Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/50—Perfumes
• • 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
  • C11D1/66—Non-ionic compounds
  • C11D1/835—Mixtures of non-ionic with cationic compounds
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/0005—Other compounding ingredients characterised by their effect
  • C11D3/001—Softening compositions
  • C11D3/0015—Softening compositions liquid
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/667—Neutral esters, e.g. sorbitan esters
• • 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
  • C11D1/66—Non-ionic compounds
  • C11D1/72—Ethers of polyoxyalkylene glycols
• • 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
  • C11D1/66—Non-ionic compounds
  • C11D1/74—Carboxylates or sulfonates esters of polyoxyalkylene glycols

Definitions

• the subject invention relates to aqueous-based fabric softener compositions having relatively high levels of perfume and low levels of cationic softener active, the compositions being intended for use in the rinse cycle of laundry washing processes.
• the subject invention also involves concentrates of such compositions, and processes for making such compositions and concentrates.
• Fabric softening or conditioning compositions intended for use in the rinse cycle of the laundering process, generally are aqueous dispersions containing a cationic softener as the active material.
• a cationic softener is typically compounds with a positively charged nitrogen atom and at least one hydrophobic long-chain substituent in the molecule.
• Suitable cationic softeners are mostly quaternary ammonium salts and imidazolinium salts, and to a lesser extent, alkylated partly elthoxylated polyamines, amine amides, ester amines, and di-quatemary compounds.
• Fabric softening or conditioning compositions for use in household washing machines during the rinse cycle are marketed extensively. They provide a countering influence on the disorder of the pile of the fibers at the textile surface as well as an electrostatic charge on it by adsorbing on the textile substrate. Such treatment imparts fluffiness to the fabric, and gives a more pleasant sensation when the fabrics are worn next to the skin.
• the cationic softeners present in these compositions also serve as carriers for perfume, imparting long-lasting freshness to the laundered fabrics.
• compositions and concentrates which are stable over long periods of time; the compositions and concentrates maintain their desired viscosity and do not separate into discrete hydrophilic and hydrophobic phases.
• the subject invention involves single strength liquid fabric softener compositions for use in the rinse cycle of a laundering process, the composition comprising:
• compositions consist of a liquid aqueous phase with discrete hydrophobic particles dispersed substantially uniformly therein.
• the compositions preferably have a viscosity of from about 50 cp to about 500 cp.
• the subject invention also involves concentrates of such single strength compositions, the concentrates comprising an amount of cationic softener plus nonionic surfactant of up to about 30%, and up to about 10% hydrophobic perfume.
• the subject invention also involves processes for making such compositions and concentrates.
• compositions include, at a minimum, a cationic fabric softener, a hydrophobic perfume, a nonionic surfactant, and water. All percentages disclosed herein are weight percent unless otherwise indicated.
• the subject invention involves single strength fabric softener compositions.
• single strength refers to compositions which are intended for addition to the rinse cycle of the laundering process as is.
• the subject invention also involves concentrates of such single strength compositions, the concentrates preferably being diluted with water prior to addition to the rinse cycle. Optionally, such concentrates can be added directly to the rinse water, in which case the recommended usage amount would be correspondingly altered.
• Typical concentrates are 2x, 3x, 5x and 10x (1x being single strength), which are then diluted at the time of use or the amount used is correspondingly reduced.
• compositions are in the form of a liquid aqueous phase with discrete hydrophobic particles dispersed substantially uniformly throughout the aqueous phase.
• the hydrophobic particles are believed to comprise the perfume surrounded by the cationic softener and nonionic surfactant.
• the size distribution of the particles is determined using known methods, such as by use of a Microtrac® SRA100 particle size analyzer from Leeds & Northrap Corp. Such methods generally provide a volume percent result which, for particles such as those in the subject invention compositions with a substantially uniform weight distribution, is substantially equivalent to weight percent.
• the diameter of the hydrophobic particles of the subject compositions generally approximates a normal distribution. It has been found that compositions having a large percentage of particles which are either too big (diameter of more than about 50 microns) or too small (diameter of less than 1 or 2 microns) are unstable.
• the mean diameter of the particles is preferably from about 3 microns to about 15 microns, more preferably from about 4 microns to about 12 microns, more preferably still from about 5 microns to about 9 microns, also preferably from about 4 microns to about 6 microns; 90% of the particles have a diameter preferably less than about 50 microns, more preferably less than about 30 microns, more preferably still less than about 20 microns, still more preferably less than about 12 microns; and 90% of the particles have a diameter preferably greater than about 1 micron, more preferably greater than about 2 microns, more preferably still greater than about 3 microns.
• compositions have a lower ratio of cationic softener to perfume than is typically found in commercial products. It has been found that compositions with such lower ratio are typically unstable; they have a tendency to separate into discrete hydrophobic and hydrophilic phases or layers, the hydrophobic layer comprising much of the perfume.
• the subject invention compositions are formulated to avoid such phase separation problems.
• compositions and concentrates of the subject invention having a low viscosity of as low as 10 cp, or even 5 cp, can be produced. However, compositions of higher viscosity are preferred for aesthetic reasons.
• the fabric softening compositions and concentrates of the subject invention preferably have a viscosity of from about 50 cp to about 500 cp, more preferably from about 80 cp to about 300 cp, more preferably still from about 100 cp to about 200 cp.
• Such higher viscosity compositions present additional challenges to achieving stable compositions and concentrates.
• alkyl means hydrocarbon chain which may be straight or branched, substituted or unsubstituted, and saturated or unsaturated with one or more double bonds.
• alkanyl means saturated alkyl
• alkenyl means alkyl with one or more double bonds.
• alkyl is preferably as follows. Preferred alkyl is straight chain. Preferred alkyl is unsubstituted. Alkyl having less than 8 carbon atoms is preferably saturated. Alkyl having 8 or more carbon atoms is preferably saturated or unsaturated with one or two double bonds.
• Cationic fabric softeners useful in the subject invention compositions include compounds having a quaternary nitrogen and at least 1 hydrophobic hydrocarbon moiety. Examples of such compounds include quaternary ammonium compounds and compounds containing a nitrogen present in a cyclic ammonium moiety.
• the cationics softeners which are useful herein include the entire class of quaternary ammonium compounds which comprise at least one alkyl moiety having from about 12 to about 30 carbon atoms. Such compounds are, only in part, be represented by the following general formula: wherein R comprises an alkyl having from about 11 to about 30, preferably from about 12 to about 22, more preferably from about 13 to about 18, carbon atoms. Each R" is independently R or R'; preferably one R" is R and the other is R'. When there are 2 or 3 R groups, one such R group can be arylalkanyl, preferably phenylalkanyl, the alkanyl having from 1 to about 8, preferably from 1 to about 3, more preferably 1 , carbon atoms.
• R' may be lower alkanyl, from about C-j to about C4.
• each R' is independently unsubstituted alkanyl or hydroxyalkanyl, such as methyl, ethyl, propyl, or hydroxyethyl.
• Two of the R' groups may, together with the nitrogen and/or one or more other heteroatoms (preferably nitrogen), form a 5- or 6-membered heteroaryl or heterocyclic ring, such as imidazolyl, tetrazolyl, pyridyl, pyrrolyl, pyrazolyl, pyrazinyl, pyrimidinyl, pyridazinyl, or saturated analog thereof.
• X a_ is any softener composition compatible anion, e.g. halo (preferably chloride or bromide), sulfate, methylsulfate, ethyisulfate, nitrate, acetate, phosphate, benzoate, formate, lactate, oleate, and the like.
• the symbol "a” represents the ionic valance of the anion and also, therefore, the number of quaternary cationic moieties in association therewith.
• the anion is merely present as a counterion of the positively charged quaternary ammonium compounds.
• Preferred anions are chloride and methylsulfate.
• Long chain alkyl moieties having from about 12 to about 30 carbon atoms which are depicted by various "R" and "T symbols herein can represent a single alkyl moiety or a mixture of different alkyl moieties.
• Mixtures of such alkyl moieties, in the form of fatty acids or fatty alcohols, are readily and inexpensively obtained from various natural fat and oil sources, such as tallow, lard, coconut oil, soybean oil, palm stearin oil, palm kernel oil, etc. Mixtures of such alkyl chains are referred to herein by referring to such sources. All the fatty moieties from such a source can be used, or only part (or a "cut"), of fatty moieties having the chain length and degree of saturation desired.
• Alkyl moieties obtained from tallow are particularly preferred for many of the quaternary ammonium compounds useful in the subject invention, because of their preferred chain length distribution.
• the term "tallow”, as used herein, means glycerides or fatty or alkyl derivatives therefrom, where the fatty acid mixtures typically have an approximate carbon chain length distribution of about 2-4% myristic, 25-35% palmitic, 20-25% stearic, 1-3% palmitoleic, 35-45% oleic, and 2-4% linoleic.
• Other sources with similar fatty acid distributions such as the fatty acids derived from palm stearin oil and from various animal tallows and lard, are also included within the term tallow.
• the tallow can also be hardened (i.e., hydrogenated) to convert part or all of the unsaturated fatty acid or alkyl moieties to saturated fatty acid or alkyl moieties.
• Preferred single alkyl long chain moieties in the subject cationic softeners include stearyl, oleyl, palmityl, palmitoleyl, myristyl, and lauryl.
• Preferred cationic softeners have two or more, preferably two, long- chain alkyl groups having from about 12 to about 24 carbon atoms or one said group and an arylalkyl group.
• compositions include acyclic quaternary ammonium salts have the formula:
• each T is independently about C12-C24. preferably about C14-C18. alkyl; alternatively, one T may be arylalkyl, preferably phenylalkyl, the alkyl portion preferably being about C1-C4 alkanyl, the phenylalkyl most preferably being benzyl;
• T is about C1-C4, preferably C-j or C2, alkanyl or hydroxyalkanyl, preferably alkanyl;
• T" is T or T, preferably T;
• X a_ is an anion as defined above.
• softeners are the well-known dialkyldimethylammonium salts, such as ditallowdimethylammonium chloride, ditallowdimethylammonium methylsulfate, di(hydrogenatedtallow)- dimethylammonium chloride, dihexadecyldiethylammonium chloride, distearyldimethylammonium chloride, dibehenyldimethylammonium chloride, di(coconut alkyl)dimethylammonium chloride. Di(hydrogenatedtallow)- dimethylammonium chloride and ditallowdimethylammonium chloride are preferred.
• dialkyldimethyl-ammonium salts examples include di(hydrogenatedtallow)dimethylammonium chloride (trade name Adogen® 442), ditallowdimethylammonium chloride (trade name Adogen® 470), distearyldimethylammonium chloride (trade name Arosurf® TA-100), all available from Witco Chemical Company.
• Dibehenyldimethylammonium chloride is sold under the trade name Kemamine® Q-2802C by Humko Chemical Division of Witco Chemical Co ⁇ oration.
• Dimethylstearylbenzyl ammonium chloride is sold under the trade names Varisoft® SDC by Witco Chemical Company and Ammonyx® 490 by Onyx Chemical Company.
• Cationic softeners useful in the subject invention compositions also include quaternary ammonium compounds having the Formula (III) or (IV), below:
• Rl is -(CH 2 ) n -Q-T 1 or T2;
• R2 is -(CH 2 )n-Q-T 1 or ⁇ 2 or R 3 ; each R 3 is independently about C1-C4 alkanyl or about C1-C4 hydroxyalkanyl, or H; preferably Ci or C2 alkanyl or hydroxyalkanyl, preferably alkanyl; each Q is selected from -O-C(O)-, -C(O)-O-, -O-C(O)-O-, -NR -C(O)-, and -C(O)-NR 4 -; preferably from -O-C(O)- and -C(O)-O-;
• R 4 is H or about C1-C4 alkanyl or about C1-C4 hydroxyalkanyl, preferably H; each T 1 is independently (the same or different) about C-
• Ci ⁇ each n is an integer from 1 to about 4, preferably 2; and ⁇ a ⁇ is a softener-compatible anion, as described hereinabove.
• quaternary ammonium compounds suitable for use in the subject compositions herein include:
• compounds 1-7 are examples of compounds of Formula (III); compound 8 is a compound of Formula (IV).
• N,N-di(tallowoyl-oxy-ethyl)-N,N-dimethyl- ammonium chloride where the tallow chains are at least partially unsaturated.
• the level of unsaturation of the tallow chain can be measured by the Iodine Value of the corresponding fatty acids, which is preferably from 5 to 100 with two categories of compounds being distinguished, having an Iodine Value below or above 25.
• Iodine Value of the corresponding fatty acids which is preferably from 5 to 100 with two categories of compounds being distinguished, having an Iodine Value below or above 25.
• a cis/trans isomer weight ratio be greater than about 30/70, preferably greater than about 50/50 and more preferably greater than about 70/30.
• the ratio of cis to trans isomers is less critical.
• Suitable quaternary ammoniums for Formula (III) and (IV) are obtained by, e.g., replacing "tallow” in the above compounds with, for example, coco, palm, lauryl, oleyl, ricinoleyl, stearyl, palmityl, or the like, said fatty acyl chains being either fully saturated, or preferably at least partly unsaturated; replacing "methyl” in the above compounds with ethyl, ethoxy, propyl, propoxy, isopropyl, butyl, isobutyl or t-butyl; replacing "chloride” in the above compounds with bromide, methylsulfate, formate, sulfate, nitrate, and the like.
• each T ⁇ is independently about C13-C21 alkyl, preferably about C15-
• R 3 and R 4 are each independently about C1-C4 alkanyl or hydroxyalkanyl, preferably C-J-C2; or, differing from general Formula (III), R 4 is -(CyH2yO) m H, wherein m is an integer from 1 to about 5, y is 2 or 3; and
• X a - is an anion as described hereinabove.
• Preferred examples of such softeners are those where n is 2, R 3 is methyl, R 4 is two or three ethoxy or propoxy groups, and T 1 C(O) is stearyl, oleyl, palmityl, palmitoleyl, tallowyl, or hydrogenated tallowyl.
• softeners are methylbis(tallowamidoethyl)(2- hydroxyethyl)ammonium methylsulfate and methylbis(hydrogenated tallowamidoethyl)(2-hydroxyethyl)ammonium methylsulfate; these materials are available from Witco Chemical Company under the trade names Varisoft® 222 and Varisoft® 110, respectively.
• ester quaternary ammonium compounds useful in the subject invention also largely a subset of Formula (III), have the formula:
• -C3, alkanyl or hydroxyalkanyl or a benzyl, preferably alkanyl or hydroxyalkanyl, e.g., methyl (most preferred), ethyl, propyl, hydroxyethyl, and the like; each R6 is independently a long chain, about C10-C23.
• alkyl preferably about C13-C19 alkyl, most preferably about C15-C17 straight chain alkyl; and the counterion X a ⁇ is as defined above.
• softeners wherein all long-chain alkyl substituents are straight-chain
• softeners include the following:
• DEQA compounds are somewhat labile to hydrolysis, they should be handled rather carefully when used to formulate the compositions herein.
• stable liquid compositions herein are formulated at a pH in the range of about 2 to about 5, preferably from about 2 to about 4.5, more preferably from about 2 to about 4.
• the pH can be adjusted by the addition of a Bronsted acid.
• DEQA softeners and methods for making them are disclosed in PCT Patent Application No. WO94/20597 (U.S. Priority Application Serial Nos. 08/024,541 and 08/142,739), which are incorporated herein by reference.
• Quaternary imidazolinium compounds useful as cationic softeners in the subject invention compositions include those having the formula:
• Z is NR 9 or O; R 9 being H or R 7 , preferably H;
• R 7 is about C1-C4 alkanyl, preferably methyl or ethyl; each R8 is independently about C9-C25, preferably about Ci 1-C19, more preferably about C13-C17 alkyl, preferably alkanyl;
• X a_ is an anion as defined above.
• cationic softeners useful in the subject invention include 1-methyl-1-(tallowylamido)ethyl-2-tallowyl-4,5-dihydroimidazolinium methylsulfate and 1 -methyl-1 -(hydrogenated tallowylamido)ethyl-2- (hydrogenatedtallowyl)-4,5-dihydroimidazolinium methylsulfate, sold under the trade names Varisoft® 475 and Varisoft® 445, respectively, by Witco Chemical Company; 1 -methyl-1 -(palmitqylamido)ethyl-2-octadecyl-4, 5- dihydroimidazolinium chloride.
• the cationic softener of the subject invention can also comprise a carboxylic acid salt of a tertiary amine and/or ester amine having the formula: R11 -R 13 (VIIO
• R ' O is a long chain aliphatic group containing from about 8 to about 30 carbon atoms; each R 1 1 and R12 are selected from the group consisting of an alkyl group containing from about 1 to about 30 carbon atoms, a hydroxyalkyl group of the formula: R 14 OH wherein R 14 is an alkylene group of from about 2 to about 30 carbon atoms, and alkyl ether groups of the formula: R 15 O(C s H2sO) r wherein R 15 is alkanyl or alkenyl group having from about 1 to about 30 carbon atoms or H, s is an integer from 1 to about 5, preferably 2 or 3, and r is an integer from about 1 to about 30; wherein R 10 , R 1 1 , R 12 , R 14 and R 15 can be ester interrupted groups; and wherein R 13 is selected from unsubstituted alkanyl, alkenyl, aryl, alkaryl and aralkyl groups having from about 8 to about 30 carbon
• R 10 is alkyl containing from about 12 to about 22 carbon atoms
• R ⁇ 2 is alkyl of from about 1 to about 22 carbon atoms
• R1° is alkyl of from about 1 to about 22 carbon atoms.
• Particularly preferred tertiary amines for static control performance are those containing unsaturation; e.g., oleyldimethylamine and/or soft tallowdimethylamine.
• Preferred amine salts are those wherein the amine moiety is a C-
• the amine and the acid, respectively, used to form the amine salt will often be of mixed chain lengths rather than single chain lengths, since these materials are normally derived from natural fats and oils, or synthetic processes which produce a mixture of chain lengths. Also, it is often desirable to utilize mixtures of different chain lengths in order to modify the physical or performance characteristics of the cationic softener.
• amine salts can be formed by a simple addition reaction, well known in the art, disclosed in U.S. Patent No. 4,237,155, Kardouche, issued December 2, 1980, which is incorporated herein by reference.
• the amine salts preferably have a thermal softening point of from about 35°C to about 100°C.
• Examples of preferred tertiary amines as starting material for the reaction between the amine and carboxylic acid to form the tertiary amine salts are: lauryldimethylamine, myristyldimethylamine, stearyldimethylamine, tallowdimethylamine, coconutdimethylamine, dilaurylmethylamine, distearylmethylamine, ditallowmethylamine, oleyldimethylamine, dioleylmethylamine, lauryldi(3-hydroxypropyl)amine, stearyldi(2-hydroxyethyl)amine, trilaurylamine, laurylethylmethylamine, and
• Preferred fatty acids are those wherein R 13 is a long chain, unsubstituted alkanyl or alkenyl group of from about 8 to about 30 carbon atoms, more preferably from about 11 to about 17 carbon atoms.
• Examples of specific carboxylic acids as a starting material are: formic acid, acetic acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, oxalic acid, adipic acid, 12-hydroxy stearic acid, benzoic acid, 4- hydroxy benzoic acid, 3-chloro benzoic acid, 4-nitro benzoic acid, 4-ethyl benzoic acid, 4-(2-chloroethyl)benzoic acid, phenylacetic acid, (4- chlorophenyl)acetic acid, (4-hydroxyphenyl)acetic acid, and phthalic acid.
• Preferred carboxylic acids are stearic, oleic, lauric, myristic, palmitic, and mixtures thereof.
• Specific preferred amine salts for use in the subject invention are oleyldimethylamine stearate, stearyldimethylamine stearate, stearyldimethylamine myristate, stearyldimethylamine oleate, stearyldimethylamine palmitate, distearylmethylamine palmitate, distearylmethylamine laurate, tallowyldimethylamine stearate, and mixtures thereof.
• a particularly preferred mixture is oleyldimethylamine stearate and distearylmethylamine myristate, in a ratio of 1 :10 to 10:1 , preferably about 1:1.
• Preferred cationic softeners useful in the subject invention compositions include the following:
• DTDMAC ditallow dimethylammonium chloride
• DSOEDMAC di(stearoyloxyethyl) dimethylammonium chloride
• Particularly preferred cationic softeners for the subject invention compositions include ditallow dimethylammonium chloride, di(stearyloxyethyl) dimethylammonium chloride, di(tallowyloxyethyl) dimethylammonium chloride.
• the single strength fabric softening compositions of the subject invention comprise from about 0.4% to about 5% cationic fabric softener, preferably from about 0.5% to about 4%, more preferably from about 0.8% to about 3%, more preferably still from about 1% to about 2%.
• the concentrates of such compositions comprise from about 0.8% to about 24% cationic fabric softener, preferably from about 2% to about 15%, also preferably still from about 3% to about 10%.
• hydrophobic perfume or “perfume” is used in its ordinary sense to refer to and include any essentially water insoluble (or very sparingly water soluble) fragrant substance or mixture of substances including natural (i.e., obtained by extraction of flowers, herbs, leaves, roots, barks, wood, blossoms or plants), artificial (i.e., a mixture of different nature oils or oil constituents) and synthetic (i.e., synthetically produced) odoriferous substances. Such materials are often accompanied by auxiliary materials, such as fixatives, extenders, stabilizers and solvents. These auxiliaries are also included within the meaning of "perfume", as used herein. Typically, perfumes are complex mixtures of a plurality of organic compounds. The formulator has the luxury of choosing from a wide variety of perfume ingredients in order to arrive at a desired perfume formulation.
• perfume ingredients useful in the perfumes of the subject invention compositions include, but are not limited to, hexyl cinnamic aldehyde; amyl cinnamic aldehyde; amyl salicylate; hexyl salicylate; terpineol; 3,7-dimethyl-cis-2,6-octadien-1-ol; 2,6-dimethyl-2-octanol; 2,6- dimethyl-7-octen-2-ol; 3,7-dimethyl-3-octanol; 3,7-dimethyl-trans-2,6- octadien-1-ol; 3,7-dimethyl-6-octen-1-ol; 3, 7-dimethyl-1 -octanol; 2-methyl-3- (para-tert-butylphenyl)-propionaldehyde; 4-(4-hydroxy-4-methylpentyl)-3- cyclohexene-1 -carbox
• fragrance materials of synthetic or natural origin which may be included in the perfume, if desired, include, but are not limited to, orange oil; lemon oil; grapefruit oil; bergamot oil; clove oil; dodecalactone gamma; methyl-2-(2-pentyl-3-oxo-cyclopentyl) acetate; beta-naphthol methylether; methyl-beta-naphthylketone; coumarin; decy (aldehyde; benzaldehyde; 4- tert-butylcyclohexyl acetate; alpha, alpha-dimethylphenethyl acetate; methylphenylcarbinyl acetate; Schiff s base of 4-(4-hydroxy-4-methylpentyl)- 3-cyclohexene-1 -carboxaldehyde and methyl anthranilate; cyclic ethyleneglycol diester of tridecandioic acid; 3,7-dimethyl-2
• perfume components are geraniol; geranyl acetate; linalool; linalyl acetate; tetrahydrolinalool; citronellol; citronellyl acetate; dihydromyrcenol; dihydromyrcenyl acetate; tetrahydromyrcenol; terpinyl acetate; nopol; nopyl acetate; 2-phenylethanol; 2-phenylethyl acetate; benzyl alcohol; benzyl acetate; benzyl salicylate; benzyl benzoate; styrallyl acetate; dimethylbenzylcarbinol; trichloromethylphenylcarbinyl methylphenylcarbinyl acetate; isononyl acetate; vetiveryl acetate; vetiverol; 2-methyl-3-(p-tert-butylphenyl)-propanal, 2-methyl-3-(
• the perfumes useful in the subject invention compositions are substantially free of halogenated materials and nitromusks.
• Suitable solvents, diluents or carriers for perfumes ingredients mentioned above are for examples, ethanol, isopropanol, diethylene glycol, monoethyl ether, dipropylene glycol, diethyl phthalate, triethyl citrate, etc.
• the amount of such solvents, diluents or carriers inco ⁇ orated in the perfumes is preferably kept to the minimum needed to provide a homogeneous perfume solution.
• Perfumes useful herein and the subject invention compositions are preferably substantially free of, more preferably free of, the solvent butyl carbitol.
• the single strength fabric softening compositions of the subject invention comprise from about 0.3% to about 1.2% hydrophobic perfume, preferably from about 0.4% to about 1%, more preferably from about 0.5% to about 0.8%.
• the concentrates of such compositions comprise from about 0.6% to about 10% hydrophobic perfume, preferably from about 1% to about 8%, also preferably from about 2% to about 5%.
• the ratio of cationic softener to perfume is from about 1:3 to about 5:1 , preferably from about 1 :2 to about 4:1 , more preferably from about 1:1 to about 3:1 , also preferably from about 1.5:1 to about 2.5:1.
• Nonionic Surfactant is from about 1:3 to about 5:1 , preferably from about 1 :2 to about 4:1 , more preferably from about 1:1 to about 3:1 , also preferably from about 1.5:1 to about 2.5:1.
• the nonionic surfactants which are useful in the subject invention compositions comprise a polar moiety and a hydrophobic moiety.
• the hydrophobic moiety is preferably at least 1 alkyl group having from about 8 to about 22, more preferably from about 12 to about 18, also preferably from about 11 to about 15, carbon atoms.
• the alkyl chain is preferably from about 10 to about 14 carbon atoms.
• Examples of polar moieties in such nonionic surfactants include alcohol, ethoxy, polyethoxy, ester, and amide.
• nonionic surfactants are compounds produced by the condensation of alkylene oxide groups, preferably ethylene oxide, (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkylaromatic in nature.
• alkylene oxide groups preferably ethylene oxide
• organic hydrophobic compound which may be aliphatic or alkylaromatic in nature.
• the length of the polyoxyalkylene group which is condensed with any particular hydrophobic group can be readily adjusted to yield a water-soluble compound having the desired balance between hydrophilic and hydrophobic.
• Preferred nonionic surfactants useful in the subject invention compositions are selected to achieve the desired viscosity, as well as stability, for the compositions.
• the nonionic surfactants useful in the subject invention compositions preferably have a HLB (hydrophilic/lipophyllic balance) of from about 6 to about 20, more preferably from about 8 to about 15.
• the preferred nonionic surfactants have a melting point above about 20°C, more preferably from about 25°C to about 65°C.
• Classes of useful nonionic surfactants include the following:
• the polyethylene oxide condensates of alkyl phenols. These compounds include the condensation products of alkyl phenols having an alkyl group containing from about 6 to about 12 carbon atoms in either a straight chain or branched chain configuration with ethylene oxide, the ethylene oxide being present in an amount equal to from about 5 to about 25 moles of ethylene oxide per mole of alkyl phenol.
• Examples of compounds of this type include nonyl phenol condensed with about 9.5 moles of ethylene oxide per mole of phenol; dodecyl phenol condensed with about 12 moles of ethylene oxide per mole of phenol; dinonyl phenol condensed with about 15 moles of ethylene oxide per mole of phenol; and diisooctyl phenol condensed with about 15 moles of ethylene oxide per mole of phenol.
• Commercially available nonionic surfactants of this type include Igepal® CO-630, marketed by the GAF Corporation; and Triton® X-45, X-114, X-100, and X-102, all marketed by the Rohm & Haas Company.
• the alkyl chain of the aliphatic alcohol can either be straight or branched, primary or secondary, and generally contains from about 8 to about 22, preferably from about 10 to about 18, more preferably from about 11 to about 15 carbon atoms.
• Ethoxylated fatty alcohols preferably have from about 4 to about 60, more preferably from about 5 to about 30 moles of ethylene oxide per mole of alcohol.
• ethoxylated alcohols examples include the condensation product of myristyl alcohol with about 10 moles of ethylene oxide per mole of alcohol; the condensation product of coconut alcohol (a mixture of fatty alcohols with alkyl chains varying in length from about 10 to about 14 carbon atoms) with about 9 moles of ethylene oxide, and the condensation product of tallow alcohol with about 25 moles of ethylene oxide.
• nonionic surfactants of this type include Tergitol® 15-S-9 moles (the condensation product of C-11-C15 linear alcohol with 9 moles ethylene oxide),Tergitol® 24-L-6 NMW (the condensation product of C12-C14 primary alcohol with 6 moles ethylene oxide with a narrow molecular weight distribution), both marketed by Union Carbide Corporation; Neodol® 45-9 (the condensation product of C-14-C15 linear alcohol with 9 moles of ethylene oxide).
• Neodol® 23-6.5 (the condensation product of C12-C13 linear alcohol with 6.5 moles of ethylene oxide), Neodol® 45-7 (the condensation product of C14-C15 linear alcohol with 7 moles of ethylene oxide), Neodol® 45-4 (the condensation product of C14- C ⁇
• the condensation products of ethylene oxide with a hydrophobic base formed by the condensation of propylene oxide with propylene glycol.
• the hydrophobic portion of these compounds has a molecular weight of from about 1500 to about 1800 and exhibits water insolubility.
• the addition of polyoxyethlene moieties to this hydrophobic portion tends to increase the water solubility of the molecules as a whole, and the liquid character of the product is retained up to the point where the polyoxyethylene content is about 50% of the total weight of the condensation product, which corresponds to condensation with up to about 40 moles of ethylene oxide.
• Examples of compounds of this type include certain of the commercially-available Pluronic® surfactants, marketed by Wyandotte Chemical Co ⁇ oration.
• the condensation products of ethylene oxide with the product resulting from the reaction of propylene oxide and ethylenediamine consist of the reaction product of ethylenediamine and excess propylene oxide, and generally has a molecular weight of from about 2500 to about 3000.
• This hydrophobic moiety is condensed with ethylene oxide to the extent that the condensation product contains from about 40% to about 80% by weight of polyoxyethylene and has a molecular weight of from about 5,000 to about 11,000.
• Examples of this type of nonionic surfactant include certain of the commercially available Tetronic® compounds, marketed by Wyandotte Chemical Co ⁇ oration.
• Semi-polar nonionic surfactants which include water-soluble amine oxides containing one alkyl moiety of from about 10 to about 18 carbon atoms and 2 moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups containing from about 1 to about 3 carbon atoms; water-soluble phosphine oxides containing one alkyl moiety of from about 10 to about 18 carbon atoms and 2 moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups containing from about 1 to about 3 carbon atoms; and water-soluble sulfonides containing one alkyl moiety of from about 10 to about 18 carbon atoms and a moiety selected from the group consisting of alkyl and hydroxyalkyl moieties of from about 1 to about 3 carbon atoms.
• Preferred semi-polar nonionic surfactants are the amine oxide surfactants having the formula:
• R20(OR21) X N(R22) 2 (IX) wherein R 0 JS an alkyl, hydroxyalkyl, or alkyl phenyl group or mixtures thereof containing from about 8 to about 22 carbon atoms; R21 is an alkylene or hydroxyalkylene group containing from about 2 to about 3 carbon atoms or mixtures thereof; x is from 0 to about 3; and each R is an alkyl or hydroxyalkyl group containing from about 1 to about 3 carbon atoms or a polyethylene oxide group containing from about 1 to about 3 ethylene oxide groups.
• the R22 groups can be attached to each other, e.g., through an oxygen or nitrogen atom to form a ring structure.
• Preferred amine oxide surfactants are C-
• Any reducing saccharide containing 5 or 6 carbon atoms can be used, e.g., glucose, galactose and galactosyl moieties can be substituted for the glucosyl moieties.
• the hydrophobic group is attached at the 2-, 3-, 4-, etc. positions thus giving a glucose or galactose as opposed to a glucoside or galactoside.
• the intersaccharide bonds can be, e.g., between the one position of the additional saccharide units and the 2-, 3-, 4-, and/or 6-positions on the preceding saccharide units.
• a polyalkyleneoxide chain joining the hydrophobic moiety and the polysaccharide moiety.
• the preferred alkyleneoxide is ethylene oxide.
• Typical hydrophobic groups include alkyl groups, either saturated or unsaturated, branched or unbranched containing from about 8 to about 18, preferably from about 10 to about 16, carbon atoms.
• the alkyl group is a straight chain saturated alkyl group.
• the alkyl group can contain up to about 3 hydroxy groups and/or the polyalkyleneoxide chain can contain up to about 10, preferably less than 5, alkyleneoxide moieties.
• Suitable alkyl polysaccharides are octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, and octadecyl, di-, tri-, tetra-, penta-, and hexaglucosides, galactosides, lactosides, glucoses, fructosides, fructoses and/or galactoses.
• Suitable mixtures include coconut alkyl, di-, tri-, tetra-, and pentaglucosides and tallow alkyl tetra- , penta-, and hexaglucosides.
• the preferred alkylpolyclycosides have the formula:
• R2 3 O(C m H 2m O)t(glycosyl) u (X) wherein R23 is selected from the group consisting of alkyl, alkylphenyl, hydroxyalky, hydroxyalkylphenyl, and mixtures thereof in which the alkyl groups contain from about 10 to about 18, preferably from about 12 to about 14, carbon atoms; m is 2 or 3, preferably 2; t is from 0 to about 10, preferably 0; and u is from about 1.3 to about 10, preferably from about 1.3 to about 3, most preferably from about 1.3 to about 2.7.
• the glycosyl is preferably derived from glucose.
• the alcohol or alkylpolyethoxy alcohol is formed first and then reacted with glucose, or a source of glucose, to form the glucoside (attachment at the 1 -position).
• the additional glycosyl units can then be attached between their 1 -position and the preceding glycosyl units 2-, 3-, 4- and/or 6-position, preferably predominately the 2-position.
• Fatty acid amide surfactants having the formula: O
• R24_ C N(R25)(R26) V ' wherein R2 4 is an alkyl group containing from about 7 to about 21 (preferably from about 9 to about 17) carbon atoms and R25 and R26 are each selected from hydrogen, C1-C4 alkyl, C1-C4 hydroxyalkyl, and -(C2H4O) w H where w varies from about 1 to about 3.
• Preferred amides are C8-C20 ammonia amides, monoethanolamides, diethanolamides, and isopropanolamides.
• Polyhydroxy fatty acid amides have the above formula with R 25 being methyl and R 2 6 being glycityl derived from a reduced sugar or alkoxylated derivative thereof.
• R 25 being methyl
• R 2 6 being glycityl derived from a reduced sugar or alkoxylated derivative thereof.
• Examples are N-methyl-N-1- deoxyglucityl cocoamide and N-methyl-N-1-deoxyglucityl oleamide.
• Such compounds and processes for making them are disclosed in U.S. Patent Nos. 2,965,576, 2,703,798, and 5,194,639, incorporated herein by reference.
• the alkyl chain of the fatty acid preferably contains from about 8 to about 22 carbon atoms, more preferably from about 14 to about 18 carbon atoms.
• Ethoxylated fatty acids having from about 2 to about 10, especially from about 2 to about 4, moles of ethylene oxide per mole of fatty acid are preferred.
• Examples of such ethoxylated fatty acids include the condensation product of fatty acids derived from tallow with about 2 moles of ethylene oxide per mole of fatty acid, commercially available as Istemul ® 610 from Arancia Tensoactivos, S.A. de C.V., Guadalajara, Mexico, and the condensation product of stearic acid with about 75 moles of ethylene oxide per mole of fatty acid, commercially available as Pegosperse® 4000 from Glyco Co ⁇ .
• Glycerol esters of fatty acids Preferred are glycerol monoesters of fatty acids.
• the alkyl of the fatty acids preferably contains from about 8 to about 22 carbon atoms, more preferably from about 10 to about 20 carbon atoms, more preferably still from about 14 to about 18 carbon atoms.
• Examples of such surfactants include glycerol monostearate (GMS) commercially available as Emulquim® 70 from Quimic S.A. de C.V., Morelia, Mexico. 10.
• Sorbitan esters and ethoxylated sorbitan esters Sorbitan esters are esterified dehydration products of sorbitol.
• sorbitan esters comprise a member selected from about C-J Q- C26- preferably about C12-C22.
• Sorbitan esters containing unsaturation e.g., sorbitan monooleate
• Details, including formula, of preferred sorbitan esters can be found in U.S. Patent Nos. 4,128,484 and 4,022,938, incorporated herein by reference.
• sorbitan esters especially the "lower" ethoxylates thereof (i.e., mono-, di-, and tri-esters wherein one or more of the unesterified -OH groups contain from 1 to about 20 oxyethylene moieties) are also useful in the composition of the present invention.
• An example of a preferred material is Polysorbate 61 known as Tween® 61 from ICI America.
• sorbitan monostearate is a preferred material.
• Mixtures of sorbitan stearate and sorbitan palmitate having stearate/palmitate weight ratios varying between 10:1 and 1:10, and 1,5-sorbitan esters are also preferred. Both the 1 ,4- and 1 ,5-sorbitan esters are preferred.
• alkyl sorbitan esters for use in the compositions of the subject invention include sorbitan monolaurate, sorbitan monomyristate, sorbitan monopalmitate, sorbitan monobehenate, sorbitan monooleate, sorbitan diiaurate, sorbitan dimyristate, sorbitan dipalmitate, sorbitan distearate, sorbitan dibehenate, sorbitan dioleate, and mixtures thereof, and mixed tallowalkyl sorbitan mono- and di ⁇ esters.
• Preferred sorbitan ester mixtures can contain up to about 15% by weight of esters of the C20-C26. and higher, fatty acids, as well as minor amounts of C ⁇ , and lower, fatty esters.
• Sorbitan esters are readily prepared by reacting hydroxy-substituted sorbitans, particularly the 1,4- and 1,5-sorbitans, with the corresponding acid, ester, or acid chloride in a simple esterification reaction.
• Commercial materials prepared in this manner will comprise mixtures usually containing minor proportions of uncyclized sorbitol, fatty acids, polymers, isosorbide structures, and the like. In the subject invention compositions, it is preferred that such impurities are present at as low a level as possible.
• Polyhydroxy fatty acid amides include N-aryloxy polyhydroxy fatty acid amide surfactants of the formula:
• N-alkyl polyhydroxy fatty acid amide surfactants of the formula:
• R 1 8 is about C7-C21 hydrocarbyl, preferably about C9-C17 hydrocarbyl, including straight-chain and branched-chain alkyl, or mixtures thereof;
• R 1 * 5 is about C2-C8 hydrocarbyl including straight-chain, branched-chain and cyclic (including aryl), and is preferably about C2-C4 alkylene, i.e., -CH2CH2- , -CH2CH2CH2- and -CH2(CH 2 )2CH 2 -;
• R 17 is about C ⁇
• R ⁇ 9 is about C ⁇ -C ⁇ alkyl or hydroxyalkyl, including methyl (preferred), ethyl, propyl, isopropyl, butyl, pen
• V preferably will be derived from a reducing sugar in a reductive amination reaction; more preferably V is a glycityl moiety.
• Suitable reducing sugars include glucose, fructose, maltose, lactose, galactose, mannose, and xylose, as well as glyceraldehyde.
• high dextrose corn syrup, high fructose corn syrup, and high maltose corn syrup can be utilized as well as the individual sugars listed above. These corn syrups may yield a mix of sugar components for V. It should be understood that it is by no means intended to exclude other suitable raw materials.
• V preferably will be selected from the group consisting of -CH2-(CHOH) z - CH 2 OH, -CH(CH 2 OH)-(CHOH) z . 1 -CH2OH, -CH 2 -
• (CHOH) 2 (CHOR 30 )(CHOH)-CH 2 OH where z is an integer from 1 to 5, inclusive, and R 3 ⁇ is H or a cyclic mono- or poly- saccharide, and alkoxylated derivatives thereof. Most preferred are glycityls wherein z is 4, particularly -CH 2 -(CHOH) -CH2OH.
• nonlimiting examples of the amine substituent group -R16-0-R17 can be, for example: 2- methoxyethyl-, 3-methoxypropyl-, 4-methoxybutyl-, 5-methoxypentyl-,
• R18_CO-N ⁇ can be, for example, cocamide, stearamide, oleamide, lauramide, myristamide, capricamide, palmitamide, tallowamide, etc.
• Preferred nonionic surfactants for the subject invention compositions include ethoxylated fatty alcohols, ethoxylated fatty acids, and glycerol esters of fatty acids.
• the subject compositions are preferably substantially free of, more preferably free of, surfactants which are alkoxylated ethers of sterols, such as cholesterol, e.g., ethoxylated cholesterol.
• Particularly preferred nonionic surfactants for the subject invention compositions include glycerol mono about C12- 20 carboxylates, ethoxylated about C12-C20 fattv acids having from about 2 to about 10 moles of ethylene oxide per mole of mole of fatty acid, and ethoxylated about C12- 20 fatty alcohols having from about 5 to about 30 moles of ethylene oxide per mole of fatty alcohol.
• the fabric softening single strength compositions of the subject invention comprise from about 0.4% to about 5% nonionic surfactant, preferably from about 0.5% to about 4%, more preferably from about 0.8% to about 3%, more preferably still from about 1% to about 2%.
• the concentrates of such compositions comprise from about 0.8% to about 20% nonionic surfactant, preferably from about 2% to about 15%, also preferably from about 3% to about 10%.
• the ratio of cationic softener to nonionic surfactant in the subject compositions and concentrates is from about 1:2 to about 4:1 , preferably from about 1 :114 to about 3:1 , also preferably from about 1 :1 to about 2:1, also preferably from about 1:1% to about V ⁇ to 1.
• the single strength fabric softening compositions of the subject invention preferably comprise a total of the amount of cationic softener plus nonionic surfactant of from about 1% to about 7%, more preferably from about 1.2% to about 6%, more preferably still from about 1.5% to about 4%, still more preferably from about 2% to about 3%.
• the concentrates of such compositions preferably comprise a total amount of cationic softener plus nonionic surfactant of from about 2% to about 30%, preferably from about 3% to about 25%, more preferably from about 4% to about 20%, also preferably from about 5% to about 15%.
• the ratio of cationic softener plus nonionic surfactant to perfume in the subject compositions and concentrates is preferably from about 1 :1 to about 10:1 , more preferably from about 2:1 to about 8:1 , more preferably still from about 3:1 to about 6:1.
• compositions and concentrates can optionally be aided by incorporation of water-soluble ionizable inorganic salts.
• ionizable salts can be used. Examples of suitable salts are the alkali or alkaline earth halides, e.g., calcium chloride, magnesium chloride, sodium chloride, potassium bromide, and lithium chloride. Calcium chloride is preferred.
• the amount of water-soluble ionizable salt inco ⁇ orated in the subject invention compositions and concentrates depends upon the desired viscosity, and the amounts of cationic softener, anionic surfactant, and perfume in the composition. The proper amount is readily determined by the formulator. Typically, the amount of salt required to achieve a desired viscosity for the subject products increases with (1) lower cationic softener levels and (2) lower nonionic surfactant levels. Care must be taken to not add too much salt, since that can easily result in instability and phase separation in the product.
• compositions and concentrates typically comprise from 0% to about 1% water-soluble ionizable inorganic salts, preferably from about 0.03% to about 0.5%, more preferably from about 0.05% to about 0.4%, also preferably from about 0.1% to about 0.3%, also preferably from about 0.2% to about 0.7%, also preferably from about 0.07% to about 0.2%.
• the subject invention compositions are aqueous-based suspensions. Because the hydrophobic materials in the subject compositions are not truly soluble in water at the levels present in the compositions, the subject compositions are dispersions of very fine particles, most of which are preferably sub-micron in size.
• the subject compositions are stable dispersions, maintaining their homogeneity as such fine particle dispersions, and not separating into discrete hydrophilic and hydrophobic phases for long periods of time.
• the subject compositions are stable and do not separate into discrete phases for at least about 6 months when stored at 25°C, more preferably for at least about 12 months when stored at 25°C.
• the single strength fabric softening compositions of the subject invention comprise from about 90% to about 98.5% water, preferably from about 92% to about 98%, more preferably from about 94% to about 97.5%, also preferably from about 95% to about 97%.
• the concentrates of such compositions comprise from about 60% to about 97% water, preferably from about 70% to about 96%, also preferably from about 80% to about 95%.
• compositions can optionally comprise a number of other ingredients commonly found in fabric softening compositions.
• Enzymes for treating fabrics can be included in the subject compositions, such enzymes including proteases, lipases, amylases, and cellulases.
• Preferred enzymes for incorporation in the subject compositions are cellulases, including both bacterial and fungal cellulases. Suitable cellulases are disclosed in U.S. Patent No.
• Cellulase is preferably included in the subject compositions such that the activity of the cellulase is from about 0.5 CEVU to about 100 CEVU per liter of a 1x composition, more preferably from about 4 CEVU to about 25 CEVU, more preferably still from about 7 CEVU to about 12 CEVU.
• the activity of a cellulase material (CEVU) is determined from the viscosity decrease of a standard CMC solution as follows. A substrate solution is prepared which contains 35g/l CMC (Hercules 7 LFD) in 0.1 M tris buffer at pH 9.0. The cellulase sample to be analyzed is dissolved in the same buffer.
• compositions preferably comprise a bactericide as a preservative.
• bactericides used in the compositions include glutaraldehyde, formaldehyde, 2-bromo-2-nitro-propane-1 ,3-diol sold by Inolex Chemicals under the tradename Bronopol®, and a mixture of 5- chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one sold by Rohm and Haas Company under the tradename Kaython®.
• compositions are preferably maintained somewhat acidic by the incorporation of a small amount of inorganic acid, such as hydrochloric acid.
• the pH of the subject single strength compositions is preferably from about 2 to about 5, more preferably from about 3 to about 4.
• Colorants are preferably incorporated in the subject invention compositions by inco ⁇ orating dye solutions in the compositions to obtain the desired color for the compositions.
• compositions include thickeners, soil release agents, antifoam agents (e.g., silicone), chelants, and others, disclosed, for example, in U.S. Patent Nos. 4,767,547 and 5,066,414.
• the single strength fabric softening compositions of the subject invention comprise from 0% to about 2% of such other optional ingredients, preferably from about 0.02% to about 0.5%.
• the concentrates of such compositions comprise from 0% to about 10% of such other optional ingredients, preferably from about 0.05% to about 5%.
• compositions preferably consist substantially of, more preferably consist of, the cationic fabric softeners, hydrophobic perfumes, nonionic surfactants, water-soluble ionizable inorganic salts, water, and optional components disclosed hereinabove, in the amounts disclosed hereinabove.
• compositions and concentrates are typically made in a mixing vessel equipped with a high-speed agitator and a water jacket for heating or cooling.
• batches can be made in a mixing vessel having a capacity of 3 liters, the vessel being cylindrical in shape, 16 cm in diameter and 23 cm high.
• the agitator used to mix the batch has a standard impeller having 6 blades having a pitch of 90°, the blades extending 4 cm from the center of the shaft.
• the "standard" agitator speed for such mixing vessel and agitator for the subject invention processes is a high speed, about 700-1000 ⁇ m. Larger mixing vessels will typically have larger diameter agitator impellers run at a slower rpm, and smaller mixing vessels will typically have smaller diameter agitator impellers run at faster rpm, such that the tip speed of the impellers are about the same.
• the processes of the subject invention used for making the subject invention compositions preferably involve four mixing stages.
• the first mixing stage is carried out at a temperature above the melting points of the cationic softener and the nonionic surfactant.
• the water is added to the mixing vessel and is preheated, either before or after addition, to the desired temperature for the first mixing stage, typically from about 30°C to about 70°C, preferably from about 40°C to about 60°C.
• the agitator is preferably run at the standard speed throughout the first stage of mixing.
• Dye solution if any, is added to the mixing vessel and blended with the water. Any hydrochloric acid is added slowly to the mixing vessel and blended.
• the cationic softener and nonionic surfactant are preheated and premixed at a temperature above their melting points, preferably at least about 5°C and preferably up to about 40°C above the water temperature.
• the cationic softener/nonionic surfactant premix is added slowly over a period to the mixing vessel, preferably at a substantially constant rate of addition of from about 10 ml/min to about 40 ml/min, with continuous agitation.
• Other minor ingredients, such as antifoam agents, preservatives, enzymes, soil release agents, etc., (but preferably not chelants), if desired in the composition, are added and blended with continuous agitation.
• the temperature of the mixture in the mixing vessel is adjusted to from about 40°C to about 60°C, preferably from about 45°C to about 55°C with continuing agitation, preferably at the standard speed, to prepare for the second stage of mixing.
• the second stage of mixing involves the slow addition of perfume to the mixing vessel at this adjusted temperature, preferably with continued agitation at the standard speed.
• the perfume is added over a period, preferably at a substantially constant rate of addition of from about 10 ml/min to about 40 ml/min. Agitation is continued for at least about 1 min, preferably for at least about 2 min, after addition of the perfume is completed.
• the mixture in the mixing vessel is homogenized in the third stage, preferably using a high-sheer (very high speed) mixer, such as a Greerco homomixer model 1-L at about 6000 to 8000 ⁇ m.
• a high-sheer very high speed
• adequate homogenization can be achieved for some compositions by mixing with a mixer such as that used for the previous steps, for longer time periods. Homogenizing is preferred because of the resulting compositions exhibit less hydrophobic particle size variation.
• the hydrophobic perfume is dispersed as small hydrophobic particles held in suspension by the surfactant activity of the cationic softener and nonionic surfactant.
• the mixture is preferably homogenized at a temperature of less than about 30°C.
• the homogenization or additional mixing can be carried out at temperatures above 30°C, preferably up to about 40°C, as long as the fourth stage of mixing is carried out at about the same temperature as the third stage.
• the mixture is preferably homogenized or mixed until the diameter of the hydrophobic particles is as specified hereinabove. Care must be taken not to over-homogenize and produce hydrophobic particles smaller than desired.
• the fourth stage of mixing for the subject processes is carried out by adding, over a period, the water-soluble, ionizable inorganic salt to the mixture, preferably with the agitator running at about one-half the standard speed (moderate speed).
• the salt is preferably added as a concentrated aqueous solution (for example, about 15% salt), at a substantially constant rate or intermittently a portion at a time at a rate of from about 5ml/min to about 40 ml min, with constant agitation. Agitation for too long after addition of the salt is completed can result in an unstable product, so such agitation is continued preferably for at most about 4 minutes, more preferably for at most about 2 minutes, after addition of the salt is completed.
• chelants are preferably added during the fourth mixing stage.
• materials are added "over a period" to aqueous mixtures being agitated. This means that the material is added at a slow enough rate (constant or intermittent) to insure that the material is homogeneously blended into the aqueous mixture.
• compositions and concentrates of the subject invention exemplify compositions and concentrates of the subject invention.
• a single strength composition having the following formula is made by the process described below.
• Example 1 having a total batch weight of 1 kg is made in a mixing vessel which is generally cylindrical in shape having a diameter of 16 cm and a height of 23 cm, and having a capacity of about 4 liters.
• the water at a temperature of 60°C, is added to the mixing vessel, and the agitator, having an impeller with 6 blades of 4 cm length (measured from the center of the shaft to the blade tip) at a pitch of 90°, is run at a speed of 1070 ⁇ m.
• the dye solution is added to the mixing vessel and blended with the water.
• the hydrochloric acid is added slowly to the mixing vessel over a period of 0.5 minutes and blended with continuous agitation.
• the DTDMAC and GMS are melted, premixed to a homogeneous liquid, and heated to 75°C. This premix is added to the mixing vessel using a metering pump to provide a constant rate of addition 22 ml/min.
• the silicone is added to the mixing vessel and blended with continued agitation.
• the mixture is circulated through a homogenizer, Greerco model 1-L, run at a speed of 6500 rpm, for about 1 min, thus producing hydrophobic particles having a mean diameter of about 6 microns with 90% of the particles having a diameter of less than about 12 microns and 90% of the particles having a dieameter of greater than about 3 microns.
• the calcium chloride is blended into the homogenized mixture in the mixing vessel with the agitator running at the speed of 500 rpm.
• the calcium chloride is added a portion at a time intermittently over a period of two minutes with continuous agitation.
• the agitation is stopped 2 minutes after all the calcium chloride is added.
• the resulting final product is allowed to cool to room temperature, and is filled into individual bottles, providing the finished product.
• Example 10 having a total batch weight of 1 kg, is made in a mixing vessel which is generally cylindrical in shape having a diameter of 16 cm and a height of 23 cm, having a capacity of 4 liters.
• the water at a temperature of 38°C, is added to the mixing vessel, and the agitator, having an impeller with 6 blades of 4 cm length (measured from the center of the shaft to the blade tip) at a pitch of 90°, is run at a speed of 750 ⁇ m.
• the dye solution is added to the mixing vessel and blended with the water.
• the hydrochloric acid is added slowly to the mixing vessel over a period of 0.5 minute and blended with continuous agitation.
• the DTDMAC and GMS are melted, premixed to a homogeneous liquid, and heated to 63°C.
• the premix is added to the mixing vessel using a metering pump to provide a constant rate of addition of 22 ml/min.
• the silicone is added to the mixing vessel and blended with continued agitation.
• the resulting final product is allowed to cool and is filled into individual bottles, providing the finished product.

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