CA2085618A1 - Free-flowing powder fabric softening composition and process for its manufacture - Google Patents

Free-flowing powder fabric softening composition and process for its manufacture

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Publication number
CA2085618A1
CA2085618A1 CA002085618A CA2085618A CA2085618A1 CA 2085618 A1 CA2085618 A1 CA 2085618A1 CA 002085618 A CA002085618 A CA 002085618A CA 2085618 A CA2085618 A CA 2085618A CA 2085618 A1 CA2085618 A1 CA 2085618A1
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CA
Canada
Prior art keywords
compound
water
weight
softening
cationic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
CA002085618A
Other languages
French (fr)
Inventor
Nahum Chavez
Israel Oliveros
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Colgate Palmolive Co
Original Assignee
Nahum Chavez
Israel Oliveros
Colgate-Palmolive
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US07/838,626 external-priority patent/US5368755A/en
Application filed by Nahum Chavez, Israel Oliveros, Colgate-Palmolive filed Critical Nahum Chavez
Publication of CA2085618A1 publication Critical patent/CA2085618A1/en
Abandoned legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/38Cationic compounds
    • C11D1/65Mixtures of anionic with cationic compounds
    • C11D1/652Mixtures of anionic compounds with carboxylic amides or alkylol amides
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/38Cationic compounds
    • C11D1/65Mixtures of anionic with cationic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/835Mixtures of non-ionic with cationic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/86Mixtures of anionic, cationic, and non-ionic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions
    • C11D11/02Preparation in the form of powder by spray drying
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005Other compounding ingredients characterised by their effect
    • C11D3/001Softening compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/26Organic compounds containing nitrogen
    • C11D3/32Amides; Substituted amides
    • C11D3/323Amides; Substituted amides urea or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/38Cationic compounds
    • C11D1/52Carboxylic amides, alkylolamides or imides or their condensation products with alkylene oxides
    • C11D1/523Carboxylic alkylolamides, or dialkylolamides, or hydroxycarboxylic amides (R1-CO-NR2R3), where R1, R2 or R3 contain one hydroxy group per alkyl group
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/38Cationic compounds
    • C11D1/62Quaternary ammonium compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/72Ethers of polyoxyalkylene glycols

Abstract

ABSTRACT

A process of producing a free-flowing spray dried particulate fabric softening composition is provided and comprises the steps of:
(a) forming a crutcher slurry containing:
(i) from about 5 to 40%, by weight, of a cationic quatemary ammonium softening compound;
(ii) from about 0.5 to 15%, by weight, of an anionic and/or a nonionic detergent compound;
(iii) from about 45 to 85%, by weight, of urea, the above percentages being based on the solios content of the slurry, in the absence of water;
(b) mixing the crutcher slurry formed in (a) to provide a uniform mixture or dispersion having an average particle size of less than about 1.0 micron and thereafter;
(c) spray drying the aforesaid mixture or dispersion in a spray tower wherein the water content of the mixture is substantially evaporated to provide free-flowing particles of a softening composition capable of being readily dispersed in water.

Description

M t147~

MEE-FLOWING POWDfR FABRIC SO~J NI~IG COMPOSlTiON
AND PROCESS FOR JTS MANLIFACTVRE

This invention relates to a free-flowing, spray-dried concentrated particulate fabric softening composition which is readi/y dispersible in water and to a process for its manufacture and use. More particularly, the present invenrion relates to an effective fabric softening composition in a form which is convenient for use, capable of containing a re/atively high proportion of cationic fabric softener, and can be economically packaged and shipped.
Fabric softening or conditioning compositions for use in househo/d washing machines are marketed extensive/y in the United States and Europe.
Genera//y, these compositions are aqueous /;quids containing as the principal active ingredient a cationic quaternary ammonium compound to impart a softening effect to fabrics treated therewith in the laundry bath Typica/iy, these fabric softeners ~the common designation for such softening compositionsJ contain from about 5 to 8% of the active catianic softening compound. In a Unlted States washing machine containing about 6~ /iters of water, norma/ly about 90 grams of a 6% active liquid fabric softener is added to the rinse cycle to achieve an acceptable softening leve/
Liqufd fabric softeners, however, have certain inherent disadvantages The level of the active cationic ~uaternary ammon~um compound capahJe of 2~8~18 being introduced into an aqueous system is generally limited by properties of solubiljty of ~he qvaternary compovnd and stability and pourabliity of the f;nal product. Conventional rinse-added fabric softening compositions contain quaternary ammonium compounds, typica//y having two /ong alky/ chains, which are substantia/ly water-insoluble materials. The softening compositions are, therefore, normally in the form of an aqveous dispersion or emulsion.
Conseqvently, at higher concentrations of the active cationic softening compound, genera/Jy above about 6%, by weight, prob/ems in product formu/ation, stabi/ity ~i.e. product separationJ, gel-formation and water dispersibi/ity are /ikely to occvr. At concentrations above about 9%, by weight, of quaternary ammonium compounds, the viscosity and stability of the aqueous liquid softener are often unacceptable for commercial purposes.
There are also economic disadvantages associated with marketing /iqvid fabric softeners. These primari/y re/ate to the substan~ia/ costs of pacJ~aging and shipping bott/es of a di/ute aqveovs /iqvid prodvct containing a re/atively /ow leve/ of active softening ingredient. The pac/~aging also poses a prob/em from an environmental standpoint. The manvfacture and disposal of p/as~ic containers, which are common/y vsed for liqvid hovsehold products are often incompatible with consumer demands in the United States and Evrope for the vse of recyc/able pac/~aging materia/s which are readi/y biodegradabJe.
According/y, there is a need in ttJe art for a fabric softenjng composit;on in particu/ate form capable of containing re/atively high concentrations of active softenjrtg ingredients and capabJe of being supplied in an economica//y pac/~aged form.

Fabric softeners in powdered form are described in the patent literatrJre.
/n U.S. Patent 2,940 816 there is described a powdered fabric softener comprised of a defined quaternary ammonium compound in combination with urea. U.S. Patent 3,256,180 describes a process for producing a fabric softener which comprises reacting urea with a quaternary ammonium compound in the presence of water to form a granular product. U.S. Patent Nos.
3,356,526 and 3,573,091 to Woldman et. al. relate to a process for preparing a powdered quaternary softener wherein a solution of the quaternary ammonium compound is sprayed onto a particulate carrier, such as urea or sodium tripolyphosphate, so as to provide particles of carrier having a coating of the softener.
U.S. Patent 4,427,558 to David discloses fabric softening particles comprised of a quaternary ammonium compound, urea, and a calcium soap such as calcium tallow soap. The process of preparation comprises forming a liquid mixture of the desired components, cooling the liquid to form a solid and then grinding to form particles. Prior to grinding, the solid is "weathered" for severa/ hours, the term "weathering " being used to describe the process of alJowing the water content of the particles to approach equilibrium with rhe environment. Particles may also be formed, according to the disclosure, by "spray coo/ing " a Jiquid mixture whereby a solid is formed with no accompanying loss of water. ~he resulting solid is then ground and weathered.
In European Patent App/ication EP 1315 tProcter & Gamb/e) there is described a process whereby mo/ten partic/es of a quaternary ammonjum compound and a dispersion inhibitor such as a fatty alcohol or fatty acid are ~ttached to spray-drjed base detergent granu/es containing surfactant and builder The emphasis in this as well as other patents in the /iterature is to avoid dispersing the cationic softening compound in the wash water in order to prevent its inactivation in the wash solution, In those patents which seek to provide a quaternary ammonium compound in the form of a readily dispersib/e powder in cold water, with particular emphasis on rinse-cyc/e app/ications, such dispersibility has remained a problem, particularly at higher concentrations of the quaternary compounds.
It has now been discovered that a highly concentrated particulate fabric softening composition can be prepared in accordance with the invention by a spray drying process which provides partic/es of a softening composition containing up to about 40% of a cationic softening compound in combination with a nonionic and/or an anionic surfactant, among other components, which particles are readi/y dispersible jn water and provide effective softening.
SUMMARY OF T~JE INVENTION
According/y, the present invention provides a free-flowing spr~y-dried particu/ate fabric softening composition which is readily dispersible in water comprising:
laJ from about 5 to 40%, by weight, of a cationic quaternary ammonium softening compound;
IbJ from about 0.5 to 15%, by weight, of an anionic and/ora nonionic detergen~ compound; and IcJ from about 45 to 85%, by weight, of urea; the balance being water.

/n a preferred embod~ment of the invention the composition further contains from about 1 to 10%, by weight, of a fatty acid alkano/amide.
The invention a/so encompasses a process of producing a free-flowing spray-dried particuiate fabric softening composition whjch is readi/y dispersible in water comprising:
~aJ forming a crutcher slurry containing:
~iJ from about 5 to 40%, by weight, of a cationic quaternary ammonium softening compound;
~ii/ from about 0. 5 to 15%, by weight, of an anionic and/or a nonionic detergent compound;
~iii) from about I to 10%, by weight, or an a/kanolamide; and tivJ from about 45 to 85%, by weight, of urea, the ~bove percentages being based on the so/ids content of the slurry, in the absence of w3ter;
~bJ mixing the crutcher sJurry formed in step ~aJ such that a uniform mixture or dispersion is formed having an aver7ge particle size of less than about 1. 0 micron and there~fter;
~cJ spray drying the aforesaid mixture or dispersion in a spray tower wherein the water content of the mixture is substantially evaporated to provide free-flowing particles of a softening composition capable of being readily dispersed jn water The invention is predicated on the discovery that a fabric softening composition can be prepared in particulate form by spr~y drying to provide a composition more highly concentr~ted than conventiona/ liquid rinse-cycle 2 ~
;ofteners. ~e resulting spr~y dried partic~es are dis,oersJ'~le in water and provjde effective softening to fabrics in a wash or r~'nse cycle aqueous bath. An essential feature of the composition of the invention is that uniform spray dried particles are formed by utilizing a mixjng step prior to spray drying the crutcher slurry such that the contents of the crutcher slurry are thoroughly dispersed and form a mixture or dispersion having an average particle size of below about 1. 0 micron, Uniform mixtures of this type may be achieved with various types of mixers, miJls or pumps known in the art, but it is preferred to use a so-called "homogenizer" such as a Gaulin Homogenizer marketed by Gaulin Corporation of Everett, Massachusetts, U. S.A. or Hilversum, Ho/land, which consists essential/y of a positive disp/acement pump to which is attached a homogenizing va/ve assembly capab/e of providing an intimate mixture having an average partic/e size diameter of be/ow about 1. 0 microns, and more preferably be/ow about 0. 7~; microns. The preferreg maximum size of partic/es in such mixture is be/ow about 5.0 microns and more preferably be/ow about 3. 0 microns.
DETAJLEf:) DESCfi~/PTlON Of J/JE JNVEN~/ON
The process of spray drying a softening composition in accordance with the invention uti/izes, for the most part, we// known technology reJating to the productjon of particu/ate detergent compositions. General/y, an a~ueovs crutcher slurry is formed containing a mixture of water with many or most of the ingredients desired in the fabric softening composition ~he soJids content of the s/urry is genera~/y from aoout 20% to about 70%, preferabJy 30% to 60%, and most preferab/y from 40% to 50~0 thereof, ~he ba/ance being water.

The crutcher s/urry is then atomjzed by pumping it an atomizing nozzle at a pressure of about 1000 to 2000 psi in~o a spray-drying tower, the typical dimensions of a commercial tower being about 35-100 feet in height and about 12-30 feet in diameter At the base of the tower, air is introduced at a temperature of from about 300-1000F which contacts the atomized s/urry to provide a hot drying gas for the drop/ets of the slurry thereby evaporating most of the water. Jhe resulting partic/es or beads are co//ected at the bottom of the tower, the moisture and heated air existjng at the top. Heat or water-sensjtive ngredients such as perfume may be post-added to the tower particles jn a subsequent mixjng or blending operation The crutcher slurry is preferably made by sequentjally adding the various components thereof in the manner which will result in the most miscjble and readily pumpable slurry for spray drying. Jhe order of addition of the various components may be varied, depending on the circumstances. Norma/ly, it is preferab/e for a// or a/most all of the water to be added to the crutcher first, preferably at about the processing temperature, after which the other components are added in sequence namely, urea, the quaternary ammonium sof~ening compound, anionic and/or nonionic surfactants, a fatty acid alkanolamides and optionally adjuvants, such as pigments, anti-oxidants and germicides.
The temperature of the aqueous medium in the crutcher wil/ usually be about room temperature or elevated, normally being in the 20 to 70C range, and preferably from about 25 to 40C.

62301~
Crutcher mixing times to obtain thoroughly mixed homogeneous s/urrles can Yary wide/y, from as littte as five minutes in sma/l crutchers and for slurr/es of higher moisture contents, to as much as one hovr, in some cases, although 30 minutes is a preferable upper /imit. Following mixing in the crutcher, the crutcher s/urry is transferred for further mixing to a "homogemzer" or s~milar mixer or pump to obtain the uniform dispersion or mixture described above having an average particle size of below about 1.0 micron.
Jhe resulting dispersion is thereafter transferred in the usual manner to a spray drying tower, which is located near the crutcher. Jhe dispersion is forced at high pressure through spray nozzles into the spray tower ~countercurrent or concurrentJ, wherein the drop/ets of the s/urry fa/l through a hot drying gas to form particles or beads of the fabric softening composition while evaporating substantially all the water The moisture content of the particles is preferably about 2 to 4%, by weight.
The cationic ~uaternary ammonium softening compounds useful for the invention include imidazolinium salts, di-long chain a/kyl quaternary ammonium sa/ts and diesterified long chain fatty acid di/ower alkyl ~uaternary ammonium salts. The general structure of the preferred imidazolinium salts is shown below r f l 1 N N R3 !
~f~ \~ j X

R

f~ ~

wherein:
P~ is a C8 to C30 a/iphatic radical and preferably a C,4 to C"~ alkyl or alkenyl;
R2 and R3 independently may be any of R, or preferably, /ower a/kyl or substituted alkyl of (~, to C4 such as haloaJkyl, hydroxya/kyl, acylaminoalkyl and the like;
X is a water-so/ubiljzing anion such as chloride, bromide, iodide, fluoride, sulfate, methosulfate, nitrite, nitrate, phosphate and carboxylate, le.g. acetate, adipate, phtha/ate, benzoate, o/eate, etc.);
Typical imidazo/inium softening compounds inc~ude:
2-heptadecy/- 1-methy/- 1-o/ey/amidoethy/ imidazo/inium ethosu/fate 2-heptadecyl- 1-methyl- J - /2-stearoylamidoJethyl - imidazolinium sulfate, 2-heptadecyl- 1-methyl- 1- /2-stearoylamidoJethyl - imidazolinium chloride, 2-coco- 1-12-hydroxyethyl~- 1-benzyl imidazolinium chloride, 2-coco- 1-~hydroxyethylJ- 1-(4-ch/orobutylJ imidazolinium chloride, 2-coco- 1-~2-hydroxyethyl)- 1-octadecenyl imidazolinium chloride, 2-tall oil fatty- 1-12-hydroxyethyl)- 1-benzyl imidazolinium ch/oride, 2-tal/ oil fatty- 1-~2 hydroxyethylJ- 1-~4-chtorobutylJ-imidazolinium chloride, 2-h~ptadecenyl- 1-12-hydroxyethyl)- 1-14-chlorobutylJ-imidazolinium chloride, 2-heptadecenyl- 1-12-hydroxyethyl) 1-benzyl imidazolinium chloride.
2-heptadecyl- 1-~hydroxyethylJ- 1-octadecylimjdazolinium ethyl sulfste.
The genera/ structure of the di-/ong chsin all~yl quaternary ammonium salts js shown below:

12J I /~ +
R N ! Y~
R

wherein the R groups are selected from C, to C30 aliphatic, preferably alkyl or alkenyl; aryl ~e,g. phenyl, toloyl, cumyl, etc.J; aralkyl ~e.g. benzyl, phenethyl, methylbenzyl, etc.J; and the halo, amide, hydroxyl, and carhoxy sustituents thereof such as halo C2 to C6 alkyl /e.g. 2-chloroethyl~; and hydroxy C2 to C6 alkyl ~e.g. 2-hydroxyethylJ; with the proviso that at least two R's are C~2 to C30 and preferably C~2 ~0 C22 and the others are lower alkyl; more preferably at least two R's are C~2 to C,O and the others are /ower alkyl of C, to C4 ~and most preferably methy/ or ethyll and Y is an anion as defined for X jn Formula ~1J.
Typical quaternary ammonium salts of formula ~2J include the following:
distearyl dimethyl ammonium chloride djtallow dimethyl ammonium chloride dihexadecyl dimethyl ammonium chloride dis~eary/ dimethyl ammonium bromide di~hydrogenated ta/low~ dimethyl ammonium bromide dJstearyl, dilisopropylJ ammonium chloride djstearyl dimethyl ammonium methosulfate.
di (hydro~qenated tallow~ dimethyl ammonium methosu/fate.
Another preferred class of the carjomc fabric softeners are diesterifjed long chajn fatty acid di/ower alkyl quaternary ammonium salts and diesterified c~

long cha~n fatty acid Jower alky1 Jower hydroxy alkyl quate~nary ammonium salts. This class of cationic fabric softeners can be represented by the generalformula:

1~ +

O
R3_ IV_ R40CR~ X

wherein RC0 represents the residue of a f~tty acid having from about 12 to 24 carbon atoms;
R2 and R3 represent independent/y a /ower a/ky/ group or a hydroxyall~yl group having 1 to 4 carbon atoms, and preferably 1 to 3 carbon atoms;
R4 represents a /ower aJky/ene group having 1 to 4 carbon atoms, preferably 1 to 3, and most preferably has 2 carbon atoms, i. e. R4 is -- CH2CH2 --; and X is a water-so/ubi/izing anion as defined above Such compounds are commercially avallable from, for instance, Stepan Chemica/ Co.
under the Stepantex trademar*, such as Stepantex VHR90 which has the formula:

CH3 V--CH2CH200CR.X

where RC0 is derived from tallow or coco fatty acids and X may be chJoride or su/fate.

The quaternary ammonium softening compound is generaJly from a~out 5 to 40%, by weight, of the partjculate softening composition, preferably from about 10 to 30%, and most preferably from about 15 ~o 25%, by weight.
An optional fabric softening ingredient is a fatty a/cohol wherein the hydrophobic group may be a straight or branched chain alky/ or alkenyl group having from about 10 to 24, preferably from abovt 10 to 20, especially preferably from about 12 to 20 carbon atoms. Specific examples of the fatty alcohol inc/ude decanol, dodecano/, tetradecanol, pentadecanol, hexadecanol, octadecano/, l~uryl alcohol, palmityl alcohol, stearyl alcohol, oleyl alcohol, and mixtvres thereof. Furthermore, the fatty alcohol may be of natural or synthetic origin and may include, for example, mixed a/cohol, such as C,6 to C,0 alcoho/s prepared by Zjegler polymerization of ethylene, The fatty alcohol may be present in the composition in a minor amount relative to the cationic fabric softener such ~hat the ratio, by weight, of the cationic fabric softener to fatty alcohol is in the range of from abovt 6:1 to 2:1, especial/y preferably about ~:1 to 3:1.
The fatty acid aJkano/amides useful in the present invention are those derived from fatty acid amides whose alkyl radical contains at least 12 carbon atoms. They preferably have the general formula:

R If_ N

O Cnfl2nOh' wherein n is 2 or 3. A preferred material is coco monoethanolamide.

2~ 8 ~ he concentration of fatty acid alkanolamide in the sof~ening composi~ion is genera//y from aoout 1 to 10%, ~y weight, and preferably from abovt 1 to 5%, by weight. The combination of fatty acid alkanolamide and quaternary ammonium softening compound in accordance with the invention provides a superior softening effect to fabrics.
An essential component of the fabric softening composition is urea. The particles general/y contain from about 45 to 85/6, by weight, of urea, preferably from about 55 to 7~%, and most preferably from ahout 60 to 70%, by weight.
Another important ingredient for purposes of improving particle solubility and dispersibility is an anionic and/or nonionic svrfactant. Among the anionic surface active agents useful in the present invention are those surface active compounds which contain an organic hydrophobic group contajning from about 8 to 26 carbon atoms and preferably from about 10 to 18 carbon atoms in their molecular structure and at /east one water-solubilizing group selected from the group of sulfonate, sulfate, carboxylate, phosphorate and phosphate so as to form a water-soluble detergent.
Examples of suitable anionic detergents include soaps, such as, the water-solubJe salts le.g., the sodium potassjum, ammonium and aJ~anol-ammonium salts~ of hlgher fatty acids or resin salts cont~ining from about 8 to 20 carbon atoms and preferably 10 to 18 carbon atoms Particularly useful are the sodium and potassium salts of the fatty acid mixtures derived fr~m coconut oil and tallow, for example, sodium coconut soap and pot~ssium tallow soap.
The anionic c~ass of detergents also includes the water-soluble sulfated and sulfonated detergents having an aliphatic, preferably an aJkyl radical containjng from a~out 8 to 26, and preferab/y from abovt J2 ro 2~ carbon atoms. Examples of the suffonated anionic detergents are the higher alky/
aromatic sulfonates such as the higher alkyl benzene sulfonates containing from about 10 to 16 carbon atoms in the higher alkyl group in a straight or branched chain, such as, for examp/e, the sodium, potassiurn and ammonium salts of higher aJkyl benzene sulfonates, higher alkyl toluene sulfonates and higher alkyl phenol sulfonates, Other suitable anionic detergents are the olefin sulfonates including long chain alkene sulfonates, long chain hydroxyalkane sulfonates or mixtures of alkene sulfonates and hydroxyalkane sulfonates and hydroxyalkane sulfonates.
Other suitable anionic detergents are su/fated ethoxylated higher fatty alcohols of the formula RO~C~t40J,r,SO3M, wherein R is a fatty alkyl of from 10 to 18 carbon atoms, m is from 2 to 6 ~preferably having a value from about 1/5 to 1/2 the number of carbon atoms in RJ and M is a solubilizing salt-forming cation, such as an alkali me~a/, ammonium, /ower a/kylamino or lower alkanolamino, or a higher alkyl benzene sulfonate wherein the higher alkyl is of 10 to 15 carbon atoms. The propor~ion of ethylene oxide in the polyethoxylated higher alkanol su/fate is preferably 2 to 5 moles of ethylene oxide groups per moJe of anionic detergent, with three moles being most preferred, especia/ly when the higher alkanol is of 11 to 15 carbon atoms. A
preferred polyethoxylated aJcohoJ sulfate detergent is marketed by SheJJ
ChemicaJ Company as Neodol 25-3S.
The most highly preferred water-soluble anionic detergent compounds are the ammonium and substituted ammonium ~such as mono, di and tri-3~ ~ethanolamineJ, al~:aii metal ~such as, sodium and potassiumJ and alka/ine earth meta/ fsuch as, ca/cium and magnesium~ sa/~s of the higher alky/ benzene su/fonares, o/efine su/fonates and higher a/ky/ su/fates. Among the above-listed anionics, the most preferred are the sodium linear a/kyl benzene svlfonates /La~S), and especia//y those wnerein the a/ky/group is a straight chain a/ky/
radica/ of 12 or 13 carbon atoms.
Among the suitab/e nonionic surfactants are ~he ethoxy/ated fatty a/coho/s having from 12 to 20 carbon atoms, and an average degrees of ethoxy/ation of 3 to 9. Preferred nonionic detergents are coconut a/coho/s having an average of 6 or 7 ethyoxy groups per mo/ecu/e and C,4-C,6 primari/y a/coho/s with 6 or 7 ethoxy groups per mo/e of higher fatty a/coho/.
Ethoxy/ated /aury/ a/coho/ having about 7 mo/es of ethoxy/ate per mo/e of a/coho/ is particularly preferred for use herejn.
Other usefu/ nonionic detergent compounds inc/ude the a/ky/po/yg/ycosjde and a/kylpo/ysaccharide surfactants which are weJ/ known in the art.
Jhe amount of anionic surfactant in the particulate composition may vary from O to 3%, and preferably will vary with the percentage of cationic softening compound as fol/ows: from about 1 to 4% of anionic surfactant when the percentage of c~tionic compound is be/ow about 20%, and from about 3 to 3%
of anionic svrfactant when the percentage of cationic softening compound is from about 20 to 40%, a/J percentages being by weight of the particuJate composition. Genera/ly, the leve/ of anion;c surfactant is from about 2 to 4 %, by weight. The nonionjc surfactant is optiona//y present from about 0.5 to 5%, by weight, and preferab/y no more than about J %, by weight.

~8~t~
The fabric softening compositions of the invention may further jnclude additional or supp/emental ingredients whjch do not adversely affect the sta~ility or functiona/ characteristics of the softening composition. Included among such supplemental ingredients are perfumes, dyes, pigments, germicjdes, soi/-release agents, f~bric crisping agents, anti-oxidants and anti-corrosion agents.

2 ~

EXAMPLE J
A granular fabric softening composition of the invention had the fo/lowing composition:

ComDonent Weiqht Percent DSDMAC' 24 Nonionic SurfactantZ 2 Sodium Dodecy/ Benzene Sulfonate 3 Cocomonoethanol Amide 3 Urea 64 Moisture Balance _ 'D;steary/ dimethyl ammonium chloride 2Ethoxylated lauryl alcohol having about 7 moles of ethoxylate per mo/e of alcohol.
Ten and one-half r10,5J grams of the above-described softening composition was added to a top-loaded washing machine in the rinse cyc/e at a water temperature of 25C and at water hardness of 100 and 320 ppm. The dispersibjlity tjme ~f the granular product jn the water was about 1.5 minutes, The softness and hydrophilicity of the resulting fabrics was measured and compared with the measured softness for fabrics conditioned in the same top loading machine with forty two ~42J grams of a commercial liquid fabric softener containing 6% of a quaternary ammonium softener. The fabrics conditioned with the granular softening composition of the invention were measurably softer and equal in hydrophilic properties to those conditioned with the commercial liquid product.

?7

Claims (7)

1. A process of producing a free-flowing spray-dried particulate fabric softening composition which is readily dispersible in water comprising:
(a) forming a crutcher slurry containing:
(i) from about 5 to 40%, by weight, of a cationic quaternary ammonium softening compound;
(ii) from about 0.5 to 15%, by weight, of an anionic and/or a ncnionic detergent compound;
(iii) from about 45 to 85%, by weight, of urea, the above percentages being based on the solids content of the slurry in the absence of water;
(b) mixing the crutcher slurry formed in (a) to provide a uniform mixture or dispersion having an average particle size of less than about 1. 0 micron and thereafter;
(c) spray drying the aforesaid mixture or dispersion in a spray tower wherein the water content of the mixture is substantially evaporated to provide free-flowing particles of a softening composition capable of being readily dispersed in water
2. A process according to claim 1 wherein the crutcher slurry further contains from about 1 to 10% of a fatty acid alkanolamide
3. A process according to claim 1 wherein the alkanolamide is cocomonoethanol amide.
4. A process according to claim 1 wherein the crutcher slurry contains from about 1 to 8% of an anionic detergent compound and from about 10 to 40% of a cationic softening agent, the above percentages being based on the solids content of the slurry,
5. A process according to claim 1 wherein the crutcher slurry contains up to about 2%, by weight, of 3 nonionic detergent compound.
6. A process according to claim 1 wherein the amount of anionic detergent in the crutcher slurry varies with the percent of cationic compound as follows: from about 1 to 4% of anionic detergent when the percent of cationic softening compound is below about 20%, and from about 3 to 8% of anionic detergent when the percent of cationic softening compound is from about 20 to 40%.
7. A process according to claim 1 wherein the cationic softening compound is distearyl dimethyl ammonium chloride.
CA002085618A 1991-12-18 1992-12-17 Free-flowing powder fabric softening composition and process for its manufacture Abandoned CA2085618A1 (en)

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US80966091A 1991-12-18 1991-12-18
US7/809,660 1991-12-18
US7/838,626 1992-02-19
US07/838,626 US5368755A (en) 1991-12-18 1992-02-19 Free-flowing powder fabric softening composition and process for the manufacture of a free-flowing fabric softening composition

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EP0659207B1 (en) * 1992-09-11 1999-03-24 Henkel Kommanditgesellschaft auf Aktien Use of detergent mixtures
DE4326975A1 (en) * 1993-08-11 1995-02-16 Henkel Kgaa Process for the preparation of anhydrous nitrogenous compounds
DE69424551T3 (en) * 1994-12-02 2005-12-29 The Procter & Gamble Company, Cincinnati Cationic surfactant containing detergent compositions and their preparation
DE19721885A1 (en) 1997-05-26 1998-12-03 Henkel Kgaa Process for the production of granules containing cationic surfactants
US6502325B1 (en) * 1999-09-02 2003-01-07 Colgate-Palmolive Co. Method of treating fabric with fabric care composition containing polycarboxylate polymer and compound derived from urea
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DE2454465A1 (en) * 1974-11-16 1976-05-20 Hoechst Ag Powdery germ inhibiting soft rinsing compsns for textiles - contg cationic soft rinse, cationic disinfectant, urea and non ionic dispersant
JPS60398B2 (en) * 1978-06-08 1985-01-08 ライオン株式会社 Manufacturing method of detergent slurry
DE2918364A1 (en) * 1979-05-07 1980-11-20 Henkel Kgaa DETERGENT FOR TEXTILES
US5259964A (en) * 1991-12-18 1993-11-09 Colgate-Palmolive Co. Free-flowing powder fabric softening composition and process for its manufacture

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HU9203998D0 (en) 1993-03-29
CZ367592A3 (en) 1993-09-15
TR26894A (en) 1994-08-22
GR920100560A (en) 1993-08-31
NO924891D0 (en) 1992-12-17
FI925743A0 (en) 1992-12-17
HUT63473A (en) 1993-08-30
NO924891L (en) 1993-06-21
PT101133A (en) 1994-03-31
CN1075759A (en) 1993-09-01
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AU662780B2 (en) 1995-09-14

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