en) 1999-04-19 2000-04-18 Method for producing non-dyed colored particles for improving the appearance of liquid automatic dishwashing detergent products, said particles and compositions

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US13004499P 1999-04-19 1999-04-19
US60/130,044 1999-04-19

Publications (1)

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Publication number Priority date Publication date Assignee Title
FI116125B (en) * 2001-07-02 2005-09-30 Sandvik Tamrock Oy Type of device

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EP0286773A2 (en) * 1987-04-17 1988-10-19 Ecolab Inc. Water insoluble encapsulated enzymes protected against deactivation by halogen bleaches
US5719115A (en) * 1993-07-05 1998-02-17 Henkel Kommanditgesellschaft Auf Aktien Coated enzyme preparation for detergents and cleaning formulations
WO1998016615A1 (en) * 1996-10-15 1998-04-23 The Procter & Gamble Company Colored particulate compositions
US5879920A (en) * 1991-10-07 1999-03-09 Genencor International, Inc. Coated enzyme-containing granule

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GB990252A (en) * 1961-03-10 1965-04-28 Procter & Gamble Agglomeration process for making granular detergent compositions
EP0286773A2 (en) * 1987-04-17 1988-10-19 Ecolab Inc. Water insoluble encapsulated enzymes protected against deactivation by halogen bleaches
US5879920A (en) * 1991-10-07 1999-03-09 Genencor International, Inc. Coated enzyme-containing granule
US5719115A (en) * 1993-07-05 1998-02-17 Henkel Kommanditgesellschaft Auf Aktien Coated enzyme preparation for detergents and cleaning formulations
WO1998016615A1 (en) * 1996-10-15 1998-04-23 The Procter & Gamble Company Colored particulate compositions

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EP1627909A1 (en) * 2004-07-22 2006-02-22 The Procter & Gamble Company Detergent compositions comprising coloured particles
WO2006020162A1 (en) * 2004-07-22 2006-02-23 The Procter & Gamble Company Detergent compositions comprising coloured particles
US7645729B2 (en) 2004-07-22 2010-01-12 The Procter & Gamble Company Detergent compositions comprising coloured particles
EP2248884A1 (en) * 2004-07-22 2010-11-10 The Procter & Gamble Company Detergent Compositions Comprising Coloured Particles

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AU4358200A (en) 2000-11-02
CA2368600A1 (en) 2000-10-26
EP1171569A1 (en) 2002-01-16
JP2002542383A (en) 2002-12-10
CA2368600C (en) 2005-04-05

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