CA2139424C - Fabric conditioning compositions and process for making them - Google Patents
Fabric conditioning compositions and process for making them Download PDFInfo
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- CA2139424C CA2139424C CA002139424A CA2139424A CA2139424C CA 2139424 C CA2139424 C CA 2139424C CA 002139424 A CA002139424 A CA 002139424A CA 2139424 A CA2139424 A CA 2139424A CA 2139424 C CA2139424 C CA 2139424C
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- fabric conditioning
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Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
-
- 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
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
- C11D11/0094—Process for making liquid detergent compositions, e.g. slurries, pastes or gels
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/467—Compounds containing quaternary nitrogen atoms derived from polyamines
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
An aqueous fabric conditioning composition comprising a homogeneous dispersion of fabric conditioning active particles having a size distribution such that the particles have a mean size of about 0.7 to 10 microns as measured by Malvern Particle Size Analyzer and preferably have 10 % of the distribution with a particle size of at least 23 % of the mean particle size. A second aspect of the invention relates to a continuous process for making the aqueous fabric conditioning composition.
Description
WO 94/01523 . ~ ~ ~ ~ PCT/EP93/01703 FABRIC CONDITIONING COMPOSITIONS
AND PROCESS FOR MAKING THEM
FIELD OF THE INVENTION
In a first aspect the invention relates to fabric conditioning compositions and in particular to compositions in aqueous media which contain a high proportion of fabric conditioning ingredients.
In a second aspect the invention relates to a continuous process for making fabric conditioning compositions.
BACKGROUND OF THE INVENTION
Aqueous fabric conditioning compositions known in the art contain fabric conditioning agents which are substantially water-insoluble cationic materials having two long alkyl chains. The materials are usually in the form of an aqueous dispersion or emulsion and the addition of more than about 8g cationic material to the composition is not usually possible without incurring problems of physical instability.
There are many advantages to having more concentrated fabric conditioning compositions, for example there are shipping and packaging economies and the consumer can exercise choice'in the type of performance obtained in that the concentrated product can be used as is or can be diluted to a conventional concentration before use.
Due to the dispersibility of formulating concentrated fabric conditioning compositions the problem of physical instability has been addressed in the art.
U.S. Patent No. 3,954,634, (Rudy) utilizes a combination of quaternary ammonium softener, saturated imidazolinium softener, unsaturated imidazolinium softener and ionizable C6181 _ l~- z -salts to formulate concentrated softeners, but the maximum - concentration achieved is only 130.
U.S. Patent No. 3,954,634, (Monson) uses a special batch processing technique of homogenization at high pressure to manufacture compositions comprising up to 15g fabric conditioning active.
The various solutions proposed, however, are not entirely satisfactory in that they either require the use of substantial quantities of materials other than the fabric softener in order to reduce the viscosity or in that special processing techniques are necessary to cope with the high viscosities generated which are not practical on a commercial scale or at concentrations above about 15~ cationic conditioning agent.
The high viscosities generated during the manufacture of concentrated fabric conditioning compositions limit the quantity of composition that can be made using conventional batch processing equipment due to the large amounts of energy requirement for shearing the gel phases formed. This tends to mean that batch equipment is operated below capacity and with long cycle times. This leads to low throughputs which are not commercially attractive.
U.S. Patent No. 4,439,335, (Burns) describes such a process.
A mixture of cationic conditioning salts and an inorganic ionizable salt are used to make a concentrated aqueous composition. The composition is made in a batch process by adding a portion of ionizable salt to water concurrently with a molten mixture of the actives at a rate necessary to keep the aqueous mix fluid and stirrable. In one example, 90kg of product are made in a 226 litres capacity main mix tank over a period of about 25 minutes.
There thus exists a need for a process for making a concentrated aqueous liquid fabric conditioning composition AMENDED SHEET
C6181 _ ~I3942~
by a process which is practical on a commercial scale. There is also a need for a concentrated aqueous liquid fabric conditioning composition based on cationic conditioning agents which is physically stable and of acceptable viscosity.
Japanese Patent Application No. 63-77479 (Yamamura/Kao) relates to a method of manufacturing a conditioning finishing agent in a line mixer by mixing water into a supply of molten quaternary ammonium salt. The agent is made by a single addition of water and the rate of production of the softening, finishing agent is only about 11.3 to 15.1 litres per minute.
we have now found that it is possible to make an aqueous fabric conditioning composition of acceptable viscosity and stability by a continuous process that is practical on a commercial scale.
The invention relates to an aqueous fabric conditioning composition comprising a homogeneous dispersion of fabric conditioning active particles having a size distribution such that t?~:e particles have a mean size of about 0.7 to 10 microns as measured by Malvern Particle Size Analyzer and have 10% of the distribution with a particle size of at least 230 of the mean particle size, more preferably at least 290 of the mean particle size, most preferably between 30~ and 50~ of the mean particle size.
In a second aspect the invention relates to a continuous process for making an aqueous fabric conditioning composition comprising the steps of:
(i) selecting a fabric conditioning active, (ii) adding the active to a continuous mixer, AMENDED SHEET
~139~~
(iii)-dispersing the fabric conditioning active in water _ under controlled shear in the continuous mixer to form a homogeneous dispersion of the active, and (iv) mixing the dispersion with portions of electrolyte under controlled shear in the continuous mixer to maintain the homogeneous dispersion.
DE'T'~TL~'D DESCRIPTION OF THE PREFERRED EMBODTMENTS
In accordance with the present invention, it has been found that it is possible to make highly concentrated aqueous fabric conditioning compositions of acceptable viscosity and stability by a continuous process that is practical on a commercial scale. Specifically a preferred first aspect of the present invention is directed to a concentrated fabric conditioning composition comprising a homogeneous dispersion of from about 8o to about 80% of cationic conditioning active particles having a size distribution such that the mean particle size is from 0.7 to 10 microns preferably 0.7% to 5 microns and 10% of the distribution has a particle size of at least 290 of the mean particle size as measured by Malvern Particle Size Analyzer.
Specifically, a second aspect of the present invention is directed to a continuous process for making an aqueous fabric conditioning composition comprising from 8~ to 800 of a cationic fabric conditioning agent and from O.Olo to 0.50 of an ionizable salt said process comprising the steps of:
(i) selecting a cationic fabric conditioning active, (ii) adding the active to a continuous mixer, (iii) dispersing the active in water under controlled shear in the continuous mixer to form a homogenous dispersion of the active, (iv) mixing the dispersion with discrete portions of ionizable salt under controlled shear in the continuous mixer to maintain the homogeneous dispersion.
AMENDED SHEET
Co'1 81 -.~ 239424 - 4a -preferably the invention is directed to a continuous process for making an aqueous fabric conditioning composition in wh,~ch said composition comprises from 8% to 80o by weight of a cationic fabric conditioning agent and from O.Ola to 0.5%
of an ionizable salt said process comprising the steps of:
(i) selecting a cationic fabric conditioning active[,] of formula ~ R, -~ +
n R: N R, X I
--J n wherein R1 and R~ are each hydrocarbyl groups containing from about 1 to about 25 carbon atoms, R3 and RQ are each hydrocarbyl groups containing from 1 to about 6 carbon atoms, X is an anion and n is an integer from 1 to about 3, (ii) adding the active to a continuous mixer, (i,~i> dispersing the active in water under controlled shear in the continuous mixer to form a homogeneous dispersion of the active, (iv) mixing the dispersion with at least 3 discrete portions of the ionizable salt under controlled shear to maintain the homogeneous dispersion.
In the context of the present invention by "mean particle size" is meant the size of which 50% of the distribution is under or D(V,0.5) in Malvern terminology. By "particle size of l00 of the distribution" is meant the size which 10% of the distribution is under D(V,0.1) in Malvern terminology.
AMENDED SHEEN
C6181 _ __ 213944 _ 5 _ The compositions of the invention are stable and pourable at - normally encountered temperatures (22°C-58.5°C) and are easily dispersible in water. In the context of the present invention "stable and pourable" means having a viscosity below about 1000cP following 2 weeks storage at 14.7°C as measured by Brookfield Viscometer on Spindle No 1 or 3.
Preferably the compositions have a viscosity below about 800cP following two weeks storage at 40.6°C and more preferably below 800cP following four weeks storage at X0.6°C.
we have found that the composition of the invention have a homogeneous dispersion of conditioning active particles. In the context of the present invention, homogeneous dispersion means a dispersion that is uniform and without pockets of flocculated active material. Compositions with a homogeneous dispersion of particles having a size distribution with a mean size in the range according to the invention have been pound to be particularly stable.
Preferably, the composition comprises from 8% to 80o by weight of a cationic fabric conditioning material, more preferably 15% to 70o and even more preferably 20o to 50o by weight.
Cationic fabric conditioning materials suitable for use in the present invention are insoluble types of general formula:
R-n 0 ~ R= N R, , X I
R.
n AMENDED SHEET
WO 94/01523 _ ~ 1 ~ 9 ~ ~ ~ PCT/EP93/01703 wherein R1 and Rz are each hydrocarbyl groups containing from about 1 to about 25 carbon atoms, R3 and R4 are each hydrocarbyl groups containing from 1 to about 6 carbon atoms.
X is an anion and n is an integer from 1 to about 3. The term hydrocarbyl as used herein encompasses alkyl, alkenyl, aryl, alkaryl, substituted alkyl and alkenyl, ester linked alkyl and alkenyl, and substituted aryl and alkaryl groups.
Common substituents found on quaternary compounds include hydroxy and alkoxy groups.
Preferred cationic fabric conditioning agents are:
(i) difatty alkyl amidoammonium salts of formula:
o R6 o RS C NH CZH4-N'-CZH9-NH-C-R, X- II
wherein RS and R, are the same as each other or different and are selected from the group consisting of C19 to C22 alkyl or alkenyl groups, and R~ is selected from the groups consisting of methyl or (CnH,nO) .t H wherein n is 2 or 3 and X is from 1 to 5, and wherein X- is an anion, preferably selected from the group consisting of halides, sulphates, acetates or alkyl sulphates having from 1 to 3 carbon atoms in the alkyl chain.
It is particularly preferred that the difattyalkyl amidoammonium salt should have a particularly low level of residual ethoxylated amine, specifically less than about 120 of the difattyalkyl amidoammonium salt;
(ii) ester-linked trialkyl ammonium salts of formula:
AND PROCESS FOR MAKING THEM
FIELD OF THE INVENTION
In a first aspect the invention relates to fabric conditioning compositions and in particular to compositions in aqueous media which contain a high proportion of fabric conditioning ingredients.
In a second aspect the invention relates to a continuous process for making fabric conditioning compositions.
BACKGROUND OF THE INVENTION
Aqueous fabric conditioning compositions known in the art contain fabric conditioning agents which are substantially water-insoluble cationic materials having two long alkyl chains. The materials are usually in the form of an aqueous dispersion or emulsion and the addition of more than about 8g cationic material to the composition is not usually possible without incurring problems of physical instability.
There are many advantages to having more concentrated fabric conditioning compositions, for example there are shipping and packaging economies and the consumer can exercise choice'in the type of performance obtained in that the concentrated product can be used as is or can be diluted to a conventional concentration before use.
Due to the dispersibility of formulating concentrated fabric conditioning compositions the problem of physical instability has been addressed in the art.
U.S. Patent No. 3,954,634, (Rudy) utilizes a combination of quaternary ammonium softener, saturated imidazolinium softener, unsaturated imidazolinium softener and ionizable C6181 _ l~- z -salts to formulate concentrated softeners, but the maximum - concentration achieved is only 130.
U.S. Patent No. 3,954,634, (Monson) uses a special batch processing technique of homogenization at high pressure to manufacture compositions comprising up to 15g fabric conditioning active.
The various solutions proposed, however, are not entirely satisfactory in that they either require the use of substantial quantities of materials other than the fabric softener in order to reduce the viscosity or in that special processing techniques are necessary to cope with the high viscosities generated which are not practical on a commercial scale or at concentrations above about 15~ cationic conditioning agent.
The high viscosities generated during the manufacture of concentrated fabric conditioning compositions limit the quantity of composition that can be made using conventional batch processing equipment due to the large amounts of energy requirement for shearing the gel phases formed. This tends to mean that batch equipment is operated below capacity and with long cycle times. This leads to low throughputs which are not commercially attractive.
U.S. Patent No. 4,439,335, (Burns) describes such a process.
A mixture of cationic conditioning salts and an inorganic ionizable salt are used to make a concentrated aqueous composition. The composition is made in a batch process by adding a portion of ionizable salt to water concurrently with a molten mixture of the actives at a rate necessary to keep the aqueous mix fluid and stirrable. In one example, 90kg of product are made in a 226 litres capacity main mix tank over a period of about 25 minutes.
There thus exists a need for a process for making a concentrated aqueous liquid fabric conditioning composition AMENDED SHEET
C6181 _ ~I3942~
by a process which is practical on a commercial scale. There is also a need for a concentrated aqueous liquid fabric conditioning composition based on cationic conditioning agents which is physically stable and of acceptable viscosity.
Japanese Patent Application No. 63-77479 (Yamamura/Kao) relates to a method of manufacturing a conditioning finishing agent in a line mixer by mixing water into a supply of molten quaternary ammonium salt. The agent is made by a single addition of water and the rate of production of the softening, finishing agent is only about 11.3 to 15.1 litres per minute.
we have now found that it is possible to make an aqueous fabric conditioning composition of acceptable viscosity and stability by a continuous process that is practical on a commercial scale.
The invention relates to an aqueous fabric conditioning composition comprising a homogeneous dispersion of fabric conditioning active particles having a size distribution such that t?~:e particles have a mean size of about 0.7 to 10 microns as measured by Malvern Particle Size Analyzer and have 10% of the distribution with a particle size of at least 230 of the mean particle size, more preferably at least 290 of the mean particle size, most preferably between 30~ and 50~ of the mean particle size.
In a second aspect the invention relates to a continuous process for making an aqueous fabric conditioning composition comprising the steps of:
(i) selecting a fabric conditioning active, (ii) adding the active to a continuous mixer, AMENDED SHEET
~139~~
(iii)-dispersing the fabric conditioning active in water _ under controlled shear in the continuous mixer to form a homogeneous dispersion of the active, and (iv) mixing the dispersion with portions of electrolyte under controlled shear in the continuous mixer to maintain the homogeneous dispersion.
DE'T'~TL~'D DESCRIPTION OF THE PREFERRED EMBODTMENTS
In accordance with the present invention, it has been found that it is possible to make highly concentrated aqueous fabric conditioning compositions of acceptable viscosity and stability by a continuous process that is practical on a commercial scale. Specifically a preferred first aspect of the present invention is directed to a concentrated fabric conditioning composition comprising a homogeneous dispersion of from about 8o to about 80% of cationic conditioning active particles having a size distribution such that the mean particle size is from 0.7 to 10 microns preferably 0.7% to 5 microns and 10% of the distribution has a particle size of at least 290 of the mean particle size as measured by Malvern Particle Size Analyzer.
Specifically, a second aspect of the present invention is directed to a continuous process for making an aqueous fabric conditioning composition comprising from 8~ to 800 of a cationic fabric conditioning agent and from O.Olo to 0.50 of an ionizable salt said process comprising the steps of:
(i) selecting a cationic fabric conditioning active, (ii) adding the active to a continuous mixer, (iii) dispersing the active in water under controlled shear in the continuous mixer to form a homogenous dispersion of the active, (iv) mixing the dispersion with discrete portions of ionizable salt under controlled shear in the continuous mixer to maintain the homogeneous dispersion.
AMENDED SHEET
Co'1 81 -.~ 239424 - 4a -preferably the invention is directed to a continuous process for making an aqueous fabric conditioning composition in wh,~ch said composition comprises from 8% to 80o by weight of a cationic fabric conditioning agent and from O.Ola to 0.5%
of an ionizable salt said process comprising the steps of:
(i) selecting a cationic fabric conditioning active[,] of formula ~ R, -~ +
n R: N R, X I
--J n wherein R1 and R~ are each hydrocarbyl groups containing from about 1 to about 25 carbon atoms, R3 and RQ are each hydrocarbyl groups containing from 1 to about 6 carbon atoms, X is an anion and n is an integer from 1 to about 3, (ii) adding the active to a continuous mixer, (i,~i> dispersing the active in water under controlled shear in the continuous mixer to form a homogeneous dispersion of the active, (iv) mixing the dispersion with at least 3 discrete portions of the ionizable salt under controlled shear to maintain the homogeneous dispersion.
In the context of the present invention by "mean particle size" is meant the size of which 50% of the distribution is under or D(V,0.5) in Malvern terminology. By "particle size of l00 of the distribution" is meant the size which 10% of the distribution is under D(V,0.1) in Malvern terminology.
AMENDED SHEEN
C6181 _ __ 213944 _ 5 _ The compositions of the invention are stable and pourable at - normally encountered temperatures (22°C-58.5°C) and are easily dispersible in water. In the context of the present invention "stable and pourable" means having a viscosity below about 1000cP following 2 weeks storage at 14.7°C as measured by Brookfield Viscometer on Spindle No 1 or 3.
Preferably the compositions have a viscosity below about 800cP following two weeks storage at 40.6°C and more preferably below 800cP following four weeks storage at X0.6°C.
we have found that the composition of the invention have a homogeneous dispersion of conditioning active particles. In the context of the present invention, homogeneous dispersion means a dispersion that is uniform and without pockets of flocculated active material. Compositions with a homogeneous dispersion of particles having a size distribution with a mean size in the range according to the invention have been pound to be particularly stable.
Preferably, the composition comprises from 8% to 80o by weight of a cationic fabric conditioning material, more preferably 15% to 70o and even more preferably 20o to 50o by weight.
Cationic fabric conditioning materials suitable for use in the present invention are insoluble types of general formula:
R-n 0 ~ R= N R, , X I
R.
n AMENDED SHEET
WO 94/01523 _ ~ 1 ~ 9 ~ ~ ~ PCT/EP93/01703 wherein R1 and Rz are each hydrocarbyl groups containing from about 1 to about 25 carbon atoms, R3 and R4 are each hydrocarbyl groups containing from 1 to about 6 carbon atoms.
X is an anion and n is an integer from 1 to about 3. The term hydrocarbyl as used herein encompasses alkyl, alkenyl, aryl, alkaryl, substituted alkyl and alkenyl, ester linked alkyl and alkenyl, and substituted aryl and alkaryl groups.
Common substituents found on quaternary compounds include hydroxy and alkoxy groups.
Preferred cationic fabric conditioning agents are:
(i) difatty alkyl amidoammonium salts of formula:
o R6 o RS C NH CZH4-N'-CZH9-NH-C-R, X- II
wherein RS and R, are the same as each other or different and are selected from the group consisting of C19 to C22 alkyl or alkenyl groups, and R~ is selected from the groups consisting of methyl or (CnH,nO) .t H wherein n is 2 or 3 and X is from 1 to 5, and wherein X- is an anion, preferably selected from the group consisting of halides, sulphates, acetates or alkyl sulphates having from 1 to 3 carbon atoms in the alkyl chain.
It is particularly preferred that the difattyalkyl amidoammonium salt should have a particularly low level of residual ethoxylated amine, specifically less than about 120 of the difattyalkyl amidoammonium salt;
(ii) ester-linked trialkyl ammonium salts of formula:
2 .~ ~3 9 4 2 ~ p~/Ep93/01703 - 7 _ R8R9R1oN' CH" CH X- III
CHZOOCRIz wherein R8, R9 and Rlo are each an alkyl or hydroxyalkyl group containing from 1 to 4 carbon atoms or a benzyl group; R11 and Rlz are each an alkyl or alkenyl chain containing from 11 to 23 carbon atoms and X- is an anion as defined above. Such ester linked compounds are more fully described in,U.S.
4,137,180, Naik.
(iii) imidazolinium salts of formula;
~N iHz Rlz--C I
~y + j / N CHz H3C ~ I
CzH4 NH
O=C
Rm wherein Rlz and R,3 are the same or different and are selected from the group consisting of C,4 to Czz alkyl or alkenyl groups, and wherein X- is an anion. Preferred compounds are those where Rlz and R1, are hydrogenated tallow.
Particularly preferred compositions comprise from about 20~
to about 35~ of a difatty alkyl amidoammonium salt of formula II above and from 2~ to about lOg of a second cationic conditioning of formulas I, III and IV or mixtures thereof.
_ g _ x.21 394 24 preferably the composition comprises from O.Olo to 0.5~ of an inorganic water-soluble ionizable salt, more preferably 0.10 to 0.3%. Examples of suitable salts are the halides of the group lA and 2A metals of the Periodic Table of Elements e.g., sodium chloride, potassium bromide, lithium chloride, calcium chloride and magnesium chloride.
Various optional materials such as are ordinarily used in fabric conditioning compositions can be used in the compositions herein. These include, for example, perfumes at 0.05% to 1.5%, antimicrobials at 0.01 to 0.2~ and dyes at O.OOlo to O.Olo.
The process of the invention enables concentrated compositions to be made on a commercial scale. The continuous process avoids the need to mix large quantities of highly viscous gels as would be encountered in a batch process and has the advantage that less energy is consumed than in an equivalent batch process.
The continuous mixer comprises a 10 cm diameter pipeline equipped with a series of in-line mixers. Addition of the components of the composition is achieved via ports located immediately upstream of a mixer at various points along the pipeline. Dynamic mixers are used to mix the active;and water and may be Gifford-Wood'''H' type equipped with a turbine capable of peripheral velocities of from 0 to 30 metres per second.
Alternative dynamic mixers to the Gifford-Wood type are Ika'~', RossTM and Dicon'r'"'.
A preferred embodiment of the process is as follows. The cationic fabric conditioning agent is heated until molten and mixed in an in-line dynamic mixer with a premix of deionized water, preservative and dye to form a homogeneous dispersion of the active in water. A solution of calcium chloride in water (2.5-lOg) is dosed and mixed under controlled shear ~6i81 - 21394 _ g _ into the dispersion in a series of distinct sequential - additions. The stream of fabric conditioning compositions is then cooled in-line and again dosed with calcium chloride.
Optionally further cooling takes place by collecting the product in an agitator vessel and recirculating the product through a heat exchanger. Calcium chloride is dosed again to adjust the viscosity and perfume is added and mixed in a relay tank.
Preferably the calcium chloride is dosed and mixed into the active once the homogeneous dispersion has been formed, that is the salt is added after the active has been mixed with water. we have found that particularly stable compositions are formed in th;~s way.
By use of this process fabric conditioning compositions can be manufactured at a rate of up to 756 litres per minute, more typically 189 to 567 litres per minute.
It is essential that when the molten fabric conditioning active and water are mixed, a homogeneous dispersion of the active is formed. Due to the viscosity resulting from water/active contacting, mixing with a dynamic mixer capable of developing a high shear rate enables the formation of a homogeneous dispersion of active particles. Homogeneity and control of the particle size distribution achieved in this manner is not possible in a batch mixer since insufficient shear is available to break up the viscous gel. Similarly, insufficient shear during salt addition results in a poor and delayed distribution of salt into the mix and attendant instability.
Preferably the molten fabric conditioning active and water are mixed in first one and then another in-line dynamic mixer before any salt addition takes place.
We have found that multistage addition of electrolyte is critical to producing stable fabric conditioning AMENDED SHEET
i 21 3942 compositions. Preferably the electrolyte is added in three stages, more preferably five stages. More preferably the electrolyte additions are not all equal with at least one portion being smaller than a subsequent portion. Preferably there is a 2 to 60 second residence time in the pipeline between each mixing stage, more preferably 4 to 20 seconds most preferably 4 to 15 seconds.
The following non-limiting examples illustrates the present invention.
0 of components in compositions indicates o by weight Example 1 The following example shows the importance of controlled shear in the mixing of the cationic fabric conditioning agent and water.
A composition comprising 16~ ACCOSOFT 540TM (a diamino ammonium methyl sulfate ex. Stepan), 6.5~ Adogen 442T"' (a tallow dimethyl ammonium chloride ex. Sherex), 0.18% CaCl~, 1.0%
perfume, 0.10 glutaraldehyde and 0.0050 Acid Blue 80 was made by pumping, with a Bran and LubbeTM piston positive displacement pump, the molten actives at 71.1°C and water at 71.1°C containing the glutaraldehyde and dye into the-pipeline of a continuous mixer immediately upstream of an in-line dynamic mixer of type 2 inch Gifford-wood and mixing at varying speeds. The resulting dispersion was pumped along the pipeline of the continuous mixer for 4 seconds and mixed with 0.02% CaCl, from a i0o solution in a further shear mixer of type Dicon at a motor speed of up to 3600rpm. The resulting composition was pumped along the pipeline of the continuous mixer for 4 seconds and mixed with 0.04% CaCl= in a further shear mixer, a Charlotte colloid mill. The resulting composition was pumped along the pipeline of the continuous mixer for 4 seconds and mixed with 0.08 CaCl= in a further shear mixer. The resulting composition was fed to a relay tank where it was cooled to 26.7°C and a further addition cf 0.04% CaCl- and l.Oo perfume was made with mixing - by an A310 Lightnin agitator.
The resulting compositions had the following properties:
SAMPLE
A* B C* D*
Active/Water Dynamic Mixer 0 15.75 34.12 52.5 Peripheral Velocity ft/s Initial V=scosity of Comp. 77 55 90 121 Haake 110s-'cP
Mean Particle Size of active 2.81 1.43 0.35 0.47 in microns [ D(v,0.5) ]
Particle size of 100 of the 0.62 0.47 0.17 0.26 distribution [ D(v,0.1) ]
0 of particle size of 10~ of 22 32.9 - -the distribution to the mean particle size.
1 week at 40.6C Viscosity - 220 1112 1944 Brookfield Ncl or 3 Spindle 2 week at 40.6C Viscosity - 233 1144 2168 Brookfield Nol or 3 Spindle 3 week at 40.6C Viscosity - 228 1144 --Brookfield Nol or 3 Spindle 4 week at 40.6C Viscosity - 243 1368 --Brookfield No1 or 3 Spindle * - Comparat.ive Examples As can be seen from the results above, the dynamic mixer speed in the first stage of the process has a significant effect on the viscosity of the composition generated even after ident_cal salt additions. Controlled shear mixing of the active and water is essential to the generation of an acceptable product.
This example shows the effect of the salt addition profile on the stability of the composition.
AMENDED SHEET
A composition comprising 160 ACCOSOFT 540, 6.50 Adogen 442, 0.180 CaCl" O.lo glutaraldehyde and 0.0050 Acid Blue 80 and l.Oo perfume was made as described in Example 1 except that active/water mix was mixed at 300 speed and CaCl, additions were made in the continuous mixer as detailed in the table below.
A B C D
Active/Water Dynamic Mixer 15.75 15.75 15.75 15.75 Peripheral Velocity ft/s First CaCl, addition a 0.02 0.04 0.07 0.14 Second CaCl2 addition o 0.04 0.10 0.07 0.00 Third CaCl, addition o 0.08 0.00 0.00 0.00 Mean Particle size 1.68 1.30 1.38 1.35 10~ distribution particle size 0.6 0.3 0.33 0.38 0 of 10% to mean particle size 35.7 23 23.9 28 1 week at 40.6C Viscosity 120 430 265 1048 Brookfield Nol or 3 Spindle cP
2 week at 40.6C Viscosity 103 951 423 1040 Brookfield No1 or 3 Spindle cP
3 week at 40.6C Viscosity 143 1176 952 1176 Brookfield Nol or 3 Spindle cP
These results show that a three stage salt addition (sample A) during processing gives a rise to a lower viscosity in the final composition.
This example shows the effect of the particle size distribution on the stability of the composition.
A composition comprising by weight 180 ACCOSOFT 540 HC (ex Stepan), 6.5% Adogen 442E-83 (ex Stepan), 0.240 CaCl2, 1.1~
perfume, 0.1~ glutaraldehyde, 0.005a Acid Blue 80 and balance water was made as described in example 1 except that (i) the active/water mix was mixed in a ROSS dynamic mixer at various speeds, (ii) the dye was added in the relay mixer and (iii) a total of five salt additions were made to the composition in AMENDED SHEET
_. _ 13 - 2139424 the following discrete portions O.Olo, 0.020 and 0.030 as a _ 2.5~ solution, 0.04 and 0.04 by weight as a loo solution.
The resulting composition was finished to 0.24% CaCl~ in a relay mixer where perfume and dye were also added. The particle size distribution and viscosity following various periods of storage up to 4 weeks at 40.6°C were measured as detailed above.
Composition Mean loo Total No. o of 10~
Particle Disribu'~ of weeks to mean Size Particle at 105F
Microns Size below 800cP
A* 2.26 0.47 0 20.8 B 1.14 0.32 0 28.1 C 1.22 0.29 1 23.8 D 1.17 0.30 1 25.6 0.93 0.27 1 29.0 _ 1.23 0.28 1 22.8 G 1.23 0.31 2 25.2 H 1.22 0.28 2 23.0 _ 2.44 0.58 2 23.8 J 1 . 18 0 . 3-2 2 2 7 . 1 K 2.08 0.47 2 22.6 1.57 0.45 2 28.7 M 1.04 0.35 3 33.7 0.93 0.32 3 39.3 O 3.96 1.32 3 34.4 ? 1.59 0.6 3 37.7 2.07 0.74 3 35.7 R 1.39 0.49 3 35.3 S 3.87 1.39 3 35.9 T 2.05 0.81 3 39.5 L' 1.27 0.54 3 42.5 V 1.24 0.46 3 37.1 ini 1.99 0.81 3 40.7 AMENDED SHEET
WO 94/01523 ~ 13 9 4 2 4 PCT/EP93/01703 Composition Mean 10~ Total No. ~ of 10~
Particle Disribu'" of weeks to mean Size Particle at 105F
Microns Size below X 1.15 0.41 3 35.7 Y 1.1 0.4 3 36.4 Z 2.08 0.7 3 33.7 AA 1.88 0.79 ~ 3 42.0 AB 2.03 0.81 4 39.9 AC 2.04 0.74 4 36.3 AD 2.04 0.71 4 34.3 AE 2.03 0.7 4 35.0 AF 1.93 0.67 4 34.7 AG 2.12 0.69 4 32.5 AH 2.08 0.74 4 35.6 AI 3.05 1.15 4 37.7 AJ 2.10 0.77 4 36.7 AK 1.86 0.72 4 38.7 AL . 2.89 0.93 4 32.2 AM 0.78 0.26 4 33.3 AN 0.77 0.26 4 33.8 AO 0.79 0.26 4 32.9 AP 0.78 0.26 4 33.3 AQ 0.84 0.27 4 32.1 AR 2.08 0.73 4 35.1 AS 1.59 0.61 4 38.4 AT 1.29 0.36 4 27.9 Composition Mean loo Total No. o of 10~
Particle Disribu'" of weeks to mean Size Particle at 40.6C
Microns Size below 800cP
AU 0.79 0.25 4 32.5 AV 1.42 0.48 4 33.8 AW 2.57 0.8 4 31.1 AX 2.15 0.74 4 34.4 * Comparative Examples These results show that preferred stabilities are obtained from a 24.5 active mixture when the mean particle size is between 0.7 and 4 microns and the percentage of the particle size of 10~ of the distribution to the mean particle size is at least 29~, preferably at least 320.
This example shows the effect of controlled shear mixing the active/water mixture in two dynamic mixers before salt addition.
A composition comprising 18~ ACCOSOFT 540 HC, 6.5g Adogen 442E-83, 1.10 perfume, 0.1% glutaraldehyde, 0.240 CaCl~ and 0.0050 Acid Blue 80 was made as described in Example 3 except that Ross Dynamic mixers were used in-line at all stages and a series of five salt additions were made in the continuous mixer. The salt additions were as described in Example 3.
AMENDED SHEET
~13~1~~'~
A B*
1st Active/Water Dynamic 2500 10000 Mixer Motor Speed rpm 2nd Active/Water Dynamic 10000 10000 Mixer Motor Speed rpm 1st salt addition Motor Velocity rpm 7500 3000 2nd salt addition Motor Velocity rpm 3000 3000 3rd salt addition Motor Velocity rpm 3000 3000 4th salt addition Motor Velocity rpm 3000 3000 5th salt addition Motor Velocity rpm 3000 3000 Mean Particle Size microns 2.1 0.47 10~ distribu'n particle size microns 0.77 0.19 ~ of 10% size to mean size 36.8 --Viscosity after 1 week at 40.6C cp 78 2225 Viscosity after 4 weeks at 40.6C cp 240 --* Comparative Examples AMENDED SHEET
CHZOOCRIz wherein R8, R9 and Rlo are each an alkyl or hydroxyalkyl group containing from 1 to 4 carbon atoms or a benzyl group; R11 and Rlz are each an alkyl or alkenyl chain containing from 11 to 23 carbon atoms and X- is an anion as defined above. Such ester linked compounds are more fully described in,U.S.
4,137,180, Naik.
(iii) imidazolinium salts of formula;
~N iHz Rlz--C I
~y + j / N CHz H3C ~ I
CzH4 NH
O=C
Rm wherein Rlz and R,3 are the same or different and are selected from the group consisting of C,4 to Czz alkyl or alkenyl groups, and wherein X- is an anion. Preferred compounds are those where Rlz and R1, are hydrogenated tallow.
Particularly preferred compositions comprise from about 20~
to about 35~ of a difatty alkyl amidoammonium salt of formula II above and from 2~ to about lOg of a second cationic conditioning of formulas I, III and IV or mixtures thereof.
_ g _ x.21 394 24 preferably the composition comprises from O.Olo to 0.5~ of an inorganic water-soluble ionizable salt, more preferably 0.10 to 0.3%. Examples of suitable salts are the halides of the group lA and 2A metals of the Periodic Table of Elements e.g., sodium chloride, potassium bromide, lithium chloride, calcium chloride and magnesium chloride.
Various optional materials such as are ordinarily used in fabric conditioning compositions can be used in the compositions herein. These include, for example, perfumes at 0.05% to 1.5%, antimicrobials at 0.01 to 0.2~ and dyes at O.OOlo to O.Olo.
The process of the invention enables concentrated compositions to be made on a commercial scale. The continuous process avoids the need to mix large quantities of highly viscous gels as would be encountered in a batch process and has the advantage that less energy is consumed than in an equivalent batch process.
The continuous mixer comprises a 10 cm diameter pipeline equipped with a series of in-line mixers. Addition of the components of the composition is achieved via ports located immediately upstream of a mixer at various points along the pipeline. Dynamic mixers are used to mix the active;and water and may be Gifford-Wood'''H' type equipped with a turbine capable of peripheral velocities of from 0 to 30 metres per second.
Alternative dynamic mixers to the Gifford-Wood type are Ika'~', RossTM and Dicon'r'"'.
A preferred embodiment of the process is as follows. The cationic fabric conditioning agent is heated until molten and mixed in an in-line dynamic mixer with a premix of deionized water, preservative and dye to form a homogeneous dispersion of the active in water. A solution of calcium chloride in water (2.5-lOg) is dosed and mixed under controlled shear ~6i81 - 21394 _ g _ into the dispersion in a series of distinct sequential - additions. The stream of fabric conditioning compositions is then cooled in-line and again dosed with calcium chloride.
Optionally further cooling takes place by collecting the product in an agitator vessel and recirculating the product through a heat exchanger. Calcium chloride is dosed again to adjust the viscosity and perfume is added and mixed in a relay tank.
Preferably the calcium chloride is dosed and mixed into the active once the homogeneous dispersion has been formed, that is the salt is added after the active has been mixed with water. we have found that particularly stable compositions are formed in th;~s way.
By use of this process fabric conditioning compositions can be manufactured at a rate of up to 756 litres per minute, more typically 189 to 567 litres per minute.
It is essential that when the molten fabric conditioning active and water are mixed, a homogeneous dispersion of the active is formed. Due to the viscosity resulting from water/active contacting, mixing with a dynamic mixer capable of developing a high shear rate enables the formation of a homogeneous dispersion of active particles. Homogeneity and control of the particle size distribution achieved in this manner is not possible in a batch mixer since insufficient shear is available to break up the viscous gel. Similarly, insufficient shear during salt addition results in a poor and delayed distribution of salt into the mix and attendant instability.
Preferably the molten fabric conditioning active and water are mixed in first one and then another in-line dynamic mixer before any salt addition takes place.
We have found that multistage addition of electrolyte is critical to producing stable fabric conditioning AMENDED SHEET
i 21 3942 compositions. Preferably the electrolyte is added in three stages, more preferably five stages. More preferably the electrolyte additions are not all equal with at least one portion being smaller than a subsequent portion. Preferably there is a 2 to 60 second residence time in the pipeline between each mixing stage, more preferably 4 to 20 seconds most preferably 4 to 15 seconds.
The following non-limiting examples illustrates the present invention.
0 of components in compositions indicates o by weight Example 1 The following example shows the importance of controlled shear in the mixing of the cationic fabric conditioning agent and water.
A composition comprising 16~ ACCOSOFT 540TM (a diamino ammonium methyl sulfate ex. Stepan), 6.5~ Adogen 442T"' (a tallow dimethyl ammonium chloride ex. Sherex), 0.18% CaCl~, 1.0%
perfume, 0.10 glutaraldehyde and 0.0050 Acid Blue 80 was made by pumping, with a Bran and LubbeTM piston positive displacement pump, the molten actives at 71.1°C and water at 71.1°C containing the glutaraldehyde and dye into the-pipeline of a continuous mixer immediately upstream of an in-line dynamic mixer of type 2 inch Gifford-wood and mixing at varying speeds. The resulting dispersion was pumped along the pipeline of the continuous mixer for 4 seconds and mixed with 0.02% CaCl, from a i0o solution in a further shear mixer of type Dicon at a motor speed of up to 3600rpm. The resulting composition was pumped along the pipeline of the continuous mixer for 4 seconds and mixed with 0.04% CaCl= in a further shear mixer, a Charlotte colloid mill. The resulting composition was pumped along the pipeline of the continuous mixer for 4 seconds and mixed with 0.08 CaCl= in a further shear mixer. The resulting composition was fed to a relay tank where it was cooled to 26.7°C and a further addition cf 0.04% CaCl- and l.Oo perfume was made with mixing - by an A310 Lightnin agitator.
The resulting compositions had the following properties:
SAMPLE
A* B C* D*
Active/Water Dynamic Mixer 0 15.75 34.12 52.5 Peripheral Velocity ft/s Initial V=scosity of Comp. 77 55 90 121 Haake 110s-'cP
Mean Particle Size of active 2.81 1.43 0.35 0.47 in microns [ D(v,0.5) ]
Particle size of 100 of the 0.62 0.47 0.17 0.26 distribution [ D(v,0.1) ]
0 of particle size of 10~ of 22 32.9 - -the distribution to the mean particle size.
1 week at 40.6C Viscosity - 220 1112 1944 Brookfield Ncl or 3 Spindle 2 week at 40.6C Viscosity - 233 1144 2168 Brookfield Nol or 3 Spindle 3 week at 40.6C Viscosity - 228 1144 --Brookfield Nol or 3 Spindle 4 week at 40.6C Viscosity - 243 1368 --Brookfield No1 or 3 Spindle * - Comparat.ive Examples As can be seen from the results above, the dynamic mixer speed in the first stage of the process has a significant effect on the viscosity of the composition generated even after ident_cal salt additions. Controlled shear mixing of the active and water is essential to the generation of an acceptable product.
This example shows the effect of the salt addition profile on the stability of the composition.
AMENDED SHEET
A composition comprising 160 ACCOSOFT 540, 6.50 Adogen 442, 0.180 CaCl" O.lo glutaraldehyde and 0.0050 Acid Blue 80 and l.Oo perfume was made as described in Example 1 except that active/water mix was mixed at 300 speed and CaCl, additions were made in the continuous mixer as detailed in the table below.
A B C D
Active/Water Dynamic Mixer 15.75 15.75 15.75 15.75 Peripheral Velocity ft/s First CaCl, addition a 0.02 0.04 0.07 0.14 Second CaCl2 addition o 0.04 0.10 0.07 0.00 Third CaCl, addition o 0.08 0.00 0.00 0.00 Mean Particle size 1.68 1.30 1.38 1.35 10~ distribution particle size 0.6 0.3 0.33 0.38 0 of 10% to mean particle size 35.7 23 23.9 28 1 week at 40.6C Viscosity 120 430 265 1048 Brookfield Nol or 3 Spindle cP
2 week at 40.6C Viscosity 103 951 423 1040 Brookfield No1 or 3 Spindle cP
3 week at 40.6C Viscosity 143 1176 952 1176 Brookfield Nol or 3 Spindle cP
These results show that a three stage salt addition (sample A) during processing gives a rise to a lower viscosity in the final composition.
This example shows the effect of the particle size distribution on the stability of the composition.
A composition comprising by weight 180 ACCOSOFT 540 HC (ex Stepan), 6.5% Adogen 442E-83 (ex Stepan), 0.240 CaCl2, 1.1~
perfume, 0.1~ glutaraldehyde, 0.005a Acid Blue 80 and balance water was made as described in example 1 except that (i) the active/water mix was mixed in a ROSS dynamic mixer at various speeds, (ii) the dye was added in the relay mixer and (iii) a total of five salt additions were made to the composition in AMENDED SHEET
_. _ 13 - 2139424 the following discrete portions O.Olo, 0.020 and 0.030 as a _ 2.5~ solution, 0.04 and 0.04 by weight as a loo solution.
The resulting composition was finished to 0.24% CaCl~ in a relay mixer where perfume and dye were also added. The particle size distribution and viscosity following various periods of storage up to 4 weeks at 40.6°C were measured as detailed above.
Composition Mean loo Total No. o of 10~
Particle Disribu'~ of weeks to mean Size Particle at 105F
Microns Size below 800cP
A* 2.26 0.47 0 20.8 B 1.14 0.32 0 28.1 C 1.22 0.29 1 23.8 D 1.17 0.30 1 25.6 0.93 0.27 1 29.0 _ 1.23 0.28 1 22.8 G 1.23 0.31 2 25.2 H 1.22 0.28 2 23.0 _ 2.44 0.58 2 23.8 J 1 . 18 0 . 3-2 2 2 7 . 1 K 2.08 0.47 2 22.6 1.57 0.45 2 28.7 M 1.04 0.35 3 33.7 0.93 0.32 3 39.3 O 3.96 1.32 3 34.4 ? 1.59 0.6 3 37.7 2.07 0.74 3 35.7 R 1.39 0.49 3 35.3 S 3.87 1.39 3 35.9 T 2.05 0.81 3 39.5 L' 1.27 0.54 3 42.5 V 1.24 0.46 3 37.1 ini 1.99 0.81 3 40.7 AMENDED SHEET
WO 94/01523 ~ 13 9 4 2 4 PCT/EP93/01703 Composition Mean 10~ Total No. ~ of 10~
Particle Disribu'" of weeks to mean Size Particle at 105F
Microns Size below X 1.15 0.41 3 35.7 Y 1.1 0.4 3 36.4 Z 2.08 0.7 3 33.7 AA 1.88 0.79 ~ 3 42.0 AB 2.03 0.81 4 39.9 AC 2.04 0.74 4 36.3 AD 2.04 0.71 4 34.3 AE 2.03 0.7 4 35.0 AF 1.93 0.67 4 34.7 AG 2.12 0.69 4 32.5 AH 2.08 0.74 4 35.6 AI 3.05 1.15 4 37.7 AJ 2.10 0.77 4 36.7 AK 1.86 0.72 4 38.7 AL . 2.89 0.93 4 32.2 AM 0.78 0.26 4 33.3 AN 0.77 0.26 4 33.8 AO 0.79 0.26 4 32.9 AP 0.78 0.26 4 33.3 AQ 0.84 0.27 4 32.1 AR 2.08 0.73 4 35.1 AS 1.59 0.61 4 38.4 AT 1.29 0.36 4 27.9 Composition Mean loo Total No. o of 10~
Particle Disribu'" of weeks to mean Size Particle at 40.6C
Microns Size below 800cP
AU 0.79 0.25 4 32.5 AV 1.42 0.48 4 33.8 AW 2.57 0.8 4 31.1 AX 2.15 0.74 4 34.4 * Comparative Examples These results show that preferred stabilities are obtained from a 24.5 active mixture when the mean particle size is between 0.7 and 4 microns and the percentage of the particle size of 10~ of the distribution to the mean particle size is at least 29~, preferably at least 320.
This example shows the effect of controlled shear mixing the active/water mixture in two dynamic mixers before salt addition.
A composition comprising 18~ ACCOSOFT 540 HC, 6.5g Adogen 442E-83, 1.10 perfume, 0.1% glutaraldehyde, 0.240 CaCl~ and 0.0050 Acid Blue 80 was made as described in Example 3 except that Ross Dynamic mixers were used in-line at all stages and a series of five salt additions were made in the continuous mixer. The salt additions were as described in Example 3.
AMENDED SHEET
~13~1~~'~
A B*
1st Active/Water Dynamic 2500 10000 Mixer Motor Speed rpm 2nd Active/Water Dynamic 10000 10000 Mixer Motor Speed rpm 1st salt addition Motor Velocity rpm 7500 3000 2nd salt addition Motor Velocity rpm 3000 3000 3rd salt addition Motor Velocity rpm 3000 3000 4th salt addition Motor Velocity rpm 3000 3000 5th salt addition Motor Velocity rpm 3000 3000 Mean Particle Size microns 2.1 0.47 10~ distribu'n particle size microns 0.77 0.19 ~ of 10% size to mean size 36.8 --Viscosity after 1 week at 40.6C cp 78 2225 Viscosity after 4 weeks at 40.6C cp 240 --* Comparative Examples AMENDED SHEET
Claims (8)
1. A concentrated aqueous fabric conditioning composition comprising a homogeneous dispersion of from 8% to 80% by weight of cationic conditioning active particles characterised in that the cationic particles have a size distribution such that the mean size of the particles is from 0.7 to 10 microns as measured by the Malvern Particle Size Analyzer and such that the particle size of 10% of the distribution [D(v, 0.1)] is at least 23% of the mean particle size, as measured by the Malvern Particle Size Analyzer; and the concentrated aqueous fabric conditioning composition is stable and pourable and has a viscosity below about 1000 centipoises after 2 weeks storage at 14.7°C as measured by a Brookfield Viscometer on spindle No. 1 or 3.
2. An aqueous fabric conditioning composition as claimed in claim 1 wherein 10% of the distribution has a particle size of at least 29% of the mean particle size as measured by Malvern Particle Size Analyzer.
3. An aqueous fabric conditioning composition as claimed in claim 1 or claim 2 wherein 10% of the distribution has a particle size of between 30% and 50% of the mean particle size as measured by Malvern Particle Size Analyzer.
4. A concentrated aqueous fabric conditioning composition as claimed in claim 1 wherein the composition comprises from 0.01% to 0.5% by weight of an ionizable salt.
5. A concentrated aqueous fabric conditioning composition as claimed in any one of the preceding claims wherein the active particles have a size distribution such that the mean particle size is from 0.7 to 5 microns as measured by Malvern Particle Size Analyzer.
6. A continuous process for making an aqueous fabric conditioning composition as claimed in any one of claims 1 to 5 in which said composition comprises from 8% to 80% by weight of a cationic fabric conditioning active and from 0.01% to 0.5% of an ionizable salt said process comprising the steps of:
(i) selecting a cationic fabric conditioning active of formula wherein R1 and R2 are each hydrocarbyl groups containing from 1 to 25 carbon atoms, R3 and R4 are each hydrocarbyl groups containing from 1 to 6 carbon atoms, x is an anion and n is an integer from 1 to about 3, (ii) adding the cationic fabric conditioning active to a continuous mixer, (iii) dispersing the active in water under controlled shear in the continuous mixer to form a homogeneous dispersion of the active, (iv) mixing the dispersion with at least 3 discrete portions of the ionizable salt under controlled shear to maintain the homogeneous dispersion.
(i) selecting a cationic fabric conditioning active of formula wherein R1 and R2 are each hydrocarbyl groups containing from 1 to 25 carbon atoms, R3 and R4 are each hydrocarbyl groups containing from 1 to 6 carbon atoms, x is an anion and n is an integer from 1 to about 3, (ii) adding the cationic fabric conditioning active to a continuous mixer, (iii) dispersing the active in water under controlled shear in the continuous mixer to form a homogeneous dispersion of the active, (iv) mixing the dispersion with at least 3 discrete portions of the ionizable salt under controlled shear to maintain the homogeneous dispersion.
7. A continuous process for making an aqueous fabric conditioning composition as claimed in claim 6 wherein the discrete portions of ionizable salt are added such that at least one portion is smaller than a subsequent portion.
8. A concentrated aqueous fabric conditioning composition obtained by the process of claim 6 or claim 7.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/909,359 US5288417A (en) | 1992-07-06 | 1992-07-06 | Fabric conditioning compositions and process for making them |
| US909359 | 1992-07-06 | ||
| PCT/EP1993/001703 WO1994001523A1 (en) | 1992-07-06 | 1993-06-30 | Fabric conditioning compositions and process for making them |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2139424A1 CA2139424A1 (en) | 1994-01-20 |
| CA2139424C true CA2139424C (en) | 2000-11-14 |
Family
ID=25427103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002139424A Expired - Lifetime CA2139424C (en) | 1992-07-06 | 1993-06-30 | Fabric conditioning compositions and process for making them |
Country Status (6)
| Country | Link |
|---|---|
| US (2) | US5288417A (en) |
| AU (1) | AU674014B2 (en) |
| BR (1) | BR9306690A (en) |
| CA (1) | CA2139424C (en) |
| WO (1) | WO1994001523A1 (en) |
| ZA (1) | ZA934843B (en) |
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| US5409621A (en) * | 1991-03-25 | 1995-04-25 | Lever Brothers Company, Division Of Conopco, Inc. | Fabric softening composition |
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| CN102120167B (en) | 2009-09-18 | 2014-10-29 | 国际香料和香精公司 | encapsulated active material |
| MX369325B (en) | 2011-03-18 | 2019-11-05 | Int Flavors & Fragrances Inc | Microcapsules produced from blended sol-gel precursors and method for producing the same. |
| EP2768933B1 (en) * | 2011-10-20 | 2015-10-14 | The Procter and Gamble Company | A continuous process of making a fabric softener composition |
| US9610228B2 (en) | 2013-10-11 | 2017-04-04 | International Flavors & Fragrances Inc. | Terpolymer-coated polymer encapsulated active material |
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| CN107708429A (en) | 2015-04-24 | 2018-02-16 | 国际香料和香精公司 | delivery system and preparation method thereof |
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| CN115089512A (en) | 2016-02-18 | 2022-09-23 | 国际香料和香精公司 | Polyurea capsule composition |
| MX2019003078A (en) | 2016-09-16 | 2019-07-08 | Int Flavors & Fragrances Inc | Microcapsule compositions stabilized with viscosity control agents. |
| US20180085291A1 (en) | 2016-09-28 | 2018-03-29 | International Flavors & Fragrances Inc. | Microcapsule compositions containing amino silicone |
| WO2019076920A1 (en) * | 2017-10-16 | 2019-04-25 | Microtherm Nv | Equipment for injection of a dispersion in a fabric and method of manufacturing a fabric containing nanostructure particle powder |
| WO2019076909A1 (en) * | 2017-10-16 | 2019-04-25 | Microtherm Nv | Equipment for injection of a dispersion in a fabric and method of manufacturing a fabric containing nanostructure particle powder |
| WO2019076922A1 (en) * | 2017-10-16 | 2019-04-25 | Microtherm Nv | Equipment for injection of a dispersion in a fabric and method of manufacturing a fabric containing nanostructure particle powder |
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| EP3970690A3 (en) | 2020-06-05 | 2022-07-06 | International Flavors & Fragrances Inc. | Consumer products with improved aesthetics |
| EP4124383A1 (en) | 2021-07-27 | 2023-02-01 | International Flavors & Fragrances Inc. | Biodegradable microcapsules |
| EP4154974A1 (en) | 2021-09-23 | 2023-03-29 | International Flavors & Fragrances Inc. | Biodegradable microcapsules |
| WO2023102033A1 (en) | 2021-12-03 | 2023-06-08 | International Flavors & Fragrances Inc. | Aqueous fabric conditioner compositions with high performance fragrances |
| EP4212239A1 (en) | 2022-01-14 | 2023-07-19 | International Flavors & Fragrances Inc. | Biodegradable prepolymer microcapsules |
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| US3681241A (en) * | 1968-03-04 | 1972-08-01 | Lever Brothers Ltd | Fabric softening |
| US3954634A (en) * | 1973-07-27 | 1976-05-04 | S. C. Johnson & Son, Inc. | Stable, low-viscosity fabric softener |
| US3933871A (en) * | 1973-11-12 | 1976-01-20 | Armstrong Chemical Company, Inc. | Fabric softener compound and processes for preparing and using the same |
| US3974076A (en) * | 1974-01-11 | 1976-08-10 | The Procter & Gamble Company | Fabric softener |
| GB1567947A (en) * | 1976-07-02 | 1980-05-21 | Unilever Ltd | Esters of quaternised amino-alcohols for treating fabrics |
| PH18436A (en) * | 1980-11-07 | 1985-07-08 | Unilever Nv | A fabric softening composition and a process for preparing it |
| US4439335A (en) * | 1981-11-17 | 1984-03-27 | The Procter & Gamble Company | Concentrated fabric softening compositions |
| US4464273A (en) * | 1982-02-10 | 1984-08-07 | Lever Brothers Company | Fabric softening composition |
| US4555349A (en) * | 1983-04-08 | 1985-11-26 | Lever Brothers Company | Fabric softening compositions |
| US4661270A (en) * | 1983-05-11 | 1987-04-28 | Colgate-Palmolive Company | Concentrated fabric softening composition and methods for making same |
| GB8414944D0 (en) * | 1984-06-12 | 1984-07-18 | Ici Plc | Fabric conditioners |
| US4844823A (en) * | 1985-01-30 | 1989-07-04 | Colgate-Palmolive Company | Fabric softener composition containing di-esterified long chain fatty acid quaternary ammonium salt |
| US4654152A (en) * | 1985-10-07 | 1987-03-31 | Domtar Inc. | Base mix fabric softener |
| US4789491A (en) * | 1987-08-07 | 1988-12-06 | The Procter & Gamble Company | Method for preparing biodegradable fabric softening compositions |
| US4844821A (en) * | 1988-02-10 | 1989-07-04 | The Procter & Gamble Company | Stable liquid laundry detergent/fabric conditioning composition |
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| US4994193A (en) * | 1988-12-15 | 1991-02-19 | The Procter & Gamble Company | Liquid fabric softener |
| GB8900027D0 (en) * | 1989-01-03 | 1989-03-01 | Procter & Gamble | Rinse-added fabric-softening compositions |
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| JPH0441776A (en) * | 1990-06-01 | 1992-02-12 | Kao Corp | Liquid soft finishing agent |
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| TW213964B (en) * | 1991-06-19 | 1993-10-01 | Procter & Gamble |
-
1992
- 1992-07-06 US US07/909,359 patent/US5288417A/en not_active Expired - Lifetime
-
1993
- 1993-06-30 BR BR9306690A patent/BR9306690A/en not_active Application Discontinuation
- 1993-06-30 WO PCT/EP1993/001703 patent/WO1994001523A1/en active Application Filing
- 1993-06-30 AU AU45628/93A patent/AU674014B2/en not_active Ceased
- 1993-06-30 CA CA002139424A patent/CA2139424C/en not_active Expired - Lifetime
- 1993-07-06 ZA ZA934843A patent/ZA934843B/en unknown
-
1994
- 1994-01-05 US US08/177,505 patent/US5411671A/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| ZA934843B (en) | 1995-01-06 |
| WO1994001523A1 (en) | 1994-01-20 |
| US5411671A (en) | 1995-05-02 |
| AU4562893A (en) | 1994-01-31 |
| AU674014B2 (en) | 1996-12-05 |
| CA2139424A1 (en) | 1994-01-20 |
| BR9306690A (en) | 1998-12-08 |
| US5288417A (en) | 1994-02-22 |
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Legal Events
| Date | Code | Title | Description |
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| EEER | Examination request |