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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
  • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
  • C11D17/047—Arrangements specially adapted for dry cleaning or laundry dryer related applications
• • 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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
• • 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

Definitions

• the invention pertains to coated particles of fabric softener which are included with detergent in the washing of fabrics.
• the particles survive the wash and release softener to the fabrics in a heated laundry dryer.
• fabric conditioning agents i.e., fabric softeners and/or antistatic agents
• present inven­tion pertains to coated particulate softener/antistatic compositions which survive the wash process and release the active softening/­antistatic agent to the laundered fabrics in the dryer.
• Fabric softening and antistatic benefits are a desirable part of the laundry process.
• Softening and antistatic compounds are, in general, quaternary ammonium compounds that are not compatible with anionic surfactants. These compounds will be referred to hereinafter as fabric softening compounds or fabric softeners, although it is to be understood that they deliver both softening and antistatic benefits to fabrics.
• the opposite electrical charge of the anionic surfactant used in most detergents and the quaternary ammonium fabric softening compounds leads to a mutual attraction which causes precipitation. This, in effect, removes surfactant and fabric softener from solution and reduces the cleaning capacity of the detergent while preventing effective fabric softener deposition on the fabric.
• microcapsules survive the wash and adhere to the fabric surface. They are then ruptured by subsequent tumbling of the fabric in the dryer, thereby releasing softener to the fabrics.
• the present invention is directed to detergent-compatible, dryer-activated fabric softening particles having diameters of from about 5 microns to about 1,200 microns comprising an inner core of a fabric softener composition comprising a cationic fabric softener compound, and an outer coating comprised of water-­insoluble material having a melting point above about 35°C.
• the particles can be incorporated into laundry detergents.
• the present invention relates to coated fabric softener particles which can be added to the wash step of the fabric laundering process and which release softener to fabrics in a laundry dryer.
• the invention also relates to laundry detergent compositions containing said particles.
• the particles of the present invention comprise an inner core of a fabric softener composition which comprises a cationic fabric softener, and an outer coating which completely surrounds the core and comprises a substantially water-insoluble material having a melting point above 35°C, preferably above 50°C.
• substantially water-insoluble herein is meant having a solubility in 35°C water of less than about 50 ppm.
• the particles have diameters of from about 5 microns to about 1,200 microns, pref­erably greater than about 500 microns, and most preferably greater than about 600 microns, with a number average of from about 900 to about 1,000 microns.
• the particles typically will be of a generally spherical shape, but can also have an irregular shape.
• the particle sizes quoted herein refer to the largest dimension (diameter or length) of the particle.
• Typical cationic fabric softeners useful herein are quaternary ammonium salts of the formula [R1R2R3R4N]+Y ⁇ wherein one or two of R1, R2, R3 and R4 groups is an organic radical containing a group selected from a C12-C22 aliphatic radical or an alkylphenyl or alkylbenzyl radical having from 10 to 16 carbon atoms in the alkyl chain, the remaining groups being selected from C1-C4 alkyl, C2-C4 hydroxyalkyl and cyclic structures in which the nitrogen atom in the above formula forms part of the ring, and Y constitutes an anionic radical such as halide, nitrate, bisulfate, methylsulfate, ethylsulfate and phos­phate, to balance the cationic charge.
• R1, R2, R3 and R4 groups is an organic radical containing a group selected from a C12-C22 aliphatic radical or an alkyl
• the hydrophobic moiety i.e., the C12-C22 aliphatic, C10-C16 alkyl phenol or alkylbenzyl radical
• the organic radical R1 or R2 may be directly attached to the quaternary nitrogen atom or may be indirectly attached thereto through an amide, ester, alkoxy, ether, or like grouping.
• the quaternary ammonium compounds useful herein include both water-soluble compounds and substantially water-insoluble compounds which are dispersible in water.
• imidazolinium compounds of the structure wherein R is a C16 to C22 alkyl group possess appreciable water solubility, but can be utilized in the present invention.
• the quaternary ammonium softener compounds used in this invention can be prepared in various ways well-known in the art and many such materials are commercially available.
• the quat­ernaries are often made from alkyl halide mixtures corresponding to the mixed alkyl chain lengths in fatty acids.
• the ditallowalkyl quaternaries are made from alkyl halides having mixed C14-C18 chain lengths. Such mixed di-long chain quater­naries are useful herein and are preferred from a cost stand­point.
• quaternary ammonium softening compounds suitable for use in the present invention. All the quaternary ammonium compounds listed can be included in the present invention, but the compilation of suitable quaternary compounds hereinafter is only by way of example and is not intended to be limiting of such compounds.
• Dioctadecyldi­methylammonium methylsulfate is an especially preferred fabric softening compound for use herein, by virtue of its high anti­static, as well as fabric softening activity; ditallowalkyldi­methylammonium methylsulfate is equally preferred because of its ready availability and its good antistatic activity; other useful di-long chain quaternary compounds are dicetyldimethylammonium chloride, didocosyldimethylammonium chloride, didodecyldimethyl­ammonium chloride, ditallowalkyldimethylammonium bromide, diole­oyldimethylammonium methylsulfate, ditallowalkyldiethylammonium chloride, ditallowalkyldipropylammonium bromide, ditallowalkyl­dibutylammonium fluoride, cetyldecylmethylethylammonium chloride, bis-[dit
• Particularly preferred quaternary ammonium fabric softening compounds are ditallowal­kyldimethylammonium chloride and ditallowalkyldimethylammonium methylsulfate.
• the fabric softener core of the particles of the invention comprises from about 70% to about 97% and most preferivelyably about 85% to about 97% of the particle. All percentages herein are "by weight” unless otherwise indicated.
• the core composition can consist entirely of cationic fabric softeners, and will generally comprise at least 10%, usually 10% to 50% cationic fabric softener.
• the core can contain additional materials such as perfume, auxiliary fabric softening agents (e.g., smectite clay, fatty alcohols and fatty amine, such as ditallowmethyl amine or 1-tallowamidoethyl-2-tallow­imidazoline), soil release agents, fabric brighteners, etc.
• auxiliary fabric softening agents e.g., smectite clay, fatty alcohols and fatty amine, such as ditallowmethyl amine or 1-tallowamidoethyl-2-tallow­imidazoline
• Typical specific suitable waxy coating materials include lauric, myristic, palmitic, stearic, arachidic and behenic acids, stearyl and behenyl alcohol, micro­crystalline wax, beeswax, spermaceti wax, candelilla wax, sor­bitan tristearate, sorbitan tetralaurate, tripalmitin, trimyristin and octacosane.
• a prefered waxy material is stearyl alcohol.
• water-insoluble polymeric materials which may be used for the coating of the particles herein are cellulose ethers such as ethyl, propyl or butyl cellulose; cellulose esters such as cellulose acetate, propionate, butyrate or acetate-butyrate; urea­formaldehyde resins, polyvinyl chloride, polyvinylidene chloride, polyethylene, polypropylene, polyacrylates, polymethacrylates, polymethyl-methacrylates and nylon.
• cellulose ethers such as ethyl, propyl or butyl cellulose
• cellulose esters such as cellulose acetate, propionate, butyrate or acetate-butyrate
• urea­formaldehyde resins polyvinyl chloride, polyvinylidene chloride, polyethylene, polypropylene, polyacrylates, polymethacrylates, polymethyl-methacrylates and nylon.
• a preferred polymeric material is ethyl cellulose.
• the polymeric coating materials can be plasticized with known plasticizing agents such as phthalate, adipate and sebacate esters, polyols (e.g., ethylene glycol), tricresyl phosphate, castor oil and camphor.
• the coating material can comprise a mixture of waxy coating materials and polymeric coating materials.
• the waxy coating material will typically comprise from about 70% to about 90% of the mixture and the polymeric material about 30% to about 10%.
• the coating material will have a hardness which corresponds to a needle penetration value of about 0.6 mm or less, and preferably less than about 0.1 mm, as measured by ASTM Test D-1321, modified by using a 100g weight instead of a 50g weight. The test is performed at 25-27°C.
• sample preparation is accomplished by dissolving the polymer in a volatile solvent and then evaporating the solvent after the polymer solution has been placed in the test container.
• sample preparation is done by melting the sample and then solidifying it in the test container in the manner set forth in the ASTM method.
• the particle size of the softener particles be similar to the particle size of the detergent granule in order to minimize segregation. This will typically be in the range of from about 500 to about 1000 microns.
• Softener particles which are smaller in size than the detergent granules can be agglomerated to form larger particles to match the particle size of the detergent granules into which they will be incorporated.
• the agglomeration can be accomplished by using water-soluble or dispersible materials such as polyvinyl alcohol, sodium carboxy­methyl cellulose, gelatin and polyoxyethylene waxes.
• the agglom­erates disintegrate when the detergent composition is added to water.
• the softener particles are fed to a highly efficient mixer (e.g., Schugi Flexomix Model 160,335 or 400 from Schugi Process Engineers USA, 41-T Tamarack Circle, Skillman, New Jersy 08558), or a pan agglom­erator.
• a highly efficient mixer e.g., Schugi Flexomix Model 160,335 or 400 from Schugi Process Engineers USA, 41-T Tamarack Circle, Skillman, New Jersy 08558
• Aqueous solution or dispersion of agglomerating agent is sprayed onto the moving particles causing them to stick to each other.
• the water is evaporated and the dried agglomerated particles are sized by sieving.
• Suitable agglomerating agents include dextrin starches, Pluronic Polyols (copolymers of ethylene oxide and/or propylene oxide with either ethylene glycol or propylene glycol) and hydratable salts such as sodium tripoly­phosphate or sodium sulfate.
• Surfactants useful in the detergent compositions herein include well-known synthetic anionic, nonionic, amphoteric and zwitterionic surfactants. Typical of these are the alkyl benzene sulfonates, alkyl- and alkylether sulfates, paraffin sulfonates, olefin sulfonates, alkoxylated (especially ethoxylated) alcohols and alkyl phenols, amine oxides, alpha-sulfonates of fatty acids and of fatty acid esters, alkyl betaines, and the like, which are well known from the detergency art. In general, such detersive surfactants contain an alkyl group in the C9-C18 range.
• the anionic detersive surfactants can be used in the form of their sodium, potassium or triethanolammonium salts; the nonionics generally contain from about 5 to about 17 ethylene oxide groups. C11-C16 alkyl benzene sulfonates, C12-C18 paraffin-sulfonates and alkyl sulfates are especially preferred in the compositions of the present type.
• Useful detergency builders for the detergent compositions herein include any of the conventional inorganic and organic water-soluble builder salts, as well as various water-insoluble and so-called “seeded” builders.
• Nonlimiting examples of suitable water-soluble, inorganic alkaline detergent builder salts include the alkali metal carbo­nates, borates, phosphates, polyphosphates, tripolyphosphates, bicarbonates, silicates, and sulfates.
• Specific examples of such salts include the sodium and potassium tetraborates, bicarbonates, carbonates, tripolyphosphates, pyrophosphates, and hexameta­phosphates.
• Seeded builders include such materials as sodium carbonate or sodium silicate, seeded with calcium carbonate or barium sulfate.
• Preferred pouch structures are multi-pouch porous sheet structures such as described in application U.S. Ser. No. 675,804, Bedenk et al., filed Nov. 28, 1984, now U.S. Pat. Nos. 4,638,907, Bedenk/Harden, issued Jan. 27, 1987; and U.S. Pat. No. 4,259,383, Eggensperger et al., issued Mar. 31, 1981, both incorporated herein by reference.
• the particles tend to collect in a relatively small area of the structure, whereas in a multi-pouch sheet structure the softener particles are distributed over a larger area of the structure thereby facilitating more even transfer of softener to fabrics in the dryer.
• Suitable pouch materials include, paper, nonwoven synthetics such as spunbonded and wet laid polyester, and porous formed film plastic sheet material.
• the individual pouches have a water-insoluble baffling means which provides some standoff between the interior major surfaces of the pouches while the multi-pouch sheet is being tumbled in the clothes dryer.
• the standoff prevents the interior major surfaces of each pouch from coming into intimate contact with each other during the drying cycle, thereby reducing the ten­dency of the molten softener to be squeezed out of the pouch during the drying cycle, which can cause fabric staining.
• the molten softener be permitted to gradually wick through the substrate and thereby gradually transfer to the tumbling fabrics.
• the baffling can be produced, for example, by printing a cross hatched glue pattern on one of the interior surfaces of the pouch material or by including a layer of poly­meric net material between the interior major surfaces of the pouches.
• Fabric softener core particles are prepared according to the following formula:
• the DTDMAMS is heated in a reaction vessel at 71°C under vacuum (Ca. 710 mm Hg) for 4 hours to remove residual moisture and/or isopropanol.
• the cetyl alcohol and sorbitan monostearate are then added, and the molten "triblend" is mixed for one hour at about 71°C.
• the triblend is transferred into a PVM 40 Ross mixer (Charles Ross & Sons Company, Hauppauge, New York 11788).
• the temperature of the triblend is then raised to 79°C - 85°C under vacuum (about 330-430 mm Hg).
• the Ross' anchor and disperser are turned on and the clay is added.
• the mixture is blended for 5 minutes and then sheared with the Ross' colloid mixer for 20 minutes.
• the perfume is then added and the mixture is blended for 5 minutes with the anchor, disperser and colloid mill still on.
• the softener composition is then poured into trays and cooled overnight at about 4°C.
• the solid softener core composition is then converted to particles by milling in a Fitzmill, Model DA506 (The Fitzpatrick Company, Elmhurst, Illinois 60126) at 4740 rpm's through a 4 mesh screen.
• the particles are then sized through 12 on 30 (U.S. Standard screens, 1.7 - 0.6 mm particle size).
• the Wurster Coater consists of an apparatus that is capable of suspending the softener core particles on a rapidly moving warm air stream. Encapsulation is accomplished by pass­ing the softener particles through a zone of finely atomized droplets of coating. As the particles move up and away from the coating nozzle, the coating begins to solidify as the particles cool. When the particles can no longer be fluidized by the air stream, they move down in the opposite direction of the fluidizing air. The coated particles then reenter the coating zone and are recycled until the desired amount of coating is applied. The coating cycle takes place within a single chamber which preferably has a partition to separate the particles moving up through the coating zone from those moving down through the cooling zone.
• the amount of fatty alcohol coating applied to the softener particles is about 15% by weight of the total coated particle. After the coating process is complete the particles are resized through 12 on 20 mesh and are then ready for use "as is” or for blending into detergent granules.
• the amount of ethyl cellulose/dibutyl sebacate solids coated onto the particles is about 5% by weight of the total coated particle weight.
• the softener particles are resized through 12 on 30 Mesh U.S. Standard screens and are then ready for use "as is” or for blending into detergent granules.
• a fabric softener core particle containing perfume capsules is prepared according to the following formula:
• the perfume capsules are prepared using a complex coacer­vation process as described in U.S. Pat. 3,697,437, supra . Briefly, the process is as follows.
• the following components are each preheated to 52°C and combined: 1000 mls of deionized water, 1000 mls of a 10% by weight solution of gelatin in deionized water (King & Knox Type A gelatin, 275 Bloom) and 1000 mls of a water-insoluble perfume.
• the solution is then emulsified via agitation at 52°C.
• the agitation speed is adjusted such that the mean particle size of the droplets is between 100 and 200 microns.
• the solution is then cooled to ambient over a 2-3 hour period with constant stirring.
• the solution is then cooled further to 5-10°C before adding 50 mls of 25% glutaraldehyde solution to chemically harden the capsule wall.
• the glutaraldehyde is allowed to react for at least 4 hrs. while the solution temperature is slowly raised to ambient.
• the triblend is transferred into a PVM 40 Ross mixer (Charles Ross & Sons Company, Hauppauge, New York 11788).
• the temperature of the triblend is then raised to 79°C - 85°C under vacuum (about 330-430 mm Hg).
• the Ross' anchor and disperser are turned on and the clay is added.
• the mixture is blended for 5 minutes and then sheared with the Ross' colloid mixer for 20 minutes.
• the perfume capsules are then added and the mixture is blended for 10 minutes with only the anchor on at its lowest speed.
• the softener composition is then poured into trays and cooled overnight at about 4°C.
• the solid softener core composition is then converted to particles by milling in a Fitzmill, Model DA506 (The Fitzpatrick Company, Elmhurst, Illinois 60126) at 4740 rpm's through a 4 mesh screen.
• the particles are then sized through 12 on 30 (U.S. Standard screens, 1.7 - 0.6 mm particle size).
• the softener particles are then coated with a 5% level of a blend of 90% Ethocel 10 and 10% Ethocel 45 (Dow Chemical Co., Midland, Michigan 48640).
• the Ethocel 10 has a Ubbelhhode viscosity betwen 9-11 and the Ethocel 45 has a viscosity of 41-49, as measured as a 5% solution in 80% toluene and 20% ethanol.
• a granular detergent/softener composition is prepared by mixing 4 parts of the coated softener particles of Example I, II or III with 96 parts of the following granular detergent composition.
• a granular bleach/softener composition is prepared by mixing 4 parts of the coated softener particles of Example I, II or III with 96 parts of the following granular bleach composition.
• a laundering article in the form of a multipouch sheet is prepared as follows.
• the sheet is comprised of two sheets of Reemay® 2420 spun­bonded polyester (DuPont, Wilmington, Delaware). In between the sheets is a honeycomb web made from polyethylene.
• the web has a thickness of approximately 0.04 inch (0.10 cm) and the cells of the web are diamond shaped, having a cross dimension of approximately 0.19 inch (0.48 cm) and a length dimension of approximately 0.63 inch (1.60 cm).
• the three-layered structure has outer edge dimensions of approximately 4.5 inches x 11 inches (11.4 cms x 27.9 cms).
• the structure is laminated together in a pattern so as to form six equal sized pouches, two pouches at each end containing about 14.7 grams each of the bleach/ethyl cellulose coated softener composition of Example V and the four pouches in between containing about 15.5 grams each of the detergent/ethyl cellulose coated softener composition of Example IV.
• the article is suitable for washing and softening laundry in a process involving washing and rinsing the fabrics, followed by tumble drying in a heated clothes dryer, wherein the article remains with the laundry throughout the entire process.
• Example VI This example is the same as Example VI, except that (1) the softener and detergent levels are, respectively, 2.2 parts and 97.8 parts, (2) the softener and bleach levels are, respectively, 2.6 parts and 97.4 parts; and (3) the multipouched sheet is comprised of a top sheet of a latex bonded, wet laid polyester/­wood pulp substrate (James River 5227, James River Corp., Greenville, South Carolina) and an embossed sheet of Reemay® 2420, a spunbonded polyester (Dupont, Wilmington, Delaware). The two sheets are laminated together with an outer edge dimen­sion of approximaely 4.5 inches x 11 inches (11.4 x 27.9 cms) and with a pattern so as to form six equal sized pouches.
• a latex bonded, wet laid polyester/­wood pulp substrate James River 5227, James River Corp., Greenville, South Carolina
• Reemay® 2420 a spunbonded polyester
• the two pouches at each end are filled with about 14.7 grams of the bleach/ethyl cellulose coated softener composition of Example V and the four pouches in between are filled with about 15.5 grams of the detergent/ethylcellulose coated softener composition of Example IV.
• the porous substrates may not be able to contain the dust adequately.
• a wetting agent selected from suitable, relatively nonvolatile, organic liquids like water, surfactant solutions, propylene or ethylene glycol, light oils, liquid polyethylene glycols, nonionic surfactants, etc., capable of forming and maintaining a tacky surface on the detergent powder particles.
• Said liquid should not be capable of forming, by itself, a barrier of any type between the substrate and the detergent composition.
• the portion of the substrate that defines the pouch that contains the detergent powder is sprayed with an effective amount, typically from about 0.01 gram to about 0.2 gram per square inch, preferably from about 0.04 gram to about 0.1 gram per square inch, of said wetting agent.
• the detergent powder is added to the detergent pouch before the wetting agent evaporates or otherwise disappears.
• the tacky detergent powder then obstructs, at least partially, the pores of the substrate, and thus minimizes the escape of the very fine detergent powder particles (dust).
• the porous substrate in this Example is coated with approximately 0.06 gram per square inch of organic liquid (propylene glycol) and, before it dries, the detergent powder is added to the sheet.
• the finished article is suitable for washing and softening laundry in a process involving washing and rinsing the fabrics, followed by tumble drying in a heated clothes dryer, wherein the article remains with the laundry throughout the entire process.

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Citations (6)

• 1987
  • 1987-11-17 EP EP87202258A patent/EP0269179A1/de not_active Withdrawn
  • 1987-11-23 CA CA000552511A patent/CA1284560C/en not_active Expired - Fee Related

Patent Citations (6)

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