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
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
  • C11D3/3738—Alkoxylated silicones
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/38—Cationic compounds
  • C11D1/62—Quaternary ammonium compounds
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/0005—Other compounding ingredients characterised by their effect
  • C11D3/001—Softening compositions
  • C11D3/0015—Softening compositions liquid
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
  • C11D3/3742—Nitrogen containing silicones

Definitions

• the present invention relates to textile treatment compositions.
• it relates to textile softening compositions for use in the rinse cycle of a textile laundering operation to provide fabric softeners having improved biodegradability, excellent fabric softening/static control benefits, and improved rewettability.
• Fabric softening compositions tend to diminish the ability of cotton fabrics to take up water.
• Traditionally there has been a trade-off between fabric softening and fabric absorbency. Normally, the use of more effective fabric softener actives and/or more fabric softener active in the rinse makes the treated fabrics, especially cotton fabrics, less water absorbent. I.e., the choice has been between better softening with high performance softener compositions and better water absorbency with poor performance softener compositions.
• the present invention provides textile treatment compositions which contain more biodegradable fabric softener actives which maintain high fabric softening performance while having improved fabric rewettability characteristics when used after a broad range of detergent types.
• liquid carrier selected from the group consisting of: water; low molecular weight organic solvents that are highly soluble/miscible in water such as C1-C4 monohydric alcohols, C2 ⁇ c 6 polyhydric alcohols, polyalkylene glycols; and mixtures thereof. All percentages, ratios and proportions are by weight, unless otherwise specified. All numbers are approximations unless otherwise stated.
• the present invention relates to rinse-added fabric softener compositions comprising, as essential components, from about 5% to about 50%, preferably from about 6% to about 35%, more preferably from about 7% to about 32%, by weight of the composition, of biodegradable cationic softener active, preferably an ester quaternary ammonium softener active (EQA) and from about 0.2% to about 20%, preferably from about 0.5% to about 10%, more preferably from about 1% to about 5%, silicone, as described hereinafter.
• biodegradable Cationic Fabric Softener Active preferably an ester quaternary ammonium softener active (EQA) and from about 0.2% to about 20%, preferably from about 0.5% to about 10%, more preferably from about 1% to about 5%, silicone, as described hereinafter.
• EQA ester quaternary ammonium softener active
• the preferred biodegradable cationic softener active containing ester linkages in the long hydrophobic groups has the formula: EP + [Y - R 2 ] m pX " wherein p is 1 to 2; m is 2 or 3; each E is a nitrogenous quaternary group of charge p+; each Y is -0-(0)C-, or -C(0)-0-; R 2 is the same or different C11-C22 hydrocarbyl or substituted hydrocarbyl substituent; and
• X is any softener-compatible anion such as chloride, bromide, methylsulfate, ethyl sulfate, formate, nitrate and the like; preferably E is selected from the group consisting of:
• each R is a C ] .- Cg alkyl or substituted alkyl group (e.g., hydroxy alkyl), preferably C-1-C3 alkyl group, e.g., methyl (most preferred), ethyl, propyl, and the like, a benzyl group, hydrogen, and mixtures thereof; wherein R is derived from C]_ ⁇ -C22 fatty acyl groups.
• a preferred EQA with E of the formula (1) above, has the formula:
• each R is a short chain C ] _- C ⁇ alkyl or substituted alkyl group (e.g., hydroxyalkyl, preferably hydroxy ethyl, preferably C1-C3, alkyl, e.g., methyl (most preferred) , ethyl, propyl, and the like, or substituted alkyl group (e.g., hydroxy alkyl, preferably hydroxyethyl), benzyl, or mixtures thereof, preferably alkyl; each R 2 is a long chain, preferably at least partially unsaturated, e.g..
• biodegradable softener actives with E (1) are N,N-di(tallowoyloxyethyl)-N,N- dimethylammoniu chloride and N,N-di (tallowyloxyethyl)- N- (2-hydroxyethyl)-N-methylammonium methyl sulfate.
• a non-limiting example of a biodegradable softener active with E (2) is 1,2-ditallowoyloxy-3- trimethylammoniopropane chloride.
• EQA compounds prepared with fully saturated alkyl groups (R 2 ) are rapidly biodegradable and excellent softeners.
• compounds prepared with at least partially unsaturated alkyl groups have many advantages
• EQA with unsaturated alkyl groups provide improved fabrics with improved water absorbency as compared to EQA with saturated alkyl groups.
• IV Iodine Value
• the EQA provides excellent antistatic effect. Antistatic effects are especially important where the fabrics are dried in a tumble dryer, and/or where synthetic materials which generate static are used. Maximum static control occurs with an IV of greater than about 20, preferably greater than about 40. When fully saturated EQA compositions are used, poor static control results. Also, formulas with higher softener concentrations will typically require higher Iodine Values.
• the benefits of concentratability include: use of less packaging material; use of less organic solvents, especially volatile organic solvents; use of less concentration aids which may add nothing to performance; etc.
• EQA containing unsaturated fatty acyl groups can be concentrated above about 13* without the need for additional concentration aids, especially surfactant concentration aids.
• EQA derived from highly unsaturated fatty acyl groups i.e., fatty acyl groups having a total unsaturation above about 65% by weight, do not provide any additional improvement in antistatic effectiveness. They may, however, be able to provide other benefits such as improved water absorbency of the fabrics.
• an IV range of from about 40 to about 65 is preferred for concentratability, maximization of fatty acyl sources, excellent softness, static control, etc.
• Highly concentrated aqueous dispersions of diester compounds can gel and/or thicken during low (about 5°C) temperature storage.
• compositions containing diester compounds made from fatty acids having an IV of from about 5 to about 25, preferably from about 10 to about 25, more preferably from about 15 to about 20, and a cis/trans isomer weight ratio greater than about 30/70, preferably greater than about 50/50, more preferably greater than about 70/30, are storage stable at low temperature with minimal odor formation. These cis/trans isomer weight ratios provide optimal concentratability at these IV ranges. In the IV range above about 25, the ratio of cis to trans isomers is less important unless higher concentrations are needed.
• the concentration that will be stable in an aqueous composition will depend on the criteria for stability (e.g., stable down to about 5°C; stable down to 0°C; doesn't gel; gels but recovers on heating, etc.) and the other ingredients present, but the maximum concentration that is stable can be raised by adding concentration aids to achieve the desired stability.
• diester compounds derived from fatty acyl groups having low IV values can be made by mixing fully hydrogenated fatty acid with touch hydrogenated fatty acid at a ratio which provides an IV of from about 5 to about 25.
• the polyunsaturation content of the touch hardened fatty acid should be less than about 5%, preferably less than about 1%.
• touch hardening the cis/trans isomer weight ratios are controlled by methods known in the art such as by optimal mixing, using specific catalysts, providing high K 2 availability, etc. Touch hardened fatty acid with high cis/trans isomer weight ratios is available commercially (i.e., Radiacid 406 from FINA) .
• R 2 can optionally be substituted with various groups such as alkoxyl ' or hydroxyl groups.
• Some of the preferred compounds can be considered to be diester variations of ditallow dimethyl ammonium chloride (DTDMAC) , which is a widely used fabric softener.
• DTDMAC ditallow dimethyl ammonium chloride
• the diester when specified, it will include the monoester that is normally present.
• the level of monoester can be controlled during the manufacture of the EQA. Preferably, some of the monoester is present.
• the overall ratios of diester to monoester are from about 100:1 to about 2:1, preferably from about 50:1 to about 5:1, more preferably from about 13:1 to about 8:1. Under high anionic detergent carry- over conditions, the di/monoester ratio is preferably about 11:1.
• the silicone herein is either a polydimethyl siloxane (polydimethyl silicone or PDMS), or a derivative thereof, ' e.g., amino silicones, ethoxylated silicones, etc.
• the PDMS is preferably one with a low molecular weight, e.g., one having a viscosity of from about 2 to about 5000 cSt, preferably from about 5 to about 500 cSt, more preferably from about 25 to about 200- cSt Silicone emulsions can conveniently be used to prepare the compositions of the present invention.
• the silicone is one that is, at least initially, not emulsified.
• the silicone should be emulsified in the composition itself.
• the silicone is preferably added to the "water seat", which comprises the water and, optionally, any other ingredients that normally stay in the aqueous phase.
• Low molecular weight PDMS is preferred for use in the fabric softener compositions of this invention.
• the low molecular weight PDMS is easier to formulate without preemulsification.
• Silicone derivatives such as a ino-functional silicones, quaternized silicones, and silicone derivatives containing Si-OH, Si-H, and/or Si-Cl bonds, can be used. However, these silicone derivatives are normally more substantive to fabrics and can build up on fabrics after repeated treatments to actually cause a reduction in fabric absorbency.
• the fabric softener composition When added to water, the fabric softener composition deposits the biodegradable cationic fabric softening active on the fabric surface to provide fabric softening effects.
• cotton fabric water absorbency is appreciably reduced when there is more than about 40 ppm, especially when there is more than about 50 ppm, of the biodegradable cationic fabric softening active in the rinse water.
• the silicone improves the fabric water absorbency, especially for freshly treated fabrics, when used with this level of fabric softener without adversely affecting the fabric softening performance. The mechanism by which this improvement in water absorbency occurs is not understood, since the silicones are inherently hydrophobic. It is very surprising that there is any improvement in water absorbency, rather than additional los_s"of water absorbency.
• the amount of PDMS needed to provide a noticeable improvement in water absorbency is dependent on the initial rewettability performance, which, in turn, is dependent on the detergent type used in the wash. Effective amounts range from about 2 ppm to about 50 ppm in the rinse water, preferably from about 5 to about 20 ppm.
• the PDMS to softener active ratio is from about 2:100 to about 50:100, preferably from about 3:100 to about 35:100, more preferably from about 4:100 to about 25:100. As stated hereinbefore, this typically requires from about 0.2% to about 20%, preferably from about 0.5% to about 10%, more preferably from about 1% to about 5% silicone.
• the PDMS also improves the ease of ironing in addition to improving the rewettability characteristics of the fabrics.
• the fabric care composition contains an optional soil release polymer
• the amount of PDMS . deposited on cotton fabrics increases and PDMS improves soil release benefits on polyester fabrics.
• the PDMS improves the rinsing characteristics of the fabric care compositions by reducing the tendency of the compositions to foam during the rinse. Surprisingly, there is little, if any, reduction in the softening characteristics of the fabric care compositions as a result of the presence of the relatively large amounts of PDMS.
• the liquid carrier in the compositions of the present invention is preferably water, the carrier also can optionally comprise low molecular weight organic solvent that is highly soluble in water, e.g., C1-C4 onohydric alcohols, C2-C5 polyhydric alcohols including alkylene glycols, polyalkylene glycols, alkylene carbonates, and mixtures thereof.
• the water can be distilled, deionized, or tap water. Mixtures of water and up to about 15% of a short chain alcohol such as ethanol, propanol, isopropanol, and mixtures thereof are preferred carriers.
• water soluble solvents examples include: ethanol, propanol, isopropanol, n- butyl alcohol, t-butyl alcohol, ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, glycerol, propylene carbonate, and mixtures thereof.
• the present invention can include other optional components conventionally used in textile treatment compositions, for example, colorants, perfumes, preservatives, optical brighteners, opacifiers, fabric conditioning agents, surfactants, stabilizers such as guar gum, anti-shrinkage agents, anti-wrinkle agents, fabric crisping agents, anti-spotting agents, germicides, fungicides, anti-corrosion agents, anti-foam agents, and the like.
• Especially preferred optional ingredients include dispersibility aids, stabilizers, soil release agents, and bacteriocides.
• the optional dispersibility aids facilitate dispersion of the compositions of the present invention in the rinse water. They are selected from the group consisting of mono-alkyl cationic quaternary ammonium compounds, mono-alkyl amine oxides, and mixtures thereof, at a total level of from 0% to about 15%, preferably from about 0.5% to about 10%, more preferably from about 1% to about 5% by weight of the composition. These materials can either be added as part of the active softener raw material, (A) , or added as a separate component.
• the total level of dispersibility aid includes any amount that may be present as part of component (A) .
• Dispersibility aids include mono-alkyl cationic quaternary ammonium compound, preferably, the monoester derivatives of the biodegradable diester fabric softener actives having the formula:
• R 4 is Cg_C22 alkyl or alkenyl group, preferably c 10 ⁇ c 18 alkyl or alkenyl group; more preferably C]_o ⁇ c l4 or C_6 ⁇ c 18 alkyl or alkenyl group; each R 5 is a C_-Cg alkyl or substituted alkyl group (e.g., hydroxy alkyl), preferably C-1-C3 alkyl group, e.g., methyl (most preferred), ethyl, propyl, and the like, a benzyl group, hydrogen, a polyethoxylated chain with from about 2 to about 20 oxyethylene units, preferably from about 2.5 to about 13 oxyethylene units, more preferably from about 3 to about 10 oxyethylene units, and mixtures thereof; and
• X " is as defined hereinbefore for (A) .
• An especially preferred dispersibility aid is monolauryl trimethyl ammonium chloride and monotallow trimethyl ammonium chloride available from Witco under the trade name Varisoft® 471.
• the R 4 group can also be attached to the cationic nitrogen atom through a group containing one, or more, ester, amide, ether, amine, etc., linking groups which can be desirable for increased concentratability of component (A), biodegradability, etc.
• linking groups are preferably within from about one to about three carbon atoms of the nitrogen atom.
• Mono-alkyl cationic quaternary ammonium compounds also include C9-C22 alkyl choline esters, preferably i2 ⁇ c 14 choline ester and/or C ⁇ g-Cig tallow choline ester, and/or biodegradable single-long-chain alkyl dispersibility aids containing an ester linkage in the long chains as described in U.S. Pat. No. 4,840,738, Hardy and Walley, issued June 20, 1989, said patent being incorporated herein by reference.
• the compositions also contain a small amount, preferably from about 2% to about 5% by weight of the composition, of organic acid.
• organic acids are described in EPA 404,471, Machin et al., published on Dec. 27, 1990, which is herein incorporated by reference.
• the organic acid is selected from the group consisting of glycolic acid, acetic acid, citric acid, and mixtures thereof.
• Ethoxylated quaternary ammonium compounds which can serve as the dispersibility aid include ethylbis (polyethoxy ethanol)alkylammonium ethylsulfate with 17 moles of ethylene oxide, available under the trade name Variquat® 66 from Witco/Sherex Chemical Company; polyethylene glycol (15) oleammonium chloride, available under the trade name Ethoquad® 0/25 from Akzo; and polyethylene glycol (15) cocomonium chloride, available under the trade name Ethoquad® C/25 from Akzo.
• ethylbis (polyethoxy ethanol)alkylammonium ethylsulfate with 17 moles of ethylene oxide available under the trade name Variquat® 66 from Witco/Sherex Chemical Company
• polyethylene glycol (15) oleammonium chloride available under the trade name Ethoquad® 0/25 from Akzo
• quaternary compounds having only a single long alkyl chain can protect the diester softener from interacting with anionic surfactants and/or detergent builders that are carried over into the rinse from the wash.solution.
• Suitable dispersibility aids include amine oxides with one alkyl or hydroxyalkyl moiety of about 8 to about 22 carbon atoms, preferably from about 10 to about 18 carbon atoms, more preferably from about 8 to about 14 carbon atoms, and two alkyl moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups with about 1 to about 3 carbon atoms.
• Examples include dimethyloctylamine oxide, diethyldecylamine oxide, bis- (2-hydroxyethyl)dodecyl- amine oxide, dimethyldodecylamine oxide, dipropyl- tetradecylamine oxide, methylethylhexadecylamine oxide, dimethyl-2-hydroxyoctadecylamine oxide, and coconut fatty alkyl dimethylamine oxide.
• Stabilizers can .also be present in the compositions of the present invention.
• the term "stabilizer, " as used herein, includes antioxidants and reductive agents. These agents are present at a level of from 0% to about 2%, preferably from about 0.01% to about 0.2%, more preferably from about 0.035% to about 0.1% for antioxidants, and more preferably from about 0.01% to about 0.2% for reductive agents. These assure good odor stability under long term storage conditions. Antioxidants and reductive agent stabilizers are especially critical for unscented or low scent products (no or low perfume) .
• antioxidants examples include a mixture of ascorbic acid, ascorbic palmitate, propyl gallate, available from Eastman Chemical Products, Inc., under the trade names Tenox® PG and Tenox® S-l; a mixture of BHT (butylated hydroxytoluene) , BHA (butylated hydroxyanisole) , propyl gallate, and citric acid, available from Eastman Chemical Products, Inc., under the trade name Tenox®-6; butylated hydroxytoluene, available from UOP Process Division under the trade name Sustane® BHT; tertiary butylhydroquinone, Eastman Chemical Products, Inc., as Tenox® TBHQ; natural tocopherols, Eastman Chemical Products, Inc., as Tenox® GT-l/GT-2; and butylated hydroxyanisole, Eastman Chemical Products, Inc., as BHA; long chain esters (C 8 - C 22 ) of gallic acid,
• Irganox® 1035 41484-35-9 Thiodiethylene bis(3,5-di- tert-butyl-4-hydroxyhydro- cinnamate
• Irganox® 1425 65140-91-2 Calcium is[monoethyl (3,5- di-tert-butyl-4 hydroxybenzyl)- phosphonate]
• Irganox® 3125 34137-09-2 3,5-Di-tert-butyl-4- hydroxy-hydrocinnamic acid triester with 1,3,5-ris (2-hydroxy-ethyl)-S- triazine-2, 4, 6- (1H,3H, 5H)- trione
• compositions herein contain from 0% to about 10%, preferably from about 0.1% to about 5%, more preferably from about 0.1% to about 2%, 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.
• Typical levels of bacteriocides used in the present compositions are from about 1 ppm to about 2,000 ppm by weight of the composition, depending on the type of bacteriocide selected.
• Methyl paraben is especially effective for preventing mold growth in aqueous fabric softening compositions with under 10% by weight of the ester compound.
• fabrics or fibers are contacted with an effective amount, generally from about 10 ml to about 150 ml (per 3.5 kg of fiber or fabric being treated) of the softener composition (including ester quaternary ammonium compound and silicone) herein in an aqueous rinse bath.
• an effective amount generally from about 10 ml to about 150 ml (per 3.5 kg of fiber or fabric being treated) of the softener composition (including ester quaternary ammonium compound and silicone) herein in an aqueous rinse bath.
• the amount used is based upon the judgment of the user, depending on concentration of the composition, fiber cr fabric type, and degree of softness desire ⁇ .
• the rinse bath contains from about 40 .o about 1,000 ppm, preferably from about 50 to about 500 ppm, more preferably from about 50 to about 150 ppm, of total active fabric softening compounds herein and from about 2 ppm to about 50 ppm, preferably from about 3 ppm to about 30 ppm, more preferably from about 5 ppm to about 20 ppm silicone.
• a HC1 solution (25%) is added to about 886 g deionized water pre-heated to about 66°C in a stainless steel mixing tank.
• the water seat is mixed with an IKA mixer (Model RW 20 DZM) at about 1500 rpm using an impeller with about 5.1 cm diameter blades.
• About 12 g of an unemulsified Dow-Corning DC-200 50 cSt PDMS is added to the mix tank, with mixing.
• Example II Process The making procedure of Example II is similar to that of Example I, except that about 10 g of an unemulsified 350 cSt PDMS is used instead of the 50 cSt PDMS.
• compositions III and IV are made by the following process:
• the silicone can be added at any point in the process while the product is hot, for better stability of the viscosity over time, it is preferred to add the silicone in the water seat (as described above) , or alternatively, immediately before perfume addition at about 63-68°C.
• the silicone is added to the water seat and mixed by milling for about 5 minutes and then about 5-10% of the diester compound premix is injected into the water seat, followed by additional milling for about 5 minutes. Then, steps 3-8 above are followed.
• the silicone is "pre-emulsified" to retard any silicone phase separation on long term storage.
• Example V is prepared by a procedure similar to that of Example III, except that a Dow- Corning CF-1469 silicone emulsion, containing about 55% of a 350 cSt PDMS is used instead of the unemulsified PDMS and the emulsion is added last to the already cooled mixture.
• a Dow- Corning CF-1469 silicone emulsion containing about 55% of a 350 cSt PDMS is used instead of the unemulsified PDMS and the emulsion is added last to the already cooled mixture.
• a HC1 solution (25%) is added to about 874 g deionized water pre-heated to about 70°C in a 1.5L stainless steel mix tank.
• This "water seat” is mixed with an IKA mixer (Model RW 25) at about 1000 rpm using an impeller with about 5.1 cm diameter blades.
• Stepanquat 6585-ET containing about 85% hydroxyethyl ester quat in ethanol, pre-heated to about 70°C, is then slowly added to the water seat, by injection at the impeller blades via a peristaltic pump.
• the mixture is cooled during mixing, and about 4.5 g of perfume, about 0.2 g of a 1.5% Kathon solution, and about 0.8% of a 1% dye solution are added when the mixture temperature reaches about 45°C.
• About 0.6 g of a 25% CaCl2 solution is added when the mixture temperature reaches about 27°C.
• the mixing is stopped when the batch temperature reaches about 24°C.
• composition VII The making procedure of Composition VII is similar to that of Example VI, except that about 12 g of an unemulsified 50 cSt PDMS is used instead of the 350 cSt PDMS emulsion.
• Example VIII
• a HC1 solution (25%) is added to about 878 g deionized water pre-heated to about 74°C 'in a 1.5L stainless steel mix tank.
• the water seat is mixed with an IKA mixer (Model RW 20 DZM) at about 1000 rpm using an impeller with about 5.1 cm diameter blades. The mixture is also milled at the same time.
• About 21.8 g of DC CF-1469 silicone emulsion is added to the mix tank, with mixing.
• a mixture of about 86.7 g of the propane ester quat and 12 g of ethanol, pre-heated to about 82°C, is then slowly added to the water seat, injected at the impeller blades via a gravity-fed drop funnel.
• the mixer rpm is increased to about 1500 rpm during this addition.
• About 0.3 g of a CaCl2 solution (25%) is added to reduce viscosity of the mixture and the mixer rpm is reduced to about 1000 rpm.
• About 0.2 g of a 1.5% Kathon solution is added.
• the mixture is chilled in an ice water bath while still mixing. The mill is turned off at this point.
• Another 0.3 g of the 25% CaCl2 solution is added when the mixture temperature reaches about 27°C.
• the mixing is stopped when the batch temperature reaches about 24°C.
• Example IX The making procedure of Example IX is similar to that of Example VIII, except that about 12 g of an unemulsified 50 cSt PDMS is used instead of the 350 cSt PDMS emulsion.
• Composition XI is similar to that of Example X, except that about 7 g of an unemulsified PDMS containing about 4 mole % of [N-(2- a inoethyl)-3-aminopropyl]methyl siloxane comonomer is used instead of the (3- aminopropyDmethyl/dimethylsiloxane copolymer.
• This amino-functional silicone has a viscosity of from about 50 to about 90 cSt, and is available from Huls America, Piscataway, New Jersey.
• Composition XII is similar to that of Example X, except that about 7 g of Silwet® :-7001, a polyethyleneoxy/polypropyleneoxy/polydimethylsiloxane copolymer, is used.
• This alkoxylated silicone is available from Union Carbide Corporation, Danbury, Connecticut.
• This polyalkylenoxy PDMS derivative has a polydimethylsiloxane backbone, with some methyl groups replaced by C 3 H 6 ⁇

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• 1995
  • 1995-03-07 CA CA002184898A patent/CA2184898C/en not_active Expired - Fee Related
  • 1995-03-07 EP EP95912777A patent/EP0749469A1/de not_active Withdrawn
  • 1995-03-07 BR BR9507056A patent/BR9507056A/pt not_active Application Discontinuation
  • 1995-03-07 MX MX9604034A patent/MX9604034A/es unknown
  • 1995-03-07 WO PCT/US1995/002842 patent/WO1995024460A1/en not_active Application Discontinuation
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