CA1204562A - Method for preparing fabric softening compositions - Google Patents
Method for preparing fabric softening compositionsInfo
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- CA1204562A CA1204562A CA000451506A CA451506A CA1204562A CA 1204562 A CA1204562 A CA 1204562A CA 000451506 A CA000451506 A CA 000451506A CA 451506 A CA451506 A CA 451506A CA 1204562 A CA1204562 A CA 1204562A
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-
- 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
- C11D3/2003—Alcohols; Phenols
- C11D3/2006—Monohydric alcohols
- C11D3/201—Monohydric alcohols linear
- C11D3/2013—Monohydric alcohols linear fatty or with at least 8 carbon atoms in the alkyl chain
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
-
- 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
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/001—Softening compositions
- C11D3/0015—Softening compositions liquid
-
- 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
- C11D3/2003—Alcohols; Phenols
- C11D3/2006—Monohydric alcohols
- C11D3/201—Monohydric alcohols linear
-
- 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
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2079—Monocarboxylic acids-salts 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2093—Esters; Carbonates
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- 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)
- Emergency Medicine (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
A B S T R A C T
A process for preparing an aqueous liquid fabric softening composition comprising making a hot molten mixture of a cationic fabric softener and a nonionic material with a low HLB, such as a fatty acid, fatty ester, fatty alcohol or lanolin, adding the molten mixture to water while still hot, mixing to form a dispersion of droplets in the water and thereafter adding an electrolyte such as a salt of lithium, sodium, potassium, calcium, magnesium or aluminium. By forming the dispersion before adding the electrolyte, the viscosity of the end product is reduced and long term stability is improved.
A process for preparing an aqueous liquid fabric softening composition comprising making a hot molten mixture of a cationic fabric softener and a nonionic material with a low HLB, such as a fatty acid, fatty ester, fatty alcohol or lanolin, adding the molten mixture to water while still hot, mixing to form a dispersion of droplets in the water and thereafter adding an electrolyte such as a salt of lithium, sodium, potassium, calcium, magnesium or aluminium. By forming the dispersion before adding the electrolyte, the viscosity of the end product is reduced and long term stability is improved.
Description
- 1 C. 1362 METHOD FOR PREPARING FABP.IC SOFTE21ING COMPC)SITIONS
.
~hP present invention relates to a method of prepaxing fabric softening compositions, in particular for preparing concentrated aqueous liquid fabric softening compositions containing water-insoluble cationic fabric softenins cents and fatty acids or other nonionic materials with a low HLB.
It is known from GB 039 556 ~U~-lLEV~ - Case C.567~ to fox~l aqueous liquid fabric softening compositions containing up to 20~ of a mixture of a water-insoluble cationic matexial and fatty acid, the fatty acid acting to improve the efficiency of softening, thereby enabling the level of the cationic material to be reduced withsut loss of performance. It is also known from EP 13780-A lPROCTER & GALE to form concentrated aqueous liquid fabric softening compositions from a mixture of a water-insoluble cationic material and a nonionic material selected from hydrocarbons, fatty acids, fatty esters and fatty alcohols, the nonionic material acting to improve the viscosity characteristics of the , 5;~
.
~hP present invention relates to a method of prepaxing fabric softening compositions, in particular for preparing concentrated aqueous liquid fabric softening compositions containing water-insoluble cationic fabric softenins cents and fatty acids or other nonionic materials with a low HLB.
It is known from GB 039 556 ~U~-lLEV~ - Case C.567~ to fox~l aqueous liquid fabric softening compositions containing up to 20~ of a mixture of a water-insoluble cationic matexial and fatty acid, the fatty acid acting to improve the efficiency of softening, thereby enabling the level of the cationic material to be reduced withsut loss of performance. It is also known from EP 13780-A lPROCTER & GALE to form concentrated aqueous liquid fabric softening compositions from a mixture of a water-insoluble cationic material and a nonionic material selected from hydrocarbons, fatty acids, fatty esters and fatty alcohols, the nonionic material acting to improve the viscosity characteristics of the , 5;~
- 2 - C.1362 product when the level of cationic material i6 above 8%.
It is also known from Go 2 039 556 and EP 13780 that preferred compositions can also include low levels of electrolyte such as respectively sodium chloride or calcium chloride, to further control product viscosity.
It is found that when such a composition is prepared by dispersing a pre-mix of the cationic and nonionic materials in water to which the electrolyte has already been added, followed by thorough mixing, the viscosity of the end product is often still higher than desired, particularly when the total active level exceeds about 8 It has been proposed in EP 52517 (PROCTER & GAMBLE) that where the composition is based on a mixture of cationic materials, some electrolyte is added, together with a premix of the cationic materials, to water with vigorous agitation and thereafter a remaining portion of the electrolyte is added. Also in US 3 681 241 (RUDY it is proposed that compositions based on a mixture of ~ationic materials are preferably formed in such a manner as to be substantially free of electrolytes, electrolytes being optionally added to the resultiny product to regulate the viscosity thereof. Further, GB 1 104 441 (UNILEV~R) discloses that products based on a cationic softener and a fatty acid ethanolamide may be made by adding water to a premix of the cationic and nonionic and then, after cooling, adding an electrolyte such as sodium carbonate to thin the product.
We have surprisingly found that, where the composition is based on a mixture of a cationic fabric softener and a nonionic material of low ~LB, and is formed by adding a premix of the ~ationic and the nonionic to water, if the electrolyte is added only after the mixing stage but not before, the end product viscosity is lower.
It is also known from Go 2 039 556 and EP 13780 that preferred compositions can also include low levels of electrolyte such as respectively sodium chloride or calcium chloride, to further control product viscosity.
It is found that when such a composition is prepared by dispersing a pre-mix of the cationic and nonionic materials in water to which the electrolyte has already been added, followed by thorough mixing, the viscosity of the end product is often still higher than desired, particularly when the total active level exceeds about 8 It has been proposed in EP 52517 (PROCTER & GAMBLE) that where the composition is based on a mixture of cationic materials, some electrolyte is added, together with a premix of the cationic materials, to water with vigorous agitation and thereafter a remaining portion of the electrolyte is added. Also in US 3 681 241 (RUDY it is proposed that compositions based on a mixture of ~ationic materials are preferably formed in such a manner as to be substantially free of electrolytes, electrolytes being optionally added to the resultiny product to regulate the viscosity thereof. Further, GB 1 104 441 (UNILEV~R) discloses that products based on a cationic softener and a fatty acid ethanolamide may be made by adding water to a premix of the cationic and nonionic and then, after cooling, adding an electrolyte such as sodium carbonate to thin the product.
We have surprisingly found that, where the composition is based on a mixture of a cationic fabric softener and a nonionic material of low ~LB, and is formed by adding a premix of the ~ationic and the nonionic to water, if the electrolyte is added only after the mixing stage but not before, the end product viscosity is lower.
- 3 - C.1362 This enables the level of electrolyte used to be reduced without detriment to the properties of the product. It has also surprisingly been found that this post-addition of electrolyte can improve the long term stability of the product.
Thus, according to the invention there is provided a process for preparing a cGncentrated aqueous liquid fabric softening composition containing at least 8% by weight water-insoluble cationic fabric softener, said process comprising the steps ofO
( i) forming a molten mixture containing the water-insoluble cationic fabric softener and a nonionic material having an HLB of not more than lo;
( ii) addir.g the molten mixture to water at an elevated temperature;
(iii) mixinq the molten mixture and the water together to form a dispersion of the molten mixture in droplet form in the water; and ivl adding electrolyte in the form of a source of lithium, sodium, potassium, calcium, magnesium or aluminium ions thereto, characterised in that the electrolyte is added after, but not before, the formation of said dispersion.
The water insoluble cationic fabric softener can be any fabric-substantive cationic compound that has a solubility in water at pi 2.5 and 20C of less than 10 g/l. Highly preferred materials are quaternary ammonium salts having two C12-C2~ alkyl or alkenyl chains, optionally substituted or interrupted by functional groups such as OH, C -CONH, -COO-, etc.
6~
Thus, according to the invention there is provided a process for preparing a cGncentrated aqueous liquid fabric softening composition containing at least 8% by weight water-insoluble cationic fabric softener, said process comprising the steps ofO
( i) forming a molten mixture containing the water-insoluble cationic fabric softener and a nonionic material having an HLB of not more than lo;
( ii) addir.g the molten mixture to water at an elevated temperature;
(iii) mixinq the molten mixture and the water together to form a dispersion of the molten mixture in droplet form in the water; and ivl adding electrolyte in the form of a source of lithium, sodium, potassium, calcium, magnesium or aluminium ions thereto, characterised in that the electrolyte is added after, but not before, the formation of said dispersion.
The water insoluble cationic fabric softener can be any fabric-substantive cationic compound that has a solubility in water at pi 2.5 and 20C of less than 10 g/l. Highly preferred materials are quaternary ammonium salts having two C12-C2~ alkyl or alkenyl chains, optionally substituted or interrupted by functional groups such as OH, C -CONH, -COO-, etc.
6~
- 4 - C.1362 Well known species of substantially water-insoluble quaternary ammonium compounds have the fo~ula R~ R3 N X
R2 ~4 wherein l and R~ represent hydrocarbyl groups of from about 12 to about 24 carbon atoms; R3 and R4 represent hydrocarbyl groups containing from 1 to about 4 carbon atoms; and X is an anion, preferably selected from halide, methyl sulfate and ethyl sulfate radicals. representative examples of these quaternary softeners include ditallow dimekhyl ammonium chloride; ditallow dimethyl ammonium methyl sulfate; dihexadecyl dimethyl amm~nium chloride;
di(hydxogenated tallow alkyl~ dimethyl ammonium chloride;
dioctadecyl dimethyl ammonium chloride; dieicosyl dimethyl ammonium chloride; didocosyl dimethyl ammonium chloride;
di~hydrogenated tallow dimethyl ammonium methyl sulfate;
dihexadecyl diethyl ammonium chloxid~; di(coconut alkyl) dimethyl ammonium chlorideO Ditallow dimethyl ammor.ium chloride, di(hydrogena~ed tallow alkyl) dimethyl ammonium chloride, di(coconut alkyl~ dime~hyl ammonium chloride and dilcoconut alkyl) dimethyl ammonium methosulfate are preferred.
Another class of preferred water-insoluble cationic matexial~ are the alkylimidazolinium salts believed to have the formula:
R2 ~4 wherein l and R~ represent hydrocarbyl groups of from about 12 to about 24 carbon atoms; R3 and R4 represent hydrocarbyl groups containing from 1 to about 4 carbon atoms; and X is an anion, preferably selected from halide, methyl sulfate and ethyl sulfate radicals. representative examples of these quaternary softeners include ditallow dimekhyl ammonium chloride; ditallow dimethyl ammonium methyl sulfate; dihexadecyl dimethyl amm~nium chloride;
di(hydxogenated tallow alkyl~ dimethyl ammonium chloride;
dioctadecyl dimethyl ammonium chloride; dieicosyl dimethyl ammonium chloride; didocosyl dimethyl ammonium chloride;
di~hydrogenated tallow dimethyl ammonium methyl sulfate;
dihexadecyl diethyl ammonium chloxid~; di(coconut alkyl) dimethyl ammonium chlorideO Ditallow dimethyl ammor.ium chloride, di(hydrogena~ed tallow alkyl) dimethyl ammonium chloride, di(coconut alkyl~ dime~hyl ammonium chloride and dilcoconut alkyl) dimethyl ammonium methosulfate are preferred.
Another class of preferred water-insoluble cationic matexial~ are the alkylimidazolinium salts believed to have the formula:
5~
- 5 - C.1362 CH Ch2 N / N - C2H~ T - c_~7 f ~9 ~8 wherein R6 is an alkyl or hydroxyal~yl group containing from 1 to I, preferably 1 or 2 carbon atoms, R7 i5 an alkyl or alkenyl group containing from 8 to 25 carbon atoms, R8 is an alkyl or alkenyl group contairling from &
to 25 carbon atoms, and Rg is hydrogen or an alkyl group containing from 1 to 4 carbon atoms and A is an anior"
preferably a halide, methosulfate or ethosulfate.
Preferreu imidazolinium salts include 1-methyl-1-(tallow~lamido-) ethyl -2-tallowyl-4,5-dihydro-imidazolinium methosulfate and l-methyl-l-(palmitoylamido) ethyl -2-octadecyl-4,5- dihydro-imidazolinium chloriùe.
Other useful imidazolinium materials are 2-heptadecyl-1-meth~l-l- [2-stearylamido)-ethyl-imidazolinium chloride and 2-lauryl-1-hydroxyethyl-1-oleyl-imidazolinium chioride. Also suitable herein are the imidazolir.ium fabric softening components of US Patent No 4 127 489.
In the present invention, the water-insoluble cationic softener is present at a total level ol at least 8%. The maximum level of cationic softener is determined by practical considerations; even with the nonionic materials to control viscosity it is not generally possible to prepare stable, pourable emulsions containing more than 26~ of cationic softener. When particularly hiqh concentrations are desired, it is preferred to use an if
- 5 - C.1362 CH Ch2 N / N - C2H~ T - c_~7 f ~9 ~8 wherein R6 is an alkyl or hydroxyal~yl group containing from 1 to I, preferably 1 or 2 carbon atoms, R7 i5 an alkyl or alkenyl group containing from 8 to 25 carbon atoms, R8 is an alkyl or alkenyl group contairling from &
to 25 carbon atoms, and Rg is hydrogen or an alkyl group containing from 1 to 4 carbon atoms and A is an anior"
preferably a halide, methosulfate or ethosulfate.
Preferreu imidazolinium salts include 1-methyl-1-(tallow~lamido-) ethyl -2-tallowyl-4,5-dihydro-imidazolinium methosulfate and l-methyl-l-(palmitoylamido) ethyl -2-octadecyl-4,5- dihydro-imidazolinium chloriùe.
Other useful imidazolinium materials are 2-heptadecyl-1-meth~l-l- [2-stearylamido)-ethyl-imidazolinium chloride and 2-lauryl-1-hydroxyethyl-1-oleyl-imidazolinium chioride. Also suitable herein are the imidazolir.ium fabric softening components of US Patent No 4 127 489.
In the present invention, the water-insoluble cationic softener is present at a total level ol at least 8%. The maximum level of cationic softener is determined by practical considerations; even with the nonionic materials to control viscosity it is not generally possible to prepare stable, pourable emulsions containing more than 26~ of cationic softener. When particularly hiqh concentrations are desired, it is preferred to use an if
- 6 - C.1362 imidazolinium softener and preferred compositions contain from 12% to 26~ of imidazolinium softener. When a di-long chain non-cyclic mono-quaternary softener is employed, it is preferred not to exceed a level of 22~, and a preferred range is 10% to 18%.
The compositions further contain nonionic materials having an ~LB of not more than 10, preferably not more than 8. The HLB scale is a known measure of the hydrophilic-lipophilic balance in any compound and can be determined from trade literature Nonionic materials having lower HLB values are less hydrophilic than those having higher HLB values.
Preferred nonionic materials are selected from:
( i) C8-C24 fatty acids;
( ;i) esters of C8-C24 fatty acidc with monohydric alcohols containing from 1-3 carbon atoms;
(iii) C10-C g fatty alcohols;
( iv) lanolin and derivatives thereof; and v) fat y acid esters of C2-C8 polyhydric alcohols.
Particularly prelerred examples of such nonionic materials include lauric acid, myristic acid, palmitic acid, iso-stearic acid, stearic acid, oleic acid, linoleic acid, undecanoic acid, methyl laurate, ethyl myrista~e, ethyl stearate, methyl palmitate, dodecanol, tetradecanol, hexadecanol, octadecanol, lanolin, lanolin alcohols, hydrogenated lanolin, ethylene glycol monostearate, glycerol monostearate and mono-iso~ stearate, sorbitan monostearate and mono-iso-stearate.
The compositions further contain nonionic materials having an ~LB of not more than 10, preferably not more than 8. The HLB scale is a known measure of the hydrophilic-lipophilic balance in any compound and can be determined from trade literature Nonionic materials having lower HLB values are less hydrophilic than those having higher HLB values.
Preferred nonionic materials are selected from:
( i) C8-C24 fatty acids;
( ;i) esters of C8-C24 fatty acidc with monohydric alcohols containing from 1-3 carbon atoms;
(iii) C10-C g fatty alcohols;
( iv) lanolin and derivatives thereof; and v) fat y acid esters of C2-C8 polyhydric alcohols.
Particularly prelerred examples of such nonionic materials include lauric acid, myristic acid, palmitic acid, iso-stearic acid, stearic acid, oleic acid, linoleic acid, undecanoic acid, methyl laurate, ethyl myrista~e, ethyl stearate, methyl palmitate, dodecanol, tetradecanol, hexadecanol, octadecanol, lanolin, lanolin alcohols, hydrogenated lanolin, ethylene glycol monostearate, glycerol monostearate and mono-iso~ stearate, sorbitan monostearate and mono-iso-stearate.
- 7 - C.1362 The nonionic material may be present at a level ox about 1~0% to about 6.0%, preferably between about 1.6 and about 4.0~.
The electrolyte is selected from the salts of lithium, sodium, potassium, calcium, magnesium, aluminium and mixtures thereof. Aluminium salts are most preferred. Sodium and potassium salts are least preferred. Preferably the salts contain monovalent anions. Pxeferred examples include aluminium chloride, aluminium chlorhydrate, calcium chloride, calcium bromide, calcium nitrate and magnesium chloride. The preferred level of highly ionic electrolyte in the inal product is at least 10 ppm and less than 3,00~ ppm, most preferably 50 ppm to 2,OGO ppm. In the case of elcctrolytes with a more covalent character such as aluminium chlorhydrate, the preferred level is at least 50 ppm and less than 12,000 ppm, most preferably from 120 to 6,0~0 ppm.
The first step in the process of toe invention i5 the formation of a molten mixture oE cationio and nonionic romponents. The temperature of this mixture is suitably less than lOO~C. When this molten mixture is added to water at an elevated temperature, such as above 40~C, preferably above 60C, and thorollghly mixed, a dispersion of the active materials in droplet form is created. The water preferably contains substantially no electrolyte at this stageO Some electrolyte may be tolerated however provided that the weight ratio of electrolyte in the final product to thaw initially present is a least 3:1 and provided that the water initially contains no more than 300 ppm electrolyte. It is preferred thaw the level of cationic material in this dispexsion is from 8% to 40~ by weight and the level of the nonionic material is pxeferably l Jo 9~ by weight. While this dispersion may be cooled to ambient temperature at this stage, it is so .1362 preferred not to cool the dispersion until after the addition of the electrolyte. The electrolyte must be added after the dispersion of the active material in droplet form has been created. it this stage, provided that at least 8% cationic fabric softener has been addeu, further amounts of the molten mixture may be added. The electrolyte is preferably added in the form of a concentrated solution, such as about 1-10% by weight.
Thus in a preferred embodiment of the invention the electrolyte is added in the form of a concentrated solution, after the formation of the dispersion but before the dispersion is cooled below 40C. This is of particular benefit if the cationic softener contains hardened (ie mainly saturated) alkyl groups.
Where the cationic raw material used for making the product already contains electrolyte, we have found it to be of advantage ii at least a portion of the added electrolyte contains the tame cation. Thus, where for example the cationic raw material contains sodium ions, the added electrolyte preferably also contains some sodium ions, advantageously together with an electrolyte containing more highly charged ions, such as calcium ions.
The compositions may also contain one or more optional ingredients selected from non-aqueous solvents such as Cl-C4 alkanols and polyhydric alcohols, pi buffering agents such as weak acids eg phosphoric, benzoic or citric acids (the pH of the compositions are preferably less than 6.0), antigelling agents, perfumes, perfume carriers, fluorescers, colourants, hydrotropes, antifoaming agents, antiredeposition agents, enzymes, optical brightening agents, opacifiers, stabilisers such as guar gum and polyethylene glycol, anti-shrinkillg agents, anti-wrinkle agents, fabric crisping agents, 5~
- 9 - C.1362 spotting agents, soil-release agents, germicides, fungicides, ~nti-oxidants, anti-corrosion agents, preservatives, dyes, bleaches and bleach precursors, drape imparting agents and antistatic agents.
These optional ingredients may be added to the active melt, to the water before forming the dispersion or after adding the electrolyte as appropriate.
It is particularly advantageous if the water to which the molten cationic/nonionic mixture is added already contains a dispersing aid. This dispersing aid should be a water-soluble non-anionic surfactant having an HLB of greater than 10, ideally greater than 12. In this context, the term ~Iwater-soluble~ means having a solubility of more than l.Og/l in water at pH 205 and at , 20C. Preferred examples include ~-ater-soluble quaternary ammonium salts (such as Arquad ~6, Arquad~2C), ethoxylated quaternary ammonium salts (such as Ethoquad 2~ 0/12), quaternary diamine and ethoxylated diamine salts (such as Duoquad T3, ethoxylated amines and diamines (such as Ethoduomee ~'r~25, Ethomeen T/lS) and their acid salts, ethoxylated fatty esters of polyhydric alcohols such as sorbitan monolaurate 20 EO), ethoxylated fatty alcohols such as Brij~58 - cetyl alcohol 20 EO) and ethoxylated fatty acids (such as Myra 49 stearic acid 20 EO).
A useful test for whether a particular material will be a suitable dispersing aid is one which xesults in a lower product viscosity after the addition of the electrolyte.
The dispersing aid may be present at a level of at least 0.1%, prefexably at least 0.2~ by weight based on the final product. Usually, it will not be necessary to ~e~o~leS no my - 10 - C.136 use more than 2.5%, preferably not more than 1.0%
dispersing aid.
It is preferred that the weight ratio of the catior.ic fabric softener material to the low HLB nonionic material is in excess of about 2.0:1, such as in excecs ox about 3O0:1, most preferably within the range of 5:1 to 20:1. A preferred composition contains about 8~ to about 22% of the cationic material, about 1.0% to about 6% of the nonionic material and from about 0.01~ to about 0.2%
of the electrolyte.
The invention will now be illustrated by the following non-limiting examples, in which parts and percentages are by weight, based on the weight of the end product. Where materials are referred to by their commercial names, the percentages quoted are percentages of the active materials.
A homogenous molten premix was prepared containing 10.~ dl~soft tallow dimethyl ammonium chloride (Arquad d~'~ 2T) and 2.6% hardened tallow fatty Acid (Prist~rene 916).
This premix was added at a temperature of 60C to demineralised water at the same temperature. After thorough mixing with a high speed constant torque stirrer the dispersion formed was allowed to cool to 25C and thereafter 0.1% calcium chloride (in the form vf a 10%
solution) and l perfume were added.
The viscosity oi the product measured llO sec 1 was 30cP.
~e,70~5 Z/~Q~e, ~?~
is C.1362 The experiment was repeated with the only difference that the calcium chloride was pre-dissolved in the water.
In this case the product viscosity was 438 cP.
This example demonstrates the benefit of post-addition of the electrolyte.
Example 1 was repeated using a molten pre-mix of 17%
dilsoft tallow imidazolinium metllosulphate ~Varisoft 475) and 3% Pristerene 4916. In this example, various levels of various electrolytes were added. The viscosity of the product was measured immediately after preparatior. and then again after lZ weeks storage at room temperature.
The results are set out in the followins Table.
Electrolyte Level Viscosity Initial After storaqe _ . _ ., NaCl 0.2% 72 400 CaCl~ 0.2% 62 12C
MgCl2 0.17% 48 91 ~lCl3 ~15~ ~0 67 This example illustrates the benefit of using calcium, magnesium or aluminium salt as the electrolyte, rather than sodium salts EXAMPLE _ Similarly beneficial results can be obtained by processing in the same manner compositions with the following formulations:
56~
- 12 - C.13~2 A. Arquad 2HT 12.0%
Pxisterene 4916 1.5~
CaC12 (added at 60C) 0.03%
Water balance Similar results are obtained when the calcium chloride is replaced by the same level of aluminium chloride or sodium chloride, added at 60C and/or when the level of Arquad 2HT and Prist~rene 4916 are changed to 10~9% and 2.6% respectively. A lower initial viscosity is achieved with these products than if identical formulations are prepared by adding the electrolyte after cooling.
. .
B. Varis~ft~475 14.5 Hardened xape seed fatty acid 3.5 CaC12 or ~gC12 0.~
water balance 20 C. Arquad 2T 17.0%
Pristerene 4916 1.0%
Aluminium chlorhydrate 1.0%
Water balance 25 D. Arquad 2T 10.9~
Pristerene 4916 2.6%
Perfume 1.0%
CaC12 tadded at 60C) 0.0~5%
Water balance E. Di(hardened tallow) imidazolinium methosulphate IVariso~t 445) 11. 0 Commercial iso-~tearic acid lex Emery) 2.5 NaCl 0.15~
water ba:Lance c~/eno fez z,~
5~
- 13 - C.1362 This composition is particularly beneficial if the sodium chloride is added at 60C, and still more beneficial if the sodium chloride is replaced by calcium chloride, magnesium chloride or aluminium chlor.ide.
F Varisoft 445 12.2%
. 1 Prifac~796~ (unhardened soyabean fatty acid containing 54~ linoleic acid and 30% oleic acid ~8~
Calcium chloride 0~%
Water balance 15 Similarly beneficial results can be obtained by processing in the same manner compositions with the following formulations:
XAMPLE NO 4~, 4B 4C 4D 4E 4F 4G
20 Ingredients Arquad ZHT 22 12 12 8 18 12 8 Lanolin 4 2 6 4 - - -Lanolin alcohol (Hartolan) - - 6 Z5 Calcium chloride* 0.1 O.D7 0.05 0.03 0.1 0.1 0.1 Perfume Water --balance------------*Added to the dispersion aftex cooling. The calcium chlorite may be replaced by a similar level of aluminium chlorideO Beneficial results may be obtained by adding the calcium chloride or other electrolyte before cooling the dispersion.
In this Example the Arquad 2~T may be replaced by Varisoft 445.
'I-~e~o fes f k-- l - C.13~2 Similarly beneficial results can be obtained by processing in the same manner compositions with the following formulations:
In~redient~
Arquad 2HT 12 8 9 15 12 Octadecanol 1 l 3 5 6 Calcium chloride 0.1 0.1 0.06 0.1 0.05 Perfume 0.6 - - l.0 0.6 Water balance In this Example the calcium chloride may be added after or (more preferably) before cooling the dispersion.
Calcium chloride may be replaced by magnesium or aluminium chloride. Arquad 2HT may be replaced by Varisoft 445.
The octadecanol may be replaced by glycerol monostearate, glycerol mono-iso-stearate, sorbitan monost~arate or ~orbitan mono-iso-stearate. Any two or more of these modifications may be combined.
~5 EXAMPLE 6 The following formulation was prepared by the method set out below.
30 Arquad 2HT 12.0%
Lanolin 4.0~
Phosphoric acid 0~03%
Perfume 0.
Calcium chloride Q.05%
Dye 0.0075%
Water balance so - 15 - C.1362 The molten mix the Arquad 2HT and the lanolin was formed at 60C. This molten mix was added to demineralised water at 60C, which already contained the phosphoric acid (added as a pH buffer). After thorough mixing to form a dispersion of the active materials in droplet form, the calcium chloride was added in the form of a 10~ solution. ThPreafter the mixture was cooled to ambient temperature and the perfume and dye added.
EXA~iPLE 7 The following formulations demonstrate the range OL
active levels that are possible within the scope of this invention. In each case the active materials were premixed at 60C, added to ~-ater at the same temperature and shear mixed to form a dispersion in droplet form.
Then the calcium chloride was added in the form of a 10~
solution. After further mixing the perfume and dye were added and thereafter the mixture was cooled to ambient temperature.
EXAMPLE NO 7~ 7B 7C 7D
Ingredients %
Arquad 2HT (hard) 12.5 14.7 17.6 14O5 Pristerene 4916 1.7 2.0 2.4 3.5 CaC12 0.05 0.06 0.07 0.05 Perfume 0.55 0.75 0O75 1.0 Dye 0.0075 0.0075 0.0075 Water balance Total active level 14O2 16O7 ~0.0 18.G
- l C.1362 _ In redients t%) _ _ _ _ Axquad 2T (soft) 12.0 14~0 16.53 11.5 11.5 Pristerene 4916 1.5 2.0 2.07 2.0 2.3 CaC12 0.04 0.06 0~07 0.03 0.03 ~erf~e 0.55 0.75 0.75 0.55 0.55 Dye 0.0075 0.0075 0.0075 0.0075 0.0075 ~JatPr balance----------------the benefit of including a dispersi~.s aid in the water to which the active premix is added is illustrated as follows. An active premix was prepared by mixing 10. 5 parts of Arquad 2HT with 2.5 parts Pristerene 4961 arld heating to 70C. This premix was then added to distilled water at 70C containing the dispersing aid. After stirring to form a dispersion in droplet form calcium chloride was added to the hot mixture using a 10%
solution. The end product composition was:
Arquad 2HT 10.5%
Pristerene 4916 2.5%
CaC12 0.03%
Dispersing aid 0.5%
fter cooling to room temperature the viscosity Gf each product was measured at 110 sec at 25C. Various materials were used as dispersing aidsO The results were as follows:
56~
- 17 C.1362 EXAMPLE NO DISPERSING I (HLB) VISCOSITY (cP) PA Ethoduomeen T/25 (18.5) 40 8B ~yrj 4g (15.0) 30 8C Brij 76 (12.4) 24 8D None (Control) 204-~40 8E Span ~0 ( 8.6) 351 In a further set of experiments using an appar~tu~
lC of slightly different dimensions but otherwise using a similar technique, the results were:
EXAMPLE NO DISP_ SIN RID (HLB) VISCOCITY (cP) l 8F Arquad 16 (15. 8) 3 8G Ethoqua~d 0/12(about 15) 27 8H Duo~,~c~T (10.7) 219 8I None (controi) 300 These results demonstrate that the product YiSCosity is lowered when the dispersing aid has an HL~ of more than lG (Example 8H for instance) but not when the dispersing aid is less than 10 (Example 8E). Alto it it apparent that the benefit is most noticeable where the dispersing aid has an HLB above 12.0 (Examples 8A to 8C~ 8F and 8G~.
The dispersing aids used in this Example are commercial ~laterials which are approximately as follows.
Ethoduomeen T/25: Ethoxylated ~-tallowyl 1,3 propane diamine with 15 ethoxylene oxlde groups pex molecule Myr] 49: Ethoxylated stearic acid with 20 ethylene oxide groups per molecule.
O/e~s a ks - 18 - C.1362 ~rij 76: Ethoxylated stearyl alcohol with ~0 ethylene oxide groups per molecule.
Span 20: Sorbitan monolaurate.
Arquad 16: Cetyl trimethyl ammonium chloride.
~thoquad 0/12: Oleyl, methyl bis (2 hydroxyethyi) ammonium chloride. 0 Duomac T: N-tallowyl 1,3 propane diamine diacetate.
Using the procecs described in Example 1, a product was formed contair.ing 10.9% Arquad 2T, 2.6% Pristerene 4916, 0.05% calcium chloride and 0.75% post-dosed perfume.
The calcium chloride was added either before addition of the molten active to the water (pre-dosed), after formation of the dispersion lpost-dosed) or part pre~dcsed and part post-dosed. In each case the viscosity of the product was measuredO The results were:
Pre-dosed CaCl~%) Post-dosed Ca 17 to) Viscosity (cP) 2~
0 ~.05 38 0.02 0.03 322 0~05 0 948 These results demonstrate the particular benefit of adding all the electxolyte after the formation of the dispersion.
5~i~
- 19 - C.1362 In all the above Examples, the initial level of electrolyte in the process water was less than 10 ppm.
EXAMPLE lO
82.5 parts of water containing 50 ppm Ca/~.gCO3 water hardness and small amounts of dye were heated to 66C in a vessel containing 3 inclined paddles of 0.88 x vessel dia~.eter. 17.5 parts of a premix of Arquad 2H5~ (75%
active) and Pris~erene 4916 at 65C was added to the stirred hot water over a period of lO minutes via a jet manifold between the top two agitators. This mixture was stirred for 20 minutes at which point 0.25 parts of a 10%
CaCl2 solution was added. After stirring for a further 10 minutes the mixture was cooled to 35C. 0.72 parts of perfume were added and stirring continued for a further 5 minutes. The product was finally cooled to 30C and stored.
The final product had the following composition Arquad 2HT 12O0 Pristerene 4916 1.5 Perfume 0.72 Added CaCl2 0.025 Water and minor ingredientsto 100
The electrolyte is selected from the salts of lithium, sodium, potassium, calcium, magnesium, aluminium and mixtures thereof. Aluminium salts are most preferred. Sodium and potassium salts are least preferred. Preferably the salts contain monovalent anions. Pxeferred examples include aluminium chloride, aluminium chlorhydrate, calcium chloride, calcium bromide, calcium nitrate and magnesium chloride. The preferred level of highly ionic electrolyte in the inal product is at least 10 ppm and less than 3,00~ ppm, most preferably 50 ppm to 2,OGO ppm. In the case of elcctrolytes with a more covalent character such as aluminium chlorhydrate, the preferred level is at least 50 ppm and less than 12,000 ppm, most preferably from 120 to 6,0~0 ppm.
The first step in the process of toe invention i5 the formation of a molten mixture oE cationio and nonionic romponents. The temperature of this mixture is suitably less than lOO~C. When this molten mixture is added to water at an elevated temperature, such as above 40~C, preferably above 60C, and thorollghly mixed, a dispersion of the active materials in droplet form is created. The water preferably contains substantially no electrolyte at this stageO Some electrolyte may be tolerated however provided that the weight ratio of electrolyte in the final product to thaw initially present is a least 3:1 and provided that the water initially contains no more than 300 ppm electrolyte. It is preferred thaw the level of cationic material in this dispexsion is from 8% to 40~ by weight and the level of the nonionic material is pxeferably l Jo 9~ by weight. While this dispersion may be cooled to ambient temperature at this stage, it is so .1362 preferred not to cool the dispersion until after the addition of the electrolyte. The electrolyte must be added after the dispersion of the active material in droplet form has been created. it this stage, provided that at least 8% cationic fabric softener has been addeu, further amounts of the molten mixture may be added. The electrolyte is preferably added in the form of a concentrated solution, such as about 1-10% by weight.
Thus in a preferred embodiment of the invention the electrolyte is added in the form of a concentrated solution, after the formation of the dispersion but before the dispersion is cooled below 40C. This is of particular benefit if the cationic softener contains hardened (ie mainly saturated) alkyl groups.
Where the cationic raw material used for making the product already contains electrolyte, we have found it to be of advantage ii at least a portion of the added electrolyte contains the tame cation. Thus, where for example the cationic raw material contains sodium ions, the added electrolyte preferably also contains some sodium ions, advantageously together with an electrolyte containing more highly charged ions, such as calcium ions.
The compositions may also contain one or more optional ingredients selected from non-aqueous solvents such as Cl-C4 alkanols and polyhydric alcohols, pi buffering agents such as weak acids eg phosphoric, benzoic or citric acids (the pH of the compositions are preferably less than 6.0), antigelling agents, perfumes, perfume carriers, fluorescers, colourants, hydrotropes, antifoaming agents, antiredeposition agents, enzymes, optical brightening agents, opacifiers, stabilisers such as guar gum and polyethylene glycol, anti-shrinkillg agents, anti-wrinkle agents, fabric crisping agents, 5~
- 9 - C.1362 spotting agents, soil-release agents, germicides, fungicides, ~nti-oxidants, anti-corrosion agents, preservatives, dyes, bleaches and bleach precursors, drape imparting agents and antistatic agents.
These optional ingredients may be added to the active melt, to the water before forming the dispersion or after adding the electrolyte as appropriate.
It is particularly advantageous if the water to which the molten cationic/nonionic mixture is added already contains a dispersing aid. This dispersing aid should be a water-soluble non-anionic surfactant having an HLB of greater than 10, ideally greater than 12. In this context, the term ~Iwater-soluble~ means having a solubility of more than l.Og/l in water at pH 205 and at , 20C. Preferred examples include ~-ater-soluble quaternary ammonium salts (such as Arquad ~6, Arquad~2C), ethoxylated quaternary ammonium salts (such as Ethoquad 2~ 0/12), quaternary diamine and ethoxylated diamine salts (such as Duoquad T3, ethoxylated amines and diamines (such as Ethoduomee ~'r~25, Ethomeen T/lS) and their acid salts, ethoxylated fatty esters of polyhydric alcohols such as sorbitan monolaurate 20 EO), ethoxylated fatty alcohols such as Brij~58 - cetyl alcohol 20 EO) and ethoxylated fatty acids (such as Myra 49 stearic acid 20 EO).
A useful test for whether a particular material will be a suitable dispersing aid is one which xesults in a lower product viscosity after the addition of the electrolyte.
The dispersing aid may be present at a level of at least 0.1%, prefexably at least 0.2~ by weight based on the final product. Usually, it will not be necessary to ~e~o~leS no my - 10 - C.136 use more than 2.5%, preferably not more than 1.0%
dispersing aid.
It is preferred that the weight ratio of the catior.ic fabric softener material to the low HLB nonionic material is in excess of about 2.0:1, such as in excecs ox about 3O0:1, most preferably within the range of 5:1 to 20:1. A preferred composition contains about 8~ to about 22% of the cationic material, about 1.0% to about 6% of the nonionic material and from about 0.01~ to about 0.2%
of the electrolyte.
The invention will now be illustrated by the following non-limiting examples, in which parts and percentages are by weight, based on the weight of the end product. Where materials are referred to by their commercial names, the percentages quoted are percentages of the active materials.
A homogenous molten premix was prepared containing 10.~ dl~soft tallow dimethyl ammonium chloride (Arquad d~'~ 2T) and 2.6% hardened tallow fatty Acid (Prist~rene 916).
This premix was added at a temperature of 60C to demineralised water at the same temperature. After thorough mixing with a high speed constant torque stirrer the dispersion formed was allowed to cool to 25C and thereafter 0.1% calcium chloride (in the form vf a 10%
solution) and l perfume were added.
The viscosity oi the product measured llO sec 1 was 30cP.
~e,70~5 Z/~Q~e, ~?~
is C.1362 The experiment was repeated with the only difference that the calcium chloride was pre-dissolved in the water.
In this case the product viscosity was 438 cP.
This example demonstrates the benefit of post-addition of the electrolyte.
Example 1 was repeated using a molten pre-mix of 17%
dilsoft tallow imidazolinium metllosulphate ~Varisoft 475) and 3% Pristerene 4916. In this example, various levels of various electrolytes were added. The viscosity of the product was measured immediately after preparatior. and then again after lZ weeks storage at room temperature.
The results are set out in the followins Table.
Electrolyte Level Viscosity Initial After storaqe _ . _ ., NaCl 0.2% 72 400 CaCl~ 0.2% 62 12C
MgCl2 0.17% 48 91 ~lCl3 ~15~ ~0 67 This example illustrates the benefit of using calcium, magnesium or aluminium salt as the electrolyte, rather than sodium salts EXAMPLE _ Similarly beneficial results can be obtained by processing in the same manner compositions with the following formulations:
56~
- 12 - C.13~2 A. Arquad 2HT 12.0%
Pxisterene 4916 1.5~
CaC12 (added at 60C) 0.03%
Water balance Similar results are obtained when the calcium chloride is replaced by the same level of aluminium chloride or sodium chloride, added at 60C and/or when the level of Arquad 2HT and Prist~rene 4916 are changed to 10~9% and 2.6% respectively. A lower initial viscosity is achieved with these products than if identical formulations are prepared by adding the electrolyte after cooling.
. .
B. Varis~ft~475 14.5 Hardened xape seed fatty acid 3.5 CaC12 or ~gC12 0.~
water balance 20 C. Arquad 2T 17.0%
Pristerene 4916 1.0%
Aluminium chlorhydrate 1.0%
Water balance 25 D. Arquad 2T 10.9~
Pristerene 4916 2.6%
Perfume 1.0%
CaC12 tadded at 60C) 0.0~5%
Water balance E. Di(hardened tallow) imidazolinium methosulphate IVariso~t 445) 11. 0 Commercial iso-~tearic acid lex Emery) 2.5 NaCl 0.15~
water ba:Lance c~/eno fez z,~
5~
- 13 - C.1362 This composition is particularly beneficial if the sodium chloride is added at 60C, and still more beneficial if the sodium chloride is replaced by calcium chloride, magnesium chloride or aluminium chlor.ide.
F Varisoft 445 12.2%
. 1 Prifac~796~ (unhardened soyabean fatty acid containing 54~ linoleic acid and 30% oleic acid ~8~
Calcium chloride 0~%
Water balance 15 Similarly beneficial results can be obtained by processing in the same manner compositions with the following formulations:
XAMPLE NO 4~, 4B 4C 4D 4E 4F 4G
20 Ingredients Arquad ZHT 22 12 12 8 18 12 8 Lanolin 4 2 6 4 - - -Lanolin alcohol (Hartolan) - - 6 Z5 Calcium chloride* 0.1 O.D7 0.05 0.03 0.1 0.1 0.1 Perfume Water --balance------------*Added to the dispersion aftex cooling. The calcium chlorite may be replaced by a similar level of aluminium chlorideO Beneficial results may be obtained by adding the calcium chloride or other electrolyte before cooling the dispersion.
In this Example the Arquad 2~T may be replaced by Varisoft 445.
'I-~e~o fes f k-- l - C.13~2 Similarly beneficial results can be obtained by processing in the same manner compositions with the following formulations:
In~redient~
Arquad 2HT 12 8 9 15 12 Octadecanol 1 l 3 5 6 Calcium chloride 0.1 0.1 0.06 0.1 0.05 Perfume 0.6 - - l.0 0.6 Water balance In this Example the calcium chloride may be added after or (more preferably) before cooling the dispersion.
Calcium chloride may be replaced by magnesium or aluminium chloride. Arquad 2HT may be replaced by Varisoft 445.
The octadecanol may be replaced by glycerol monostearate, glycerol mono-iso-stearate, sorbitan monost~arate or ~orbitan mono-iso-stearate. Any two or more of these modifications may be combined.
~5 EXAMPLE 6 The following formulation was prepared by the method set out below.
30 Arquad 2HT 12.0%
Lanolin 4.0~
Phosphoric acid 0~03%
Perfume 0.
Calcium chloride Q.05%
Dye 0.0075%
Water balance so - 15 - C.1362 The molten mix the Arquad 2HT and the lanolin was formed at 60C. This molten mix was added to demineralised water at 60C, which already contained the phosphoric acid (added as a pH buffer). After thorough mixing to form a dispersion of the active materials in droplet form, the calcium chloride was added in the form of a 10~ solution. ThPreafter the mixture was cooled to ambient temperature and the perfume and dye added.
EXA~iPLE 7 The following formulations demonstrate the range OL
active levels that are possible within the scope of this invention. In each case the active materials were premixed at 60C, added to ~-ater at the same temperature and shear mixed to form a dispersion in droplet form.
Then the calcium chloride was added in the form of a 10~
solution. After further mixing the perfume and dye were added and thereafter the mixture was cooled to ambient temperature.
EXAMPLE NO 7~ 7B 7C 7D
Ingredients %
Arquad 2HT (hard) 12.5 14.7 17.6 14O5 Pristerene 4916 1.7 2.0 2.4 3.5 CaC12 0.05 0.06 0.07 0.05 Perfume 0.55 0.75 0O75 1.0 Dye 0.0075 0.0075 0.0075 Water balance Total active level 14O2 16O7 ~0.0 18.G
- l C.1362 _ In redients t%) _ _ _ _ Axquad 2T (soft) 12.0 14~0 16.53 11.5 11.5 Pristerene 4916 1.5 2.0 2.07 2.0 2.3 CaC12 0.04 0.06 0~07 0.03 0.03 ~erf~e 0.55 0.75 0.75 0.55 0.55 Dye 0.0075 0.0075 0.0075 0.0075 0.0075 ~JatPr balance----------------the benefit of including a dispersi~.s aid in the water to which the active premix is added is illustrated as follows. An active premix was prepared by mixing 10. 5 parts of Arquad 2HT with 2.5 parts Pristerene 4961 arld heating to 70C. This premix was then added to distilled water at 70C containing the dispersing aid. After stirring to form a dispersion in droplet form calcium chloride was added to the hot mixture using a 10%
solution. The end product composition was:
Arquad 2HT 10.5%
Pristerene 4916 2.5%
CaC12 0.03%
Dispersing aid 0.5%
fter cooling to room temperature the viscosity Gf each product was measured at 110 sec at 25C. Various materials were used as dispersing aidsO The results were as follows:
56~
- 17 C.1362 EXAMPLE NO DISPERSING I (HLB) VISCOSITY (cP) PA Ethoduomeen T/25 (18.5) 40 8B ~yrj 4g (15.0) 30 8C Brij 76 (12.4) 24 8D None (Control) 204-~40 8E Span ~0 ( 8.6) 351 In a further set of experiments using an appar~tu~
lC of slightly different dimensions but otherwise using a similar technique, the results were:
EXAMPLE NO DISP_ SIN RID (HLB) VISCOCITY (cP) l 8F Arquad 16 (15. 8) 3 8G Ethoqua~d 0/12(about 15) 27 8H Duo~,~c~T (10.7) 219 8I None (controi) 300 These results demonstrate that the product YiSCosity is lowered when the dispersing aid has an HL~ of more than lG (Example 8H for instance) but not when the dispersing aid is less than 10 (Example 8E). Alto it it apparent that the benefit is most noticeable where the dispersing aid has an HLB above 12.0 (Examples 8A to 8C~ 8F and 8G~.
The dispersing aids used in this Example are commercial ~laterials which are approximately as follows.
Ethoduomeen T/25: Ethoxylated ~-tallowyl 1,3 propane diamine with 15 ethoxylene oxlde groups pex molecule Myr] 49: Ethoxylated stearic acid with 20 ethylene oxide groups per molecule.
O/e~s a ks - 18 - C.1362 ~rij 76: Ethoxylated stearyl alcohol with ~0 ethylene oxide groups per molecule.
Span 20: Sorbitan monolaurate.
Arquad 16: Cetyl trimethyl ammonium chloride.
~thoquad 0/12: Oleyl, methyl bis (2 hydroxyethyi) ammonium chloride. 0 Duomac T: N-tallowyl 1,3 propane diamine diacetate.
Using the procecs described in Example 1, a product was formed contair.ing 10.9% Arquad 2T, 2.6% Pristerene 4916, 0.05% calcium chloride and 0.75% post-dosed perfume.
The calcium chloride was added either before addition of the molten active to the water (pre-dosed), after formation of the dispersion lpost-dosed) or part pre~dcsed and part post-dosed. In each case the viscosity of the product was measuredO The results were:
Pre-dosed CaCl~%) Post-dosed Ca 17 to) Viscosity (cP) 2~
0 ~.05 38 0.02 0.03 322 0~05 0 948 These results demonstrate the particular benefit of adding all the electxolyte after the formation of the dispersion.
5~i~
- 19 - C.1362 In all the above Examples, the initial level of electrolyte in the process water was less than 10 ppm.
EXAMPLE lO
82.5 parts of water containing 50 ppm Ca/~.gCO3 water hardness and small amounts of dye were heated to 66C in a vessel containing 3 inclined paddles of 0.88 x vessel dia~.eter. 17.5 parts of a premix of Arquad 2H5~ (75%
active) and Pris~erene 4916 at 65C was added to the stirred hot water over a period of lO minutes via a jet manifold between the top two agitators. This mixture was stirred for 20 minutes at which point 0.25 parts of a 10%
CaCl2 solution was added. After stirring for a further 10 minutes the mixture was cooled to 35C. 0.72 parts of perfume were added and stirring continued for a further 5 minutes. The product was finally cooled to 30C and stored.
The final product had the following composition Arquad 2HT 12O0 Pristerene 4916 1.5 Perfume 0.72 Added CaCl2 0.025 Water and minor ingredientsto 100
Claims (9)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for preparing a concentrated aqueous liquid fabric softening composition containing at least 8%
by weight water-insoluble cationic fabric softener, said process comprising the steps of:
( i) forming a molten mixture containing the water-insoluble cationic fabric softener and a nonionic material having an HLB of not more than 10;
( ii) adding the molten mixture to water at an elevated temperature;
(iii) mixing the molten mixture and the water together to form a dispersion of the molten mixture in droplet form in the water; and ( iv) adding electrolyte in the form of a source of lithium, sodium, potassium, calcium, magnesium or aluminium ions thereto, characterised in that the electrolyte is added after, but not before, the formation of said dispersion.
by weight water-insoluble cationic fabric softener, said process comprising the steps of:
( i) forming a molten mixture containing the water-insoluble cationic fabric softener and a nonionic material having an HLB of not more than 10;
( ii) adding the molten mixture to water at an elevated temperature;
(iii) mixing the molten mixture and the water together to form a dispersion of the molten mixture in droplet form in the water; and ( iv) adding electrolyte in the form of a source of lithium, sodium, potassium, calcium, magnesium or aluminium ions thereto, characterised in that the electrolyte is added after, but not before, the formation of said dispersion.
2. A process according to Claim 1, characterised in that the composition is cooled to ambient temperature after the addition of the electrolyte.
3. A process according to Claim 1, characterised in that the electrolyte is selected from a source of calcium, magnesium or aluminium ions.
4. A process according to Claim 1, characterised in that the water-insoluble cationic fabric softener is selected from water-insoluble quaternary ammonium salts and imidazolinium salts.
5. A process according to Claim 1, characterised in that the nonionic material is selected from ( i) C8-C24 fatty acids;
( ii) esters of C8-C24 fatty acids with monohydric alcohols containing from 1-3 carbon atoms;
(iii) C10-C18 fatty alcohols;
( iv) lanolin and derivatives thereof; and ( v) fatty acid esters of C2-C8 polyhydric alcohols.
( ii) esters of C8-C24 fatty acids with monohydric alcohols containing from 1-3 carbon atoms;
(iii) C10-C18 fatty alcohols;
( iv) lanolin and derivatives thereof; and ( v) fatty acid esters of C2-C8 polyhydric alcohols.
6. A process according to Claim 1, characterised in that the weight ratio of the cationic fabric softening agent to the nonionic material in the composition is from 5:1 to 20:1.
7. A process according to Claim 1, characterised in that the water to which the molten mixture is added in step (ii), already contains a dispersing aid.
8. A process according to Claim 7, characterised in that the dispersing aid is selected from water-soluble cationic and water-soluble nonionic surfactants having an HLB of more than 10.
9. A process according to Claim 1, characterised in that after the addition of the electrolyte, the composition contains from 8% to 22% of the water-insoluble cationic fabric softening material, from 0.5% to 4% of the nonionic material, and from 0.01% to 0.2% of the electrolyte.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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GB8309663 | 1983-04-08 | ||
GB8309663 | 1983-04-08 |
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CA1204562A true CA1204562A (en) | 1986-05-20 |
Family
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CA000451506A Expired CA1204562A (en) | 1983-04-08 | 1984-04-06 | Method for preparing fabric softening compositions |
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EP (1) | EP0122140A3 (en) |
JP (1) | JPS59199865A (en) |
AU (1) | AU550895B2 (en) |
BR (1) | BR8401627A (en) |
CA (1) | CA1204562A (en) |
ES (1) | ES531386A0 (en) |
GB (1) | GB2139259B (en) |
GR (1) | GR81778B (en) |
IN (1) | IN159970B (en) |
MY (1) | MY8700539A (en) |
NO (1) | NO841373L (en) |
NZ (1) | NZ207721A (en) |
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Publication number | Priority date | Publication date | Assignee | Title |
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GB8410318D0 (en) * | 1984-04-19 | 1984-05-31 | Unilever Plc | Fabric softening composition |
DE3641314A1 (en) * | 1986-12-03 | 1988-06-09 | Henkel Kgaa | LAUNDRY TREATMENT AGENT BASED ON LAYERED SILICATE |
US5116520A (en) * | 1989-09-06 | 1992-05-26 | The Procter & Gamble Co. | Fabric softening and anti-static compositions containing a quaternized di-substituted imidazoline ester fabric softening compound with a nonionic fabric softening compound |
EP0687291B2 (en) * | 1993-03-01 | 2005-08-24 | The Procter & Gamble Company | Concentrated biodegradable quaternary ammonium fabric softener compositions and compounds containing intermediate iodine value unsaturated fatty acid chains |
WO1995031524A2 (en) * | 1994-05-18 | 1995-11-23 | The Procter & Gamble Company | Concentrated biodegradable fabric softener compositions |
US5474690A (en) * | 1994-11-14 | 1995-12-12 | The Procter & Gamble Company | Concentrated biodegradable quaternary ammonium fabric softener compositions containing intermediate iodine value fatty acid chains |
US5634969A (en) * | 1995-02-10 | 1997-06-03 | Rheox, Inc. | Organoclay compositions |
US5696292A (en) * | 1995-02-10 | 1997-12-09 | Witco Corporation | Process for producing quarternary ammonium compounds |
GB0121802D0 (en) * | 2001-09-10 | 2001-10-31 | Unilever Plc | Fabric conditioning compositions |
EP2069466A1 (en) | 2006-10-06 | 2009-06-17 | Dow Corning Corporation | Process for preparing fabric softener compositions |
BRPI0807730A2 (en) * | 2007-02-28 | 2014-12-30 | Unilever Nv | TISSUE CONDITIONING METHOD AND SOLID COMPOSITION FOR TISSUE TREATMENT |
GB201215753D0 (en) * | 2012-09-04 | 2012-10-17 | Reckitt Benckiser Nv | Composition |
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GB1104441A (en) * | 1964-07-08 | 1968-02-28 | Unilever Ltd | Fabric conditioner |
ATE20534T1 (en) * | 1981-03-07 | 1986-07-15 | Procter & Gamble | TEXTILE TREATMENT AGENTS AND THEIR PREPARATION. |
-
1984
- 1984-04-02 NZ NZ207721A patent/NZ207721A/en unknown
- 1984-04-03 GR GR74297A patent/GR81778B/el unknown
- 1984-04-04 IN IN92/BOM/84A patent/IN159970B/en unknown
- 1984-04-05 ZA ZA842586A patent/ZA842586B/en unknown
- 1984-04-06 EP EP84302401A patent/EP0122140A3/en not_active Ceased
- 1984-04-06 PT PT78379A patent/PT78379A/en unknown
- 1984-04-06 ES ES531386A patent/ES531386A0/en active Granted
- 1984-04-06 NO NO841373A patent/NO841373L/en unknown
- 1984-04-06 BR BR8401627A patent/BR8401627A/en not_active IP Right Cessation
- 1984-04-06 AU AU26485/84A patent/AU550895B2/en not_active Ceased
- 1984-04-06 CA CA000451506A patent/CA1204562A/en not_active Expired
- 1984-04-06 GB GB08409037A patent/GB2139259B/en not_active Expired
- 1984-04-09 JP JP59070742A patent/JPS59199865A/en active Pending
-
1987
- 1987-12-30 MY MY539/87A patent/MY8700539A/en unknown
Also Published As
Publication number | Publication date |
---|---|
MY8700539A (en) | 1987-12-31 |
AU2648584A (en) | 1984-10-11 |
EP0122140A2 (en) | 1984-10-17 |
AU550895B2 (en) | 1986-04-10 |
BR8401627A (en) | 1984-11-13 |
EP0122140A3 (en) | 1985-12-04 |
GB2139259A (en) | 1984-11-07 |
GB8409037D0 (en) | 1984-05-16 |
ZA842586B (en) | 1985-11-27 |
GB2139259B (en) | 1986-07-16 |
JPS59199865A (en) | 1984-11-13 |
PT78379A (en) | 1984-05-01 |
ES8602106A1 (en) | 1985-11-01 |
GR81778B (en) | 1984-12-12 |
IN159970B (en) | 1987-06-13 |
NO841373L (en) | 1984-10-09 |
NZ207721A (en) | 1986-10-08 |
ES531386A0 (en) | 1985-11-01 |
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