WO2000063332A2 - Process for coating a particle with a polymeric coating having unique dissolution characteristics - Google Patents

Process for coating a particle with a polymeric coating having unique dissolution characteristics Download PDF

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Publication number
WO2000063332A2
WO2000063332A2 PCT/US2000/010390 US0010390W WO0063332A2 WO 2000063332 A2 WO2000063332 A2 WO 2000063332A2 US 0010390 W US0010390 W US 0010390W WO 0063332 A2 WO0063332 A2 WO 0063332A2
Authority
WO
WIPO (PCT)
Prior art keywords
water
cellulose ether
alkyl cellulose
coating
range
Prior art date
Application number
PCT/US2000/010390
Other languages
French (fr)
Other versions
WO2000063332A3 (en
Inventor
Jeffrey Donald Painter
Joseph Herbert Thien
Eugene Steven Sadlowski
Original Assignee
The Procter & Gamble Company
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 The Procter & Gamble Company filed Critical The Procter & Gamble Company
Priority to AU43585/00A priority Critical patent/AU4358500A/en
Publication of WO2000063332A2 publication Critical patent/WO2000063332A2/en
Publication of WO2000063332A3 publication Critical patent/WO2000063332A3/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082Special 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
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039Coated compositions or coated components in the compositions, (micro)capsules
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/222Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • C11D3/225Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC

Definitions

  • the present invention generally relates to liquid detergent compositions More particularly, the invention relates to a process for coating particles which are useful in liquid detergent compositions, with a minimum but effective amount of a protective polymeric alkyl cellulose ether coating which remains insoluble in the liquid detergent composition but becomes soluble in the wash solution.
  • liquid detergent products such as liquid automatic dishwashing (ADW), liquid hand dishwashing formulas (LDLs), or liquid laundry detergent products prefer that these products having a pleasing color or appearance.
  • ADW liquid automatic dishwashing
  • LDLs liquid hand dishwashing formulas
  • liquid laundry detergent products prefer that these products having a pleasing color or appearance.
  • Providing a pleasing color to the liquid detergent is one way of improving its appearance.
  • Adding solid particles which are suspended in a liquid detergent composition is another way to improve the aesthetics of the product.
  • Another way is to make the particles colored and match their color to the base color of the liquid detergent composition to create a pleasing combination of colors.
  • the invention meets the needs above by providing a process for coating a solid or composite particle with a protective alkyl cellulose ether polymeric coating which is insoluble in a liquid detergent product but soluble in the wash solution of the liquid detergent product.
  • the process comprises the following steps An alkyl cellulose ether polymer is dispersed in water.
  • the temperature of the water is at least about 60 °C.
  • the alkyl cellulose ether polymer and water are present in a weight ratio in a range of from about 1:99 to about 30:70, polyme ⁇ water.
  • the alkyl cellulose ether polymer in water dispersion is then cooled to a temperature below at least about 40 °C and a sprayable alkyl cellulose ether polymer in water solution is formed.
  • the sprayable alkyl cellulose ether polymer in water solution is sprayed on the solid or composite particle while the temperature of the sprayable solution is simultaneously maintained below about 40 °C.
  • a coating of the alkyl cellulose ether on the solid or composite particle is formed.
  • liquid dishwashing detergent composition By “liquid dishwashing detergent composition”, “liquid dishwashing composition” or “liquid dishwashing detergent product” it is meant a detergent composition that is employed in manual (i.e. hand) or automatic dishwashing
  • liquid dishwashing detergent product it is meant a detergent composition that is employed in manual (i.e. hand) or automatic dishwashing
  • the hydration is accomplished by the step of dispersing an alkyl cellulose ether polymer in water m a weight ratio in a range of from about 1 99 to about 30:70, polymer-water and forming a sprayable alkyl cellulose ether polymer in water solution.
  • the weight ratio of polymer to water is m a range of from about 1:99 to about 20:80, preferably from about 3-97 to about 10:90, more preferably from about 4-96 to about 6-94. and most preferably about 5:95
  • the dispersion is accomplished in a contained equipped with a stirring device
  • the temperature of the water during the stirring is maintained above about 60 °C, desirably, in a range of from about 60 °C to about 90 °C, preferably from about 60 °C to about 80 °C, and most preferably from about 70 °C to about 80 °C.
  • the alkyl cellulose ether polymer in water dispersion is cooled to a temperature below at least about 40 °C to assure adequate hydration of the methyl cellulose in the water to form a solution of alkyl cellulose ether in water.
  • the temperature of sprayable alkyl cellulose ether polymer in water solution is desirably maintained below about 40 °C while spraying this solution on the particle
  • the temperature of the solution is preferably maintained within a range of from about 30 °C to about 40 °C, more preferably in a range of from about 32 °C to about 38 °C, even more preferably in a range of from about 33 °C to about 37 °C and most preferably at a temperature of about 35 °C.
  • the coating is desirably present in 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 detrimentally contribute to unwanted residue deposition in the washing machine.
  • the pH value of the sprayable solution is maintained withm a range of from about pH 8.0 to about pH 9.5, and preferably, from about pH 8.5 to about pH 9.0. It is desirable to maintain withm the above pH range to allow for full solubihzation of the methyl cellulose in water before spraying.
  • the colored polymeric coating is insoluble in a liquid automatic dishwashing detergent composition but soluble in the wash solution.
  • the coating is prepared from alkyl cellulose ethers.
  • the alkyl cellulose ethers are 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 polyvinyl alcohol
  • PVA having a molecular weight, desirably in 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.
  • Helium pycnometry measurement devices are well-known to those skilled in the art and available from the Micromet ⁇ cs Co.
  • Polyacrylate polymer 1 0 — — — — —

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Emergency Medicine (AREA)
  • Detergent Compositions (AREA)

Abstract

A process for coating a solid or composite particle with a protective alkyl cellulose ether polymeric coating which is insoluble in a liquid detergent product but soluble in the wash solution of the liquid detergent product is disclosed. In this process, an alkyl cellulose ether polymer is dispersed in water. The temperature of the water is at least about 60 °C. The alkyl cellulose ether polymer in water dispersion is then cooled to a temperature below at least about 40 °C and a sprayable alkyl cellulose ether polymer in water solution is formed which is then sprayed on the solid or composite particle while the temperature of the sprayable solution is simultaneously maintained below about 40 °C. A coating of the alkyl cellulose ether on the solid or composite particle is formed.

Description

PROCESS FOR COATING A PARTICLE WITH A POLYMERIC COATING HAVING UNIQUE DISSOLUTION CHARACTERISTICS
TECHNICAL FIELD
The present invention generally relates to liquid detergent compositions More particularly, the invention relates to a process for coating particles which are useful in liquid detergent compositions, with a minimum but effective amount of a protective polymeric alkyl cellulose ether coating which remains insoluble in the liquid detergent composition but becomes soluble in the wash solution.
BACKGROUND OF THE INVENTION
It has been recognized that consumers of liquid detergent products, such as liquid automatic dishwashing (ADW), liquid hand dishwashing formulas (LDLs), or liquid laundry detergent products prefer that these products having a pleasing color or appearance. Providing a pleasing color to the liquid detergent is one way of improving its appearance. Adding solid particles which are suspended in a liquid detergent composition is another way to improve the aesthetics of the product. Another way is to make the particles colored and match their color to the base color of the liquid detergent composition to create a pleasing combination of colors.
In the past, in an effort to improve the aesthetics of a liquid detergent products, the particles added to these products have been coated with thick waxy or wax-based coatings This has a major disadvantage of detrimentally causing filming, particularly on glass, stainless steel and plastic surfaces because the water-insoluble waxes melt and are released into the wash solution duπng the high temperature encountered during an automatic dishwashing process.
It has been desirable to have a process for forming a coating on a particle for a liquid dishwashing product that does not cause a significant amount of unwanted filming on glass, stainless steel and plastic. In view of the foregoing, it has thus been desirable to have a process for coating particles which are useful in liquid detergent compositions for improvement or aesthetics, with a minimum but effective amount of a protective polymeric alkyl cellulose ether coating which remains insoluble in the liquid detergent composition but becomes soluble in the wash solution. The inventors of the present invention have discovered a process for coating particles with a minimum but effective amount of a protective polymeric alkyl cellulose ether coating which remains insoluble in the liquid detergent composition but becomes soluble in the wash solution. 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 coating a solid or composite particle with a protective alkyl cellulose ether polymeric coating which is insoluble in a liquid detergent product but soluble in the wash solution of the liquid detergent product.
In one aspect of the present invention, the process comprises the following steps An alkyl cellulose ether polymer is dispersed in water. The temperature of the water is at least about 60 °C. The alkyl cellulose ether polymer and water are present in a weight ratio in a range of from about 1:99 to about 30:70, polymeπwater. The alkyl cellulose ether polymer in water dispersion is then cooled to a temperature below at least about 40 °C and a sprayable alkyl cellulose ether polymer in water solution is formed. Then, the sprayable alkyl cellulose ether polymer in water solution is sprayed on the solid or composite particle while the temperature of the sprayable solution is simultaneously maintained below about 40 °C. A coating of the alkyl cellulose ether on the solid or composite particle is formed.
DETAILED DESCRIPTION OF THE INVENTION Definitions - By "liquid dishwashing detergent composition", "liquid dishwashing composition" or "liquid dishwashing detergent product" it is meant a detergent composition that is employed in manual (i.e. hand) or automatic dishwashing Without being bound to any particular theory, it has been discovered that when an alkyl cellulose ether polymer is sufficiently hydrated before spraying on the particle or prill, the resultant polymer coating on the particle or prill remains stable, unbroken and undissoHed in the liquid dishwashing composition The Process In the preferred embodiment of the present invention, the hydration is accomplished by the step of dispersing an alkyl cellulose ether polymer in water m a weight ratio in a range of from about 1 99 to about 30:70, polymer-water and forming a sprayable alkyl cellulose ether polymer in water solution. Desirably, the weight ratio of polymer to water is m a range of from about 1:99 to about 20:80, preferably from about 3-97 to about 10:90, more preferably from about 4-96 to about 6-94. and most preferably about 5:95 The dispersion is accomplished in a contained equipped with a stirring device The temperature of the water during the stirring is maintained above about 60 °C, desirably, in a range of from about 60 °C to about 90 °C, preferably from about 60 °C to about 80 °C, and most preferably from about 70 °C to about 80 °C. After dispersing the alkyl cellulose ether m water as described above, the alkyl cellulose ether polymer in water dispersion is cooled to a temperature below at least about 40 °C to assure adequate hydration of the methyl cellulose in the water to form a solution of alkyl cellulose ether in water. In the preferred embodiment, the temperature of sprayable alkyl cellulose ether polymer in water solution is desirably maintained below about 40 °C while spraying this solution on the particle The temperature of the solution is preferably maintained within a range of from about 30 °C to about 40 °C, more preferably in a range of from about 32 °C to about 38 °C, even more preferably in a range of from about 33 °C to about 37 °C and most preferably at a temperature of about 35 °C.
In the preferred embodiment, the coating is desirably present in 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 detrimentally contribute to unwanted residue deposition in the washing machine. In the preferred embodiment, the pH value of the sprayable solution is maintained withm a range of from about pH 8.0 to about pH 9.5, and preferably, from about pH 8.5 to about pH 9.0. It is desirable to maintain withm the above pH range to allow for full solubihzation of the methyl cellulose in water before spraying.
It has been surprisingly found that by using the above process steps, a protective methyl cellulose polymeric coating is formed, which is insoluble in a liquid detergent product but soluble m the wash solution of the liquid detergent product, while at the same time, requiring only about 5% polymer by weight of the particle. This offers an advantage because by using a smaller the quantity of polymer used for coating the prill or particle, there is a reduction in the amount of polymer residue that can potentially re-deposit on the dishware and dishwasher, when the particle dissolves in the wash solution. Polymeric coating
In the preferred embodiment, the colored polymeric coating is insoluble in a liquid automatic dishwashing detergent composition but soluble in the wash solution. The coating is prepared from alkyl cellulose ethers. Desirably, the alkyl cellulose ethers are 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 polyvinyl alcohol
(PVA) having a molecular weight, desirably in 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.
Accordingly, having thus described the invention in detail, it will be obvious to those skilled m 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.
Methods for measuπng density are well known to those skilled in the art. Without limiting the scope of the invention, examples of these methods for liquids can be found in Vogels Textbook of Practical Organic Chemistry (Fourth Edition), 1978, published by Longman Inc,
New York. A preferred method for measuπng the density of a solid helium pycnometry. Helium pycnometry measurement devices are well-known to those skilled in the art and available from the Micrometπcs Co.
Examples of typical hand and automatic liquid dishwashing formulas are outlined below. Detailed descriptions of typical hand and automatic liquid dishwashing ingredients can be found in U. S. Pat. No. 6,020,294, issued February 1, 2000, to Getty, et al., U. S. Pat. No. 5,912,218, issued June 15, 1999, to Chatterjee, et al.; [New LDL3 application will be added]; U.S. Pat. No 5,415,814 issued 16 May 1995. to Ofosu-Asante et al. All of these references are hereby incorporated by reference.
EXAMPLE A
Ingredient (weight % active) A B C D E
Sodium Tπpolyphosphate 17 5 16.0 — 8 0 16.0
Potassium Tπpolyphosphate — — 16.0 8 0 16.0
Sodium Silicate 6 0 1.0 — — —
Potassium hydroxide 3 6 5.6 5 6 1 0 1 0
Sodium hydroxide 2 0 2.0 2 0 — —
Polyacrylate polymer 1 0 — — — —
Nomonic surfactant ... 0.5 0 8 0 7 1.5 -
Sodium hypochloπte 1.15 — — — —
Polvacrylate polymer thickener 1.5 1.5 1.5 1.5 1.0
Solid Prill 0.5 0.5 0.5 0.5 0.7
Protease enzyme — — — — 0.01
Water and minors Bal. Bal. Bal. Bal. Bal.
TOTAL 100.0 100.0 100.0 100.0 100.0
1 ΞXAMPLE B
Composition
Ingredient F G H
% Weight
Ammonium Ci 2-13 alkyl ethoxy / 1) 28.0 27.0 26.0 sulfate
Coconut amme oxide 4.5 6.0 2.5
Alcohol Ethoxylate CgEi 1 5.0 — 5.0
Ammonium xylene sulfonate — 4.0 4.0
Ethanol 4.0 4.0 4.0
Magnesium chloride 3.3 3.3 3.3
Amylase enzyme — — 0.001
Prills 1.0 0.5 1.0
Thixcin 0.5 0.1 —
Water and minors Balance -

Claims

WHAT IS CLAIMED IS:
1. A process for coating a solid or composite particle with a protective alkyl cellulose ether polymeric coating which is insoluble in a liquid detergent product but soluble in the wash solution of the liquid detergent product, characterized by the steps of: dispersing alkyl cellulose ether polymer m water wherein the temperature of said water is at least 60 °C, and wherein said alkyl cellulose ether polymer and said water are present in a weight ratio in a range of from 1 :99 to 30:70, polymeπwater; cooling said alkyl cellulose ether polymer in water dispersion to a temperature below at least 40 °C and forming a sprayable alkyl cellulose ether polymer in water solution; spraying said sprayable alkyl cellulose ether polymer in water solution on said solid or composite particle while simultaneously maintaining the temperature of said sprayable solution below 40 °C; and forming a coating of said alkyl cellulose ether on said solid or composite particle.
2. The process according to claim 1, including dispersing said alkyl cellulose ether polymer in said water m a weight ratio in a range of from 3:97 to 10:90, polymer:water.
3. The process according to any of claims 1-2, including dispersing said alkyl cellulose ether polymer in said water in a weight ratio in a range of from 4:96 to 6:94, polymeπwater.
4 The process according to any of claims 1-3, wherein the temperature of the water duπng said dispersion step is maintained in a range of from 60 °C to 90 °C
5. The process according to any of claims 1-4, wherein the temperature of the water during said dispersion step is maintained in a range of from 60 °C to 80 °C.
6. The process according to any of claims 1-5, including maintaining the temperature of said sprayable solution withm a range of from 33 °C to 37 °C.
7. The process according to any of claims 1-6, wherein said alkyl cellulose ether is methyl cellulose.
8. The process according to any of claims 1-7, wherein said coating is present in an amount in a range of from 1% to 25% by weight of said particle.
9. The process according to any of claims 1 -8 including the step of maintaining the pH value of said sprayable solution in a range of from pH 8.0 to pH 9.5
10. A liquid dishwashing detergent composition characterized by less than 50% free water and from 0.02% to 2.5% of the solid or composite particles prepared according to the process of claim 1.
PCT/US2000/010390 1999-04-19 2000-04-18 Process for coating a particle with a polymeric coating having unique dissolution characteristics WO2000063332A2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU43585/00A AU4358500A (en) 1999-04-19 2000-04-18 Process for coating a particle with a polymeric coating having unique dissolution characteristics

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US13004399P 1999-04-19 1999-04-19
US60/130,043 1999-04-19

Publications (2)

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WO2000063332A2 true WO2000063332A2 (en) 2000-10-26
WO2000063332A3 WO2000063332A3 (en) 2001-02-22

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3128336A1 (en) * 1981-07-17 1983-01-27 Henkel KGaA, 4000 Düsseldorf "METHOD FOR PRODUCING COATED NUCLEAR BLEACHING ACTIVATORS"
EP0298222A2 (en) * 1987-07-10 1989-01-11 Ecolab Inc. Encapsulated bleaches
GB2309974A (en) * 1996-02-08 1997-08-13 Procter & Gamble Use of cellulose ethers for soil removal
GB2309975A (en) * 1996-02-08 1997-08-13 Procter & Gamble Use of cellulose ethers in dishwashing

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3128336A1 (en) * 1981-07-17 1983-01-27 Henkel KGaA, 4000 Düsseldorf "METHOD FOR PRODUCING COATED NUCLEAR BLEACHING ACTIVATORS"
EP0298222A2 (en) * 1987-07-10 1989-01-11 Ecolab Inc. Encapsulated bleaches
GB2309974A (en) * 1996-02-08 1997-08-13 Procter & Gamble Use of cellulose ethers for soil removal
GB2309975A (en) * 1996-02-08 1997-08-13 Procter & Gamble Use of cellulose ethers in dishwashing

Also Published As

Publication number Publication date
WO2000063332A3 (en) 2001-02-22
AU4358500A (en) 2000-11-02

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