EP0734433B1 - Viskositätsstabile konzentrierte weichspülerzusammensetzungen - Google Patents

Viskositätsstabile konzentrierte weichspülerzusammensetzungen Download PDF

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Publication number
EP0734433B1
EP0734433B1 EP95904876A EP95904876A EP0734433B1 EP 0734433 B1 EP0734433 B1 EP 0734433B1 EP 95904876 A EP95904876 A EP 95904876A EP 95904876 A EP95904876 A EP 95904876A EP 0734433 B1 EP0734433 B1 EP 0734433B1
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Prior art keywords
group
fabric softening
alkyl
acid
formula
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French (fr)
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EP0734433A1 (de
EP0734433B2 (de
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John Cort Severns
Alice Marie Vogel
Errol Hoffman Wahl
Robert Mermelstein
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Procter and Gamble Co
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Procter and Gamble Co
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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
    • C11D3/0005—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
    • C11D1/645—Mixtures of compounds all of which are cationic
    • 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

Definitions

  • the present invention relates to concentrated aqueous textile treatment compositions.
  • it relates to textile treatment compositions for use in the rinse cycle of a textile laundering operation to provide fabric softening/static control benefits, the compositions being characterized by excellent storage stability and excellent viscosity stability after freeze/thaw cycling.
  • Aqueous textile treatment compositions suitable for providing fabric softening and static control benefits during laundering are well-known in the art and have found wide-scale commercial application.
  • aqueous, rinse-added, fabric softening compositions contain, as the active softening component, substantially water-insoluble cationic materials having two long alkyl chains. Typical of such materials are di-hydrogenated tallow di-methyl ammonium chloride and imidazolinium compounds substituted with two stearyl groups. These materials are normally prepared in the form of a dispersion in water.
  • Cationic softener materials are normally supplied by the manufacturer containing about 70%-90% of active material in an organic liquid such as isopropanol or ethanol, sometimes containing a minor amount of water (up to 10%).
  • Retail fabric softening compositions are then prepared by dispersion of the softener in warm or hot water under carefully controlled conditions.
  • the physical form and dispersibility constraints of these industrial concentrates are such as to preclude their direct use by the domestic consumer; indeed, they can pose severe processing problems even for the industrial supplier of retail fabric softening compositions.
  • the present invention contains diester quaternary ammonium material (hereinafter referred to as "DEQA") as an essential component. Two primary types of DEQA are preferred.
  • the first type of DEQA preferably comprises, as the primary active, compounds of the formula: [(R) 4-m -N (+) -[(CH 2 ) n -Y-R 2 ] m ] X (-) wherein each R substituent is a short chain C 1 -C 6 , preferably C 1 -C 3 alkyl or hydroxyalkyl group, e.g., methyl (most preferred), ethyl, propyl, hydroxyethyl, and the like, benzyl or mixtures thereof each m is 2 or 3; each n is from 1 to about 4; each Y is -O-(O)C-, or -C(O)-O-, but not -OC(O)O-; each R 2 is a long chain C 12 -C 22 hydrocarbyl, or substituted hydrocarbyl substituent, preferably C 15 -C 19 alkyl or alkylene, most preferably C 15 -C 17 straight chain alkyl or alkylene
  • substituents R and R 2 can optionally be substituted with various groups such as alkoxyl or hydroxyl groups, and can be straight, or branched so long as the R 2 groups maintain their basically hydrophobic character.
  • the preferred compounds can be considered to be diester variations of ditallow dimethyl ammonium chloride (hereinafter referred to as "DTDMAC”), which is a widely used fabric softener. At least 80% of the DEQA is in the diester form, and from 0% to 20% can be DEQA monoester (e.g., only one of the ester groups is hydrolyzed to yield either-Y-H, or an -OH group).
  • the diester when specified, it can include the monoester that is present.
  • the percentage of monoester should be as low as possible, preferably no more than about 2.5%.
  • the overall ratios of diester to monoester are from 100:1 to 2:1, preferably from 50:1 to 5:1, more preferably from 13:1 to 8:1.
  • the di/monoester ratio is preferably about 11:1.
  • the level of monoester present can be controlled in manufacturing the DEQA.
  • the above compounds used as the biodegradable quaternized ester-amine softening material in the practice of this invention, can be prepared using standard reaction chemistry.
  • an amine of the formula RN(CH 2 CH 2 OH) 2 is esterified at both hydroxyl groups with an acid chloride of the formula R 2 C(O)Cl, then quaternized with an alkyl halide, RX, to yield the desired reaction product (wherein R and R 2 are as defined hereinbefore).
  • RX alkyl halide
  • this reaction sequence allows a broad selection of agents to be prepared.
  • the following are non-limiting examples (wherein all long-chain alkyl substituents are straight-chain): where -C(O)R 2 is derived from hardened tallow fatty acid.
  • stable liquid compositions herein are formulated at a neat pH in the range of from 2.5 to 4. The pH can be adjusted by the addition of a Bronsted acid. pH ranges for making stable softener compositions containing diester quaternary ammonium fabric softening compounds are disclosed in U.S. Pat. No. 4,767,547, Straathof, issued Aug. 30, 1988.
  • Suitable Bronsted acids include the inorganic mineral acids, carboxylic acids, in particular the low molecular weight (C 1 -C 5 ) carboxylic acids, and alkylsulfonic acids.
  • Suitable inorganic acids include HCl, H 2 SO 4 , HNO 3 and H 3 PO 4 .
  • Suitable organic acids include formic, acetic, citric, methylsulfonic and ethylsulfonic acids.
  • Preferred acids are hydrochloric, phosphoric, and citric acids.
  • the primary active has the general formula: wherein each Y, R, R 2 , and X (-) have the same meanings as before.
  • Such compounds include those having the formula: [CH 3 ] 3 N (+) [CH 2 CH(CH 2 OC[O]R 2 )OC(O)R 2 ] C1 (-) where C(O)R 2 is derived from hardened tallow fatty acid.
  • each R is a methyl or ethyl group and preferably each R 2 is in the range of C 15 to C 19 Degrees of branching and substitution can be present in the alkyl chains.
  • the anion X (-) in the molecule is the same as in DEQA (1) above.
  • the diester when specified, it can include the monoester that is present.
  • the amount of monoester that may be present is the same as in DEQA (1).
  • the present invention may also contain mixtures of the two primary types of DEQA.
  • compositions prepared by the present invention contain as an essential component a co-active fabric softening material, as described hereinafter, which is different from the biodegradable diester quaternary ammonium softening material
  • Di(2-amidoethyl)methyl quaternary ammonium salts are also suitable for use as Component (B) in the compositions of the invention herein, especially those having the formula: wherein each R 7 is selected from the group consisting of C 14 to C 20 alkyl and alkenyl groups, wherein each R 8 is selected from methyl, ethyl, and -(C m H 2m O) n 3H, wherein n 3 is from 1 to about 5, preferably 3, and wherein m, and X (-) have the same meaning as before.
  • This class of agents is disclosed in U.S. Pat. No. 4,134,840, Minegishi et al., issued January 16, 1979.
  • Exemplary materials are di((2-hydrogenatedtallowamidoethyl) ethoxylated (2 ethoxy groups) methyl ammonium methylsulfate, di(2-oleylamidoethyl) propoxylated (3-propoxy groups) methyl ammonium bromide, di(2-palmitoleylamidoethyl) dimethyl ammonium ethylsulfate and di(2-stearylamidoethyl) propoxylated (2 propoxy groups) methyl ammonium methylsulfate.
  • An exemplary commercial material suitable for use as Component (B) herein is di(2-tallowamidoethyl) ethoxylated methyl ammonium methylsulfate (such that the I.V. Component B is about 31) sold under the name Varisoft 222, from Witco Chemical Company.
  • a co-active fabric softening material for use as component (B) in the composition of the invention herein can also have the formula: wherein each R 9 is C 15 - C 17 alkyl group such that the IV of the parent fatty acid of this R 9 group is from 20 to 100, preferably from 30 to 70, most preferably from 35 to 60; and X (-) has the-same meaning as before.
  • a preferred fabric softening material of the present invention is prepared according to the synthesis disclosed in U.S. Pat. No. 3,915,867, Kang et al., issued October 28, 1975.
  • the fabric softening material generally comprises the reaction of purified C 14 -C 18 fatty acid alkylester mixture, triethanolamine, and a quaternizing reagent, preferably dimethyl sulfate.
  • the select fatty acid alkylesters are preferably a mixture of substantial amounts of oleic, palmitic, stearic add alkyl esters and may include minor amounts of other fatty substances.
  • a co-active fabric softening material suitable for use as Component (B) in the composition of the invention can also have the formula: wherein each R 10 is a C 12 - C 22 hydrocarbyl or substituted hydrocarbyl substituent, preferably C 15 - C 19 alkyl or alkylene, most preferably C 15 - C 17 straight chain alkyl or alkylene such that the IV of the parent fatty acid of this R 10 group is from 20 to 100, preferably from 30 to 70, most preferably from 35 to 60; and R and X (-) have the same meaning as before.
  • Tallow is a convenient and inexpensive source of long chain alkyl and alkenyl materials.
  • a specific example of a diester quaternary ammonium compound suitable for use in this invention herein include:
  • Suitable diester quaternary ammoniums of this invention are obtained by, e.g.: replacing "tallowyl” in the above compounds with, for example, cocoyl, palmoyl, lauryl, oleyl, stearyl, palmityl, or the like; replacing "methyl” in the above compounds with ethyl, propyl, isopropyl, butyl, isobutyl, t-butyl, or the hydroxy substituted analogs of these radicals; replacing "chloride” in the above compounds with bromide, methylsulfate, formate, sulfate, or nitrate.
  • the anion is merely present as a counterion of the positively charged quaternary ammonium compounds disclosed herein.
  • the scope of this invention is not considered limited to any particular anion.
  • the materials herein can be prepared by standard esterification and quaternization reactions, using readily available starting materials. General methods for preparation are disclosed in U.S. Pat. No. 4,137,180.
  • a co-active fabric softening material suitable for use as Component (B) in the composition of the invention can also have the formula: [(R) 4-m -N (+) -[(CH 2 ) n -Y-R 11 ] m ] X (-) except for those according to (3), wherein each R 11 is a long chain C 12 -C 22 , hydrocarbyl, or substituted hydrocarbyl substituent, preferably C 15 -C 19 alkyl or alkylene, most preferably C 15 -C 17 straight chain alkyl or alkylene such that the IV of the parent fatty acid of this R 11 group is from 20 to 100, preferably from 30 to 70, most preferably from 35 to 60; and each m, n, Y, R and X (-) have the same meaning as before.
  • the DEQA (A) material is (1), the requirement for component (B) is not met by this material and it is not present.
  • the present invention may also contain mixtures of the various co-active fabric softening materials.
  • compositions of the present invention herein comprise from about 15% to about 35%, preferably from about 20% to about 32%, most preferably from about 22% to about 27% of component (A) + component (B).
  • the ratio of component (A) to component (B) is from 0.25:1 to 4:1, preferably from 0.3:1 to 1.5:1.
  • the present invention utilizes an acid of sufficient concentration to keep the pH at the desired level and optionally, to fully protonate component (B) to the extent that it is not already quaternized.
  • the composition of the present invention is prepared using a molten premix of components (A) + (B), (hereinafter referred to as premix).
  • premix molten premix of components (A) + (B), (hereinafter referred to as premix).
  • premix molten premix of components (A) + (B), (hereinafter referred to as premix).
  • premix molten premix of components (A) + (B), (hereinafter referred to as premix).
  • premix molten premix of components (A) + (B), (hereinafter referred to as premix).
  • the premix is injected into an acid/water seat, then high shear milling is conducted and, electrolyte is added in no specific order.
  • the electrolyte is selected from the group consisting of the Group IA and IIA metals of the periodic table of elements, e.g., calcium chloride, sodium chloride, potassium bromide, and lithium chloride, and ammonium salts, e.g., ammonium chloride and lysine HCl.
  • the acid/water seat has an acid concentration up to about 2%.
  • the acid to (B) molar ratio is from about 0:1 to about 1.2:1.
  • the acid to (A) molar ratio is from about 0:1 to about 0.2:1.
  • the neat pH of the final composition is preferably from about 2.5 to about 4.
  • Suitable acids include the Bronsted acids, especially inorganic mineral acids and organic acids such as carboxylic acids.
  • Carboxylic acids include, in particular, the low molecular weight (C 1 -C 5 ) carboxylic acids of the formula R 12 -COOH (R 12 being a C 1 -C 5 or H alkyl group).
  • Suitable organic acids are selected from the group having the formula R 13 CH 2 SO 3 H, wherein R 13 is hydrogen or C 1 to C 4 alkyl.
  • Suitable specific organic acids include formic, methylsulfonic, ethylsulfonic, citric, gluconic, and aromatic carboxylic acids like benzoic acid.
  • Suitable inorganic acids include HCl, HBr, H 2 SO 4 , H 2 SO 3 , HNO 3 , and H 3 PO 4 .
  • Preferred acids are phosphoric, formic, acetic, hydrochloric, citric, and methylsulfonic acids. Mixtures of the above organic and inorganic acids are also suitable. Typically, acids such as citric, hydrochloric, phosphoric, and sulfuric are used because of their low cost and availability.
  • compositions of the present invention herein comprise from about 60% to about 90%, preferably from about 65% to about 85% of an aqueous liquid carrier.
  • the preferred aqueous carrier is water which can contain minor ingredients.
  • Fully-formulated fabric softening compositions made by the process of the present invention can optionally contain one or more of the following ingredients.
  • the fabric softening compositions herein optionally contain an aqueous emulsion of a predominantly linear polydialkyl or alkyl aryl siloxane in which the alkyl groups can have from one to five carbon atoms and can be wholly, or partially, fluoridated.
  • Suitable silicones are polydimethyl siloxanes having a viscosity, at 25°C, of from about 100 to about 100,000 centistokes, preferably from about 1,000 to about 12,000 centistokes. In some applications as low as 1 centistoke materials are preferred.
  • the fabric softening compositions herein can contain from about 0.1% to about 10%, of the silicone component.
  • the fabric softening compositions herein contain from 0% to about 3%, preferably from about 0.01% to about 2%, of a thickening agent.
  • suitable thickening agents include: cellulose derivatives, synthetic high molecular weight polymers (e.g., carboxyvinyl polymer and polyvinyl alcohol), and cationic guar gums.
  • the cellulosic derivatives that are functional as thickening agents herein can be characterized as certain hydroxyethers of cellulose, such as Methocel, marketed by Dow Chemicals, Inc.; also, certain cationic cellulose ether derivatives, such as Polymer JR-125, JR-400, and JR-30M, marketed by Union Carbide.
  • cationic guar gums such as Jaguar Plus, marketed by Stein Hail, and Gendrive 458, marketed by General Mills.
  • Preferred thickening agents herein are selected from the group consisting of methyl cellulose, hydroxypropyl methylcellulose, hydroxybutyl methylcellulose, or mixtures thereof, said cellulosic polymer having a viscosity in 2% aqueous solution at 20C of from about 15 to about 75,000 centipoises.
  • an optional soil release agent may be added.
  • the addition of the soil release agent may occur in combination with the premix, in combination with the acid/water seat, before or after electrolyte addition, or after the final composition is made.
  • the softening composition prepared by the process of the present invention herein can contain from 0% to about 10%, preferably from 0.2% to about 5%, of a soil release agent.
  • a soil release agent is a polymer.
  • Polymeric soil release agents useful in the present invention include copolymeric blocks of terephthalate and polyethylene oxide or polypropylene oxide, and the like.
  • a preferred soil release agent is a copolymer having blocks of terephthalate and polyethylene oxide. More specifically, these polymers are comprised of repeating units of ethylene terephthalate and polyethylene oxide terephthalate at a molar ratio of ethylene terephthalate units to polyethylene oxide terephthalate units of from 25:75 to about 35:65, said polyethylene oxide terephthalate containing polyethylene oxide blocks having molecular weights of from about 300 to about 2000. The molecular weight of this polymeric soil release agent is in the range of from about 5,000 to about 55,000.
  • Another preferred polymeric soil release agent is a crystallizable polyester with repeat units of ethylene terephthalate units containing from about 10% to about 15% by weight of ethylene terephthalate units together with from about 10% to about 50% by weight of polyoxyethylene terephthalate units, derived from a polyoxyethylene glycol of average molecular weight of from about 300 to about 6,000, and the molar ratio of ethylene terephthalate units to polyoxyethylene terephthalate units in the crystallizable polymeric compound is between 2:1 and 6:1.
  • this polymer include the commercially available materials Zelcon 4780 (from Dupont) and Milease T (from ICI).
  • Highly preferred soil release agents are polymers of the generic formula: in which each X can be a suitable capping group, with each X typically being selected from the group consisting of H, and alkyl or acyl groups containing from about 1 to about 4 carbon atoms.
  • p is selected for water solubility and generally is from about 6 to about 113, preferably from about 20 to about 50.
  • u is critical to formulation in a liquid composition having a relatively high ionic strength. There should be very little material in which u is greater than 10. Furthermore, there should be at least 20%, preferably at least 40%, of material in which u ranges from about 3 to about 5.
  • the R 14 moieties are essentially 1,4-phenylene moieties.
  • the term "the R 14 moieties are essentially 1,4-phenylene moieties” refers to compounds where the R 14 moieties consist entirely of 1,4-phenylene moieties, or are partially substituted with other arylene or alkarylene moieties, alkylene moieties, alkenylene moieties, or mixtures thereof.
  • Arylene and alkarylene moieties which can be partially substituted for 1,4-phenylene include 1,3-phenylene, 1,2-phenylene, 1,8-naphthylene, 1,4-naphthylene, 2,2-biphenylene, 4,4-biphenylene, and mixtures thereof.
  • Alkylene and alkenylene moieties which can be partially substituted include 1,2-propylene, 1,4-butylene, 1,5-pentylene, 1,6-hexamethylene, 1,7-heptamethylene, 1,8-octamethylene, 1,4-cyclohexylene, and mixtures thereof.
  • the degree of partial substitution with moieties other than 1,4-phenylene should be such that the soil release properties of the compound are not adversely affected to any great extent.
  • the degree of partial substitution which can be tolerated will depend upon the backbone length of the compound, i.e., longer backbones can have greater partial substitution for 1,4-phylene moieties.
  • compounds where the R 14 comprise from about 50% to about 100% 1,4-phenylene moieties (from 0% to about 50% moieties other than 1,4-phenylene) have adequate soil release activity.
  • polyesters made according to the present invention with a 40:60 mole ratio of isophthalic (1,3-phenylene) to terephthalic (1,4-phenylene) acid have adequate soil release activity.
  • the R 14 moieties consist entirely of (i.e., comprise 100%) 1,4-phenylene moieties, i.e., each R 14 moiety is 1,4-phenylene.
  • suitable ethylene or substituted ethylene moieties include ethylene, 1,2-propylene, 1,2-butylene, 1,2-hexylene, 3-methoxy-1,2-propylene, and mixtures thereof
  • the R 15 moieties are essentially ethylene moieties, 1,2-propylene moieties, or mixtures thereof. Inclusion of a greater percentage of ethylene moieties tends to improve the soil release activity of compounds. Surprisingly, inclusion of a greater percentage of 1,2-propylene moieties tends to improve the water solubiity of compounds.
  • 1,2-propylene moieties or a similar branched equivalent is desirable for incorporation of any substantial part of the soil release component in the liquid fabric softener compositions.
  • each p is at least about 6, and preferably is at least about 10.
  • the value for each n usually ranges from about 12 to about 113. Typically the value for each p is in the range of from about 12 to about 43.
  • soil release agents can also act as scum dispersants.
  • the premix can be combined with an optional scum dispersant, other than the soil release agent, and heated to a temperature at or above the melting point(s) of the components.
  • the preferred scum dispersants herein are formed by highly ethoxylating hydrophobic materials.
  • the hydrophobic material can be a fatty alcohol, fatty acid, fatty amine, fatty acid amide, amine oxide, quaternary ammonium compound, or the hydrophobic moieties used to form soil release polymers.
  • the preferred scum dispersants are highly ethoxylated, e.g., more than about 17, preferably more than about 25, more preferably more than about 40, moles of ethylene oxide per molecule on the average, with the polyethylene oxide portion being from about 76% to about 97%, preferably from about 81% to about 94%, of the total molecular weight.
  • the level of scum dispersant is sufficient to keep the scum at an acceptable, preferably unnoticeable to the consumer, level under the conditions of use, but not enough to adversely affect softening. For some purposes it is desirable that the scum is nonexistent.
  • the amount of anionic or nonionic detergent, etc.. used in the wash cycle of a typical laundering process the efficiency of the rinsing steps prior to the introduction of the compositions herein, and the water hardness, the amount of anionic or nonionic detergent surfactant and detergency builder (especially phosphates and zeolites) entrapped in the fabric (laundry) will vary.
  • the minimum amount of scum dispersant should be used to avoid adversely affecting softening properties.
  • scum dispersion requires at least about 2%, preferably at least about 4% (at least 6% and preferably at least 10% for maximum scum avoidance) based upon the level of softener active.
  • levels of about 10% (relative to the softener material) or more one risks loss of softening efficacy of the product especially when the fabrics contain high proportions of nonionic surfactant which has been absorbed during the washing operation.
  • Preferred scum dispersants are: Brij 700; Varonic U-250; Genapol T-500, Genapol T-800; Plurafac A-79; and Neodol 25-50.
  • bactericides used in the compositions of this invention include glutaraldehyde, formaldehyde, 2-bromo-2-nitro-propane-1,3-diol sold by Inolex Chemicals, located in Philadelphia, Pennsylvania, under trade name Bronopol, and a mixture of 5-chloro-2-methyl-4-isothiazoline-3-one and 2-methyl-4-isothiazoline-3-one sold by Rohm and Haas Company under the trade name Kathon CG/ICP.
  • Typical levels of bactericides used in the present compositions are from about 1 to about 1,000 ppm by weight of the agent.
  • the present invention can include optional components conventionally used in textile treatment compositions, for example, short chain alcohols such as ethanol, or propylene glycol, colorants, perfumes, preservatives, optical brighteners, opacifiers, surfactants, stabilizers such as guar gum and polyethylene glycol, anti-shrinkage agents, fabric crisping agents, spotting agents, germicides, fungicides, anti-oxidants such as butylated hydroxy toluene, anti-corrosion agents, and the like.
  • short chain alcohols such as ethanol, or propylene glycol
  • colorants such as ethanol, or propylene glycol
  • perfumes preservatives, optical brighteners, opacifiers, surfactants, stabilizers such as guar gum and polyethylene glycol
  • anti-shrinkage agents such as guar gum and polyethylene glycol
  • fabric crisping agents such as spotting agents
  • germicides such as fungicides
  • anti-oxidants such as buty
  • compositions of the present invention are preferably used in the rinse cycle of the conventional automatic laundry operations.
  • rinse water has a temperature of from about 15°C to about 60°C.
  • Fabrics or fibers are contacted with an effective amount, generally from about 20 ml to about 300 ml (per 3.5 kg of fiber or fabric being treated), of the compositions herein in an aqueous bath.
  • an effective amount generally from about 20 ml to about 300 ml (per 3.5 kg of fiber or fabric being treated), of the compositions herein in an aqueous bath.
  • the amount used is based upon the judgment of the user, depending on concentration of the softening materials, (A) + (B), fiber or fabric type, degree of softness desired, and the like.
  • from about 20 ml to about 300 ml of 9% to 40% dispersion of the softening materials (A) + (B) are used in a 25 gallon laundry rinse bath to soften and provide antistatic benefits to a 3.5 kg load of mixed fabrics.
  • the rinse bath contains from about 20 ppm to about 250 ppm of the fabric softening materials (A) + (B) herein. More preferably for United States conditions, the rinse bath contains from about 50 ppm to about 150 ppm of the fabric softening materials (A) + (B). More preferably for European conditions, the rinse bath contains from about 250 ppm to about 450 ppm of the fabric softening materials (A) + (B). More preferably for Japanese conditions, the rinse bath contains from about 30 ppm to about 80 ppm of the fabric softening materials (A) + (B). These concentration levels achieve superior fabric softening and static control.
  • the first three ingredients in each Formula are co-melted in a pyrex beaker, covered with a concave watchglass, for three hours at about 80-85°C to form the premix.
  • the water, HCl, and silicone antifoam are separately weighed into a sealed container and heated to about 83°C to form the water seat.
  • the premix is then injected into the water seat over three to four minutes at about 72°C while stirring at from about 1500 to about 3000 r.p.m.
  • a 15% aqueous solution of Lysine/HCl is added to the water seat/premix dispersion over seven minutes at about 71°C while stirring at from about 500 to about 1000 r.p.m..
  • the perfume, and the silicone DC-200 are added to the dispersion over thirty seconds.
  • the dispersion is milled for two minutes at about 70°C at from about 4000 to about 8000 r.p.m. of the mill.
  • a 40% aqueous solution of soil release polymer is added to the dispersion over two minutes at about 66°C while stirring at from about 500 to about 1000 r.p.m..
  • the dispersion is then chilled in an ice bath at about 25°C for 8 minutes while stirring at from about 200 to about 500 r.p.m..
  • compositions containing mixtures of the two softener active materials, Component (A) and Component (B), (Formulas 2-4), have more stable viscosities at temperatures down to 10°C, than compositions containing only the individual softener active Component (A) or Component (B), (Formulas 1 and 5).
  • Ditallow Imidazoline Amide in the amount of 375g is melted by heating to about 93°C.
  • This molten softener is then dispersed into 376g of deionized water at about 82°C containing 90g of a 28.25% HCl solution and 4.8g of the DC-2210 silicone antifoam over five minutes while stirring with an IKA model RW20 DZM stirrer at 400-600 r.p.m..
  • the resulting dispersion is stirred for an additional four minutes.
  • a second aliquot of about 82°C deionized water in the amount of 580g is stirred into the thick dispersion over two and one half minutes.
  • a blend of 20.25g of perfume and 2.85g of DC-200 silicone fluid is then added to the dispersion over thirty seconds, followed by two and one half minutes of mixing with an IKA Ultra-Turrax T50 high shear mill at 8000 r.p.m..
  • the dispersion is then cooled to room temperature over three minutes by passing it through a small plate and frame heat exchanger.
  • the preservative in the amount of 0.3g is added at room temperature following the cool down.
  • N,N-di(hydrogenated tallowyl-oxy-ethyl)-N,N-dimethyl ammonium chloride in the amount of 431g and 24g of ethanol are melted at about 91°C.
  • This molten softener is dispersed into 954g of deionized water at about 82°C containing 8.25g of a 0.968 N HCl solution, 4.8g of DC-2210 silicone antifoam and 18.75g of a 40% solution of soil release polymer over five and one half minutes while stirring at 800-1100 r.p.m.. Subsequently, 35g of an aqueous 15% CaCl2 solution is stirred into the dispersion over four and one half minutes.
  • a blend of 20.25g of perfume and 2.85g of DC-200 silicone fluid is then added to the dispersion over thirty seconds, followed by two and one half minutes of mixing with a high shear mill at 8000 r.p.m..
  • the preservative in the amount of 0.3g is added just prior to cool-out.
  • the dispersion is then cooled to room temperature over two and one half minutes by passing through a small plate and frame heat exchanger.
  • Ditallow Imidazoline Amide in the amount of 214g, 115.5g N,N-di(tallowyl-oxy-ethyl)-N,N-dimethyl ammonium chloride and 19g of ethanol are co-melted at about 91°C.
  • This molten softener mixture is dispersed into 1,102g of deionized water at about 82°C containing 14.55g of HCl and 4.8g of DC-2210 silicone antifoam over five and one half minutes while stirring at 800-1100 r.p.m..
  • 37.5g of an aqueous 15% CaCl2 solution is stirred into the dispersion over four and one half minutes.
  • a blend of 20.25g of perfume and 2.85g of DC-200 silicone fluid is then added to the dispersion over thirty seconds, followed by two and one half minutes of mixing with high shear mill at 8000 r.p.m..
  • the dispersion is then cooled to room temperature over two and one half minutes by passing it through a small plate and frame heat exchanger.
  • the preservative in the amount of 0.3g is added at room temperature following cool-out.
  • Example II Materials prepared in the same manner as Example III except that the amounts of imidazoline, N,N-di(hydrogenated tallowyl-oxy-ethyl)-N,N-dimethyl ammonium chloride, ethanol, and HCl vary according to the formulas shown above.

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Claims (7)

  1. Stabile, wäßrige, flüssige, konzentrierte Wäscheweichmacherzusammensetzung, umfassend:
    (A) bioabbaubares quaternäres Diester-Ammonium-Wäscheweichmachermaterial, gewählt aus der Gruppe, bestehend aus: [ (R)4-m-N(+)-[(CH2)n-Y-R2]m ] X(-) worin jedes R aus der Gruppe gewählt ist, bestehend aus C1-C6-Alkyl- oder -Hydoxyalkylgruppen: jedes m 2 ist, jedes n 1 bis 4 ist; jedes R2 aus der Gruppe gewählt ist, bestehend aus C12-C22-Hydrocarbyl- oder substituierten Hydrocarbylgruppen, so daß die Iodzahl (IV) der Stammfettsäure dieser R2-Gruppe weniger als 10 beträgt; jedes Y die Bedeutung -O-(O)C- oder -C(O)-O, jedoch nicht OC(O)O hat; und wobei X(-) ein kompatibles Anion ist; oder
    Figure 00390001
    worin Y, R, R2 und X(-) jeweils die gleichen Bedeutungen wie oben haben; oder Mischungen hiervon: und
    (B) coaktives Wäscheweichmachermaterial, gewählt aus der Gruppe, bestehend aus:
    Figure 00390002
    worin jedes R7 aus der Gruppe gewählt ist, bestehend aus C14-C20-Alkyl- und -Alkenylgruppen;jedes R8 aus Methyl, Ethyl und -(CmH2mO)n3H gewählt ist; worin n3 1 bis 5 ist; und worin in und X(-) jeweils die gleichen Bedeutungen wie oben haben;
    oder
    Figure 00400001
    worin jedes R9 eine C15-C17-Fettalkylgruppe ist, so daß die Iodzahl (IV) der Stammfettsäure dieser R9-Gruppe 20 bis 100 beträgt, und X(-) die gleiche Bedeutung wie oben hat; oder
    Figure 00400002
    worin jedes R10 ein C12-C22-Hydrocarbyl- oder substituierter Hydrocarbylsubstituent ist, so daß die Iodzahl (IV) der Stammfettsäure dieser R10-Gruppe 20 bis 100 beträgt, und R und X(-) die gleichen Bedeutungen wie oben haben; oder [ (R)4-m-N(+)-[(CH2)n-Y-R11]m ] X(-) mit Ausnahme derjenigen gemäß (3), worin jedes R11 ein langkettiger C12-C22-Hydrocarbyl- oder substituierter Hydrocarbylsubstituent ist, so daß die Iodzahl (IV) der Stammfettsäure dieser R11-Gruppe 20 bis 100 beträgt, und m, n, Y, R und X(-) jeweils die gleichen Bedeutungen wie oben haben: oder Mischungen hiervon: wobei die Gesamtmenge der Komponenten (A) + (B) 15 bis 35%, vorzugsweise 20 bis 32%. weiter vorzugsweise 22 bis 27%, beträgt, wobei das Verhältnis von (A) zu (B) 0,25:1 bis 4:1, und nach weiter bevorzugt 0,3:1 bis 1,5:1 beträgt; wobei, wenn (A) die Bedeutung (1) hat, (B) nicht (5) ist: wobei, wenn (A) die Bedeutung (2) hat, (B) nicht (4) ist; wobei, wenn (A) die Bedeutung (1) hat, wobei ein R Methyl und das andere C2H4OH ist, (B) nicht (3) ist: wobei, wenn B (3) [CH2CH2OH] (CH3) +N [(CH2CH2OC(O) R2] X(-) ist, X- wie vorangehend definiert ist, A nicht (1) ist; und wobei vorzugsweise das fertige, wäßrige, konzentrierte Wäscheweichmachermittel einen unverdünnten pH von 2,5 bis 4 aufweist.
  2. Stabile, wäßrige, flüssige, konzentrierte Wäscheweichmacherzusammensetzung nach Anspruch 1, umfassend:
    (A) bioabbaubares, quaternäres Diester-Ammonium-Wäscheweichmachermaterial der Formel: [ (R)4-m-N(+)-[(CH2)n-Y-R2]m ] X(-) worin jedes R aus der Gruppe gewählt ist, bestehend aus C1-C6-Alkyl- oder -Hydroxyalkylgruppen: jedes in 2 ist; jedes n 1 bis 4 ist: jedes R2 aus der Gruppe gewählt ist, bestehend aus C12-C22-Hydrocarbyl- oder substituierten Hydrocarbylgruppen, so daß die Iodzahl (IV) der Stammfettsäure dieser R2-Gruppe weniger als 10 beträgt; jedes Y -O-(O)C- oder -C(O)-O, jedoch nicht OC(O)O ist; und wobei X(-) ein kompatibles Anton ist; und
    (B) coaktives Wäscheweichmachermaterial der Formel
    Figure 00410001
    worin jedes R7 aus der Gruppe gewählt ist, bestehend aus C14-C20-Alkyl- und -Alkenylgruppen; jedes R8 aus Methyl, Ethyl und -(CmH2mO)n3H gewählt ist; worin n3 1 bis 5 ist; und worin m und X(-) jeweils die gleiche Bedeutung wie oben haben.
  3. Stabile, wäßrige, flüssige, konzentrierte Wäscheweichmacherzusammensetzung nach Anspruch 1, umfassend
    (A) bioabbaubares, quaternäres Diester-Ammonium-Wäscheweichmachermaterial der Formel:
    Figure 00410002
    worin jedes Y-O-(O)C oder -C(O)-O-, jedoch nicht -OC(O)O ist; und wobei jedes R aus der Gruppe gewählt ist, bestehend aus C1-C6-Alkyl- oder Hydroxyalkylgruppen; jedes R2 aus der Gruppe gewählt ist, bestehend aus C12-C22-Hydrocarbyl- oder substituierten Hydrocarbylgruppen, so daß die Iodzahl (IV) der Stammfettsäure dieser R2-Gruppe weniger als 10 beträgt, und wobei X(-) ein kompatibles Anton ist; und
    (B) coaktives Wäscheweichmachermaterial der Formel
    Figure 00420001
    worin jedes R7 aus der Gruppe gewählt ist, bestehend aus C14-C20-Alkyl- und -Alkenylgruppen; jedes R8 aus Methyl, Ethyl und -(CmH2mO)n3H gewählt ist; worin n3 1 bis 5 ist: und worin m und X(-) jeweils die gleichen Bedeutungen wie oben haben.
  4. Stabile, wäßrige, flüssige, konzentrierte Wäscheweichmacherzusammensetzung nach Anspruch 1, umfassend
    (A) bioabbaubares, quaternäres Diester-Ammonium-Wäscheweichmachermaterial der Formel:
    Figure 00420002
    worin jedes Y -O(O)C oder -C(O)O-, jedoch nicht -OC(O)O ist; und worin jedes R aus der Gruppe gewählt ist, bestehend aus C1-C6-Alkyl- oder Hydroxyalkylgruppen; jedes R2 aus der Gruppe gewählt ist, bestehend aus C12-C22-Hydrocarbyl- oder substituierten Hydrocarbylgruppen, so daß die Iodzahl (IV) der Stammfettsäure dieser R2-Gruppe weniger als 10 beträgt, und worin X(-) ein kompatibles Anion ist; und
    (B) coaktives Wäscheweichmachermaterial der Formel
    Figure 00430001
    worin jedes R9 eine C15-C17-Fettalkylgruppe ist, so daß die IV der Stammfettsäure dieser R9-Gruppe 20 bis 100 beträgt, und worin X(-) die gleiche Bedeutung wie oben hat.
  5. Stabile, wäßrige, flüssige, konzentrierte Wäscheweichmacherzusammensetzung nach Anspruch 1, umfassend
    (A) bioabbaubares, quaternäres Diester-Ammonium-Wäscheweichmachermaterial der Formel:
    Figure 00430002
    worin jedes Y -O(O)C oder -C(O)O-, jedoch nicht -OC(O)O ist; und worin jedes R aus der Gruppe gewählt ist, bestehend aus C1-C6-Alkyl- oder -Hydroxyalkylgruppen; jedes R2 aus der Gruppe gewählt ist, bestehend aus C12-C22-Hydrocarbyl- oder substituierten Hydrocarbylgruppen, so daß die Iodzahl (IV) der Stammfettsäure dieser R2-Gruppe weniger als 10 beträgt, und worin X(-) ein kompatibles Anion ist; und
    (B) coaktives Wäscheweichmachermaterial der Formel [ (R)4-m-N(+)-[(CH2)n-Y-R11]m ] X(-) worin jedes R11 ein langkettiger C12-C22-Hydrocarbyl- oder substituierter Hydrocarbylsubstituent ist, so daß die Iodzahl (IV) der Stammfettsäure dieser R11-Gruppe 20 bis 100 beträgt, und m, n, Y, R und X(-) jeweils die gleichen Bedeutungen wie oben haben: oder Mischungen hiervon.
  6. Verfahren zur Herstellung einer Zusammensetzung nach mindestens einem der Ansprüche 1-5, umfassend die Schritte der Verwendung einer geschmolzenen Vormischung, umfassend:
    A. Vormischen von (A) bioabbaubarem, quaternärem Diester-Ammonium-Wäscheweichmachermittel und (B) sekundärem Wäscheweichmachermittel; und
    B. Injizieren der Vormischung in eine Säure/Wasser-Auflage, vorzugsweise umfassend eine Säure, gewählt aus der Gruppe, bestehend aus anorganischen Mineralsäuren und organischen Säuren der Formel R12COOH, worin R12 eine C1-C5H- oder Alkylgruppe ist, oder R13 CH2SO3H, worin R13 Wasserstoff oder C1-C4-Alkyl ist, und Mischungen hiervon: wobei weiter vorzugsweise die Säure Phosphorsäure, Chlorwasserstoffsäure, Citronensäure oder Mischungen hiervon ist: wobei vorzugsweise die Säurekonzentration der Säure/Wasser-Auflage bis zu 2% beträgt; und wobei vorzugsweise das Molverhältnis von Säure zu (B) 0:1 bis 1,2:1 beträgt: und
    C. Durchführen von Hochscher-Mahlen und Zugeben von Elektrolyt, vorzugsweise gewählt aus der Gruppe, bestehend aus Salzen von Metallen der Gruppe IA und IIA des Periodensystems, vorzugsweise Calciumchlorid oder Ammoniumsalzen.
  7. Verfahren nach Anspruch 6, wobei die Vormischung mit einem Schaumdispergiermittel kombiniert wird.
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US6559117B1 (en) * 1993-12-13 2003-05-06 The Procter & Gamble Company Viscosity stable concentrated liquid fabric softener compositions
GB9816659D0 (en) * 1998-07-30 1998-09-30 Dow Europ Sa Composition useful for softening, cleaning, and personal care applications and processes for the preparation thereof
GB0021765D0 (en) 2000-09-05 2000-10-18 Unilever Plc A method of preparing fabric conditioning compositions
GB0021766D0 (en) 2000-09-05 2000-10-18 Unilever Plc Fabric conditioning compositions
MXPA04012377A (es) * 2002-06-13 2005-02-25 Procter & Gamble Composiciones que comprenden un sistema activo suavizante de telas que comprende por lo menos dos activos cationicos suavizantes de telas.
US6927202B2 (en) 2002-09-19 2005-08-09 Unilever Home & Personal Care, Usa Division Of Conopco, Inc. Fabric conditioning compositions
CN102230278B (zh) * 2011-06-07 2013-02-13 廊坊乐万家联合家化有限公司 一种浓缩衣物柔顺剂及其制备方法
EP3390603A4 (de) * 2015-12-15 2019-07-10 Rhodia Operations Verfahren zur erhöhung der stabilität einer zusammensetzung unter verwendung von qav und polysacchariden
US10351805B2 (en) * 2015-12-22 2019-07-16 Rhodia Operations Compositions comprising a quat and a mixture of a nonionic and two cationic polysaccharides

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