EP0334430A2 - Abgeschreckte Weichspülerteilchenzusammensetzung - Google Patents

Abgeschreckte Weichspülerteilchenzusammensetzung Download PDF

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Publication number
EP0334430A2
EP0334430A2 EP89200662A EP89200662A EP0334430A2 EP 0334430 A2 EP0334430 A2 EP 0334430A2 EP 89200662 A EP89200662 A EP 89200662A EP 89200662 A EP89200662 A EP 89200662A EP 0334430 A2 EP0334430 A2 EP 0334430A2
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EP
European Patent Office
Prior art keywords
fabric softener
softener
particles
detergent
softener composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP89200662A
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English (en)
French (fr)
Other versions
EP0334430A3 (de
Inventor
Ralph Robert Royce
Bernard Karl Kremer
Paul David Bisio
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Procter and Gamble Co
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Procter and Gamble Co
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Filing date
Publication date
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Publication of EP0334430A2 publication Critical patent/EP0334430A2/de
Publication of EP0334430A3 publication Critical patent/EP0334430A3/de
Withdrawn legal-status Critical Current

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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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0052—Cast detergent compositions
    • 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
    • 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 fabric softener compositions which are included with detergent in the washing of fabrics.
  • the fabric softener survives the wash and releases softener to the fabrics in a heated laundry dryer.
  • fabric conditioning agents i.e., fabric softeners and/or antistatic agents
  • present inven­tion pertains to 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.
  • An object of the present invention is to provide a harder softener particulate which has a smooth surface without fissures.
  • Another object is to provide an improved process for making an improved and less sticky particulate fabric softener.
  • the present invention is directed to detergent-compatible, particulate, dryer-activated quench cooled cationic fabric softener having a differential penetration value of at least about 0.1 mm less than a comparable but nonquench cooled fabric softener composition.
  • the particulate fabric softener of the present invention preferably has at least one surface which is sub­stantially smooth or flat.
  • the smooth or flat surface area pref­erably ranges from about 10% to about 100% of the surface area of the particulate.
  • the present invention relates to an improved process for making particulate fabric softener, said process comprising quench cooling molten fabric softener via intimate contact with a solid cooling device.
  • the present invention is directed to detergent-compatible, dryer-activated fabric softening particles comprising a quench cooled cationic fabric softener composition.
  • This invention also relates to a quench cooled fabric softener process for preparing same.
  • the invention also relates to laundry detergent compo­sitions containing said quench cooled softener particles.
  • the quench cooled fabric softener composition can be added to the wash step of the fabric laundering process.
  • the process comprises quenching molten fabric softener on a cooling device.
  • the softener is formulated to survive the wash and is released to the fabrics in a heated laundry dryer.
  • the quench cooled, detergent-compatible, dryer-activated fabric softener composition of this invention comprises from about 70% to about 100% of fabric softener material, at least about 10% of which is a cationic fabric softener.
  • the quench cooled softener composition has a melting point of from about 40°C to about 80°C, preferably from about 45°C to about 60°C.
  • the quench cooled softener of the present invention is cooled by intimately contacting the molten fabric softener to a cooling device, pref­erably a moving belt cooler or a chilled rolls.
  • the molten fabric softener is metered onto the cooling device as a thin film or a particulate where it is solidified in a few seconds.
  • the molten fabric softener is applied to the cooling device as a thin film having a preferred thickness of from about 0.3 mm to about 6.4 mm, more preferably from about 0.4 mm to about 4.4 mm, and most preferably from about 0.5 mm to about 2.5 mm.
  • DSC differential scanning curve
  • Nonquench cooled softener can be made from molten fabric softener which is conventionally cooled solid in several minutes to several hours or cooled in a spray tower. In a conventional spray tower process, molten fabric softener is cooled quickly, however, such prills are distinguished from the quench cooled softeners of the present invention in that they are not in intimate contact with a solid cooling device.
  • the quench cooled softener of the present invention is harder than comparable prilled fabric softener.
  • the quench cooled softener composition of this invention has a differential penetration value of at least about 0.1 mm less than a comparable nonquench cooled softener composition.
  • the differ­ential penetration value can be less than 0.2 mm or less than about 0.4 mm.
  • Penetration values herein are measured by ASTM Test D-1321 modified by using a 100 gm weight.
  • Softener prills have numerous air holes and are much softer than the quench cooled and nonquench tray cooled softener because the latter two are more solid.
  • the quench cooled softener compositions of the present invention can have an absolute penetration value of up to about 2 mm, but preferably less than 1.5 mm, and more preferably about 1 mm or less.
  • the harder the soft­ener particle the better the handling of the particle for coating and packing purposes. The harder they are the less sticky and the better the handling.
  • the quench cooled fabric softener com­position can have from 0% to about 30% of a coating surrounding the particulate fabric softener composition.
  • the coating is preferably a substantially water-insoluble material having a melting point above about 35°C and a penetration value of about 0.6 mm or less.
  • the quench cooled fabric softener particles preferably have diameters of from about 100 microns to about 5,000 microns, pref­erably from about 300 microns to about 3,000 microns, and most preferably greater than about 500 microns up to about 2,000 microns, with a number average of from about 500 to about 1,200 microns.
  • the particles can be of a generally spherical shape, but can have an irregular cubical shape with one or more flat or smooth surfaces.
  • the particle sizes quoted herein refer to the largest dimension (diameter thickness or length) of the particle.
  • molten fabric softener is applied onto a quenching device having a temperature below the melting point of the softener composition.
  • the molten softener can be applied to the cooling device in the form of particles, ribbons, sheets, etc., whereby a heat exchange occurring between the cooling device and softener solidifies or quenches the molten softener solid.
  • This "quenching" effect on the softener composition is believed to provide a harder or more crystalline softener.
  • the quenched fabric softener has a greater area under its DSC curve than a comparable slow-cooled softener.
  • the process itself is more robust, more flexible than prill­ing, yet provides a superior softener product.
  • the particles made from the quenched fabric softener are more conducive to encapsulation.
  • the quench cooled softener has more flat surfaces than tray cooled softeners. The flat surfaces allow more efficient coating. The processing time is reduced and the yields are high. Some quench cooled processes provide softener particles which are more uniform in size.
  • the processing window is wider for the process of the present invention than for the processes of the prior art.
  • Glue guns, spray nozzles, etc. can be used to spray the molten softener onto the cooling device to achieve tailored quenched particles.
  • a weir or a similar device can be used to meter a sheet or a ribbon of molten softener onto the cooling device.
  • the solid softener can then ground to a tailored particle size.
  • An electronically controlled pastille-forming apparatus or a screen printer can be used to provide uniform softener particles.
  • Preferred cooling devices are steel belt coolers and chill rolls.
  • a preferred cooling device commercially available is a Sandvik Rotoform System comprising dropformers or weirs, and a rotating steel belt cooler (Sandvik Process Systems, Inc., Totowa, New Jersey 07512).
  • the cooling device must be capable of releasing the quenched cooled softener product via doctoring or some other separation means and is thus distinguished from substrate impreg­nated cooled softener.
  • 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.
  • the anionic group which can be the counter-ion in the quaternary compounds useful herein is typically a halide (e.g., chloride or bromide), nitrate, bisulfate, ethylsulfate, or methyl­sulfate.
  • a halide e.g., chloride or bromide
  • nitrate e.g., bisulfate, ethylsulfate, or methyl­sulfate.
  • the methylsulfate and chloride ions are the preferred counter-ions from an availability standpoint; while the methylsul­fate anion is most preferred because of its minimization of cor­rosive effects on the automatic clothes dryers in which it is used.
  • 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
  • the fabric softener is the core of particles and comprises from about 70% to about 97% and most preferably 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
  • the core has 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 coating materials are substantially water-insoluble materials, typically (but not necessarily) selected from waxy materials such as paraffinic waxes, microcrystall ine waxes, animal waxes, vegetable waxes, saturated fatty acids and fatty alcohols having from 12 to 40 carbon atoms in their alkyl chain, and fatty esters such as fatty acid triglycerides, fatty acid esters of sorbitan and fatty acid esters of fatty alcohols, or from sub­stantially water-insoluble polymers.
  • waxy materials such as paraffinic waxes, microcrystall ine waxes, animal waxes, vegetable waxes, saturated fatty acids and fatty alcohols having from 12 to 40 carbon atoms in their alkyl chain
  • fatty esters such as fatty acid triglycerides, fatty acid esters of sorbitan and fatty acid esters of fatty alcohols, or from sub­stantially water-insoluble polymers.
  • 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 preferred 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; urea-­formaldehyde 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
  • urea-­formaldehyde 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 surrounds the cationic fabric softener core and is present in an amount of from 0% to about 30%, preferably from about 3% to about 15% by weight of the particle.
  • 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.
  • Penetration values of a number of suitable coating materials are shown in the following table. TABLE 1 Penetration Values of Representative Coating Materials Material Penetration in mm Stearyl alcohol 0.57 Ethyl cellulose 0.09 Cellulose acetate 0.00 Ethyl cellulose + 10% dibutyl sebacate 0.00 70% Stearyl alcohol + 30% C30 alcohol 0.32 90% Stearyl alcohol + 10% Elvax-43101 0.12 90% Stearyl alcohol + 10% BE-Square-1952 0.40 1 Terpolymer of ethylene, vinyl acetate and acid from DuPont 2 Microcrystalline wax from Petrolite, Specialty Polymers Group
  • the function of the coating which surrounds the fabric softener is to prevent the softener from becoming dissolved and/or dispersed in the wash water when the particles are pres­ent during the wash step of a laundry process, and thereby prevent interaction between the fabric softener and the deter­gent.
  • a substan­tial amount of the particles adhere to, or become entrapped within folds of the fabrics.
  • the coating and the fabric softener core composition melt, thereby permitting the softener to spread throughout the fabric load and soften the fabrics.
  • 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 particles of softener composition are preferably coated with coating material which is either melted or dissolved in a volatile solvent.
  • the coating is done at a temperature which is below the melting point of the softener composition, and the coated particles are then cooled (or the solvent is evaporated) to solidify the coating.
  • the coating is typically applied in a fluid­ized bed type apparatus.
  • a suitable type of apparatus is that described in U.S. Pat. No. 3,196,827, Wurster et al., issued July 27, 1965, incorporated by reference herein.
  • solid softener core particles are suspended on an air stream which carries them in a smooth cyclic flow past the coating nozzle, which sprays them with fluid coating material.
  • the atomized coating fluid covers the surfaces of the core particles.
  • the coated particles are lifted on the air stream and the fluid coating solidifies on the surface of the particles as the air stream lifts them away from the nozzle.
  • the particles then settle out of the air stream and begin another cycle which takes them past the nozzle again.
  • the process is repeated until the desired amount of coating has been deposited on the particles.
  • the amount of coating applied to the softener core particles is typically from about 3% to about 30%, preferably about 3% to about 15% by weight of total particle (i.e., core plus coating).
  • 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 Jersey 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 Jersey 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.
  • the particles of the present invention are preferably formu­lated into detergent compositions.
  • Such compositions typically comprise detersive surfactants and detergency builders and, optionally, additional ingredients such as bleaches, enzymes, fabric brighteners and the like.
  • the particles are present in the detergent composition at a level sufficient to provide from about 0.5% to about 10%, and preferably from about 1% to about 5% of quaternary ammonium fabric softener in the detergent composition.
  • the remainder of the detergent composition will comprise from about 1% to about 50%, preferably from about 10% to about 25% detersive surfactant, and from about 15% to about 60%, preferably from about 20% to about 45% of a detergency builder, and, if desired, other optional laundry detergent components.
  • 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.
  • suitable organic alkaline detergency builder salts are: (1) water-soluble amino polyacetates, e.g., sodium and potassium ethylenediaminetetraacetates, nitrilotriacetates, and N-(2-hydroxyethyl)nitrilodiacetates; (2) water-soluble salts of phytic acid, e.g., sodium and potassium phytates; (3) water-­soluble polyphosphonates, including sodium, potassium and lithium salts of ethane-1-hydroxy-1,1-diphosphonic acid, sodium, potas­sium, and lithium salts of methylenediphosphonic acid and the like.
  • water-soluble amino polyacetates e.g., sodium and potassium ethylenediaminetetraacetates, nitrilotriacetates, and N-(2-hydroxyethyl)nitrilodiacetates
  • water-soluble salts of phytic acid e.g., sodium and potassium phytates
  • Seeded builders include such materials as sodium carbonate or sodium silicate, seeded with calcium carbonate or barium sulfate.
  • Optional detergent composition components include enzymes (e.g., proteases and amylases), halogen bleaches (e.g., sodium and potassium dichloroisocyanurates), peroxyacid bleaches (e.g., diperoxydodecane-1,12-dioic acid), inorganic percompound bleach­es (e.g., sodium perborate), activators for perborate (e.g., tetraacetylethylenediamine and sodium nonanoyloxybenzene sulfo­nate), soil release agents (e.g., methylcellulose) soil suspending agents (e.g., sodium carboxymethylcellulose) and fabric bright­eners.
  • enzymes e.g., proteases and amylases
  • halogen bleaches e.g., sodium and potassium dichloroisocyanurates
  • peroxyacid bleaches e.g., diperoxydodecane-1,12-dioic acid
  • the particles can be added to the wash solution in a sealed, porous water-insoluble pouch such as the type described in U.S. Pat. No. 4,223,029, Mahler et al., issued Sept. 16, 1980, incor­porated by reference herein.
  • Detergent granules can be included in the pouch with the softener particles.
  • Preferred pouch structures are multi-pouch porous sheet structures such as described in U.S. Pat. No. 4,638,907, Bedenk/Harden, issued Jan. 27, 1987, incor­porated herein by reference. A single pouch structure can also be used. Several examples are currently on the market.
  • Suitable pouch materials include, paper, nonwoven synthetics such as spunbonded and wet laid polyester, and porous formed film plastic sheet material.
  • Suitable formed plastic film material is disclosed in commonly assigned U.S. Pat. No. 4,679,643, Curro and Linman, issued Dec. 16, 1986. Said film has finely divided apertures smaller than most of the particulate materials inside and is capable of surviving the wash and dryer temperatures.
  • Molten fabric softener which has a melting point of about 54°C is prepared using the following formula: Ingredient Wt. % Ditallowdimethylammonium methylsulfate (DTDMAMS) 44 Sorbitan monostearate 22 Cetyl alcohol 22 Syloid® 234 (silica gel) 12 Total 100
  • 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 Ross Versamix mixer (Charles Ross & Sons Company, Hauppauge, New York 11788).
  • the temperature of the triblend is then raised to 79°-85°C under vacuum (about 330-430 mm Hg).
  • the Ross anchor and disperser are turned on and the Syloid 234 is added.
  • the mixture is blended for 5 minutes and then sheared with the Ross colloid mixer for 20 minutes. (Some of the molten softener composition is poured into trays and cooled overnight in a 4°C room. Thickness: 1.5 mm. This is used as a control.)
  • the molten softener mixture is transferred or pumped to the head of a steel belt cooler via heated piping.
  • the softener is placed on the moving steel belt cooler, a Sandvik Process System belt (Sandvik Process Systems, Inc., Totowa, NJ 07512) directly from the piping, via a distribution bar or a distribution piping across the width of the belt.
  • a weir is used to meter the molten softener in the form of a 0.06 inch (1.5 mm) thick film onto the moving cooled belt.
  • the belt is cooled via waterjets underneath the belt.
  • the temperature range in the first meter zone is from 32°-38°C, the second zone from 20°-32°C, and the third zone from 10°-20°C and combinations. Each zone is about 5 meters.
  • the length of the belt is 18 meters.
  • the belt is moving at a rate of about 40 feet (13 meters/min.) per minute, but can be adjusted to a rate of from about 30 to 80 feet per minute (9 to 25 meters per minute).
  • the molten softener becomes solid film in about 40 seconds.
  • the film of softener traveling along the belt is quenched below its melting point, in this case the quenching temperature is below 32°C.
  • the object is to quench the softener while main­taining intimate contact between the softener and the belt. Separation of the softener (curling up) by instantaneous quench­ing still produces a superior softener product.
  • Quench cooled softener is released from the cooling belt by a doctoring device at the end of the belt and is delivered to a prebreaker, which breaks the solidified film into particles less than 4 inches (10.16 cm) in diameter.
  • quench cooled softener is taken after being doctored off the belt but before prebreaking the sample to measure the hardness of the softener film.
  • the quench cooled softener of this example had a penetration value of about 0.8 mm and the above-mentioned overnight cooled controlled fabric softener had a penetration value of about 1 mm. A 0. 1 mm difference penetration is a significant difference.
  • the solid quenched softener prebreak is then converted to particles by milling in a Fitzmill, Model DAS06 (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 particles of this example are cubical in shape with one or two flat sur­faces. There are little or no fissures on the particle surfaces.
  • Example I To improve the hot water wash survivability of the softener, the particles of Example I are coated with a hot melt of fatty alcohol-based coating.
  • the coating is a mixture of 90% stearyl alcohol and 10% Elvax-4310, a terpolymer of ethylene, vinyl acetate and acid from E.I. du Pont de Nemours & Co., Polymer Products Dept., 1007 Market St., Wilmington, Delaware 19898.
  • the coating is applied in an 18 Inch Wurster coater (Coating Place, Inc., P.O. Box 248, Verona, Wisconsin 53593). A de­tailed description of this type of equipment can be found in U.S. Pat. No. 3,196,827, supra , incorporated by reference herein.
  • 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 quench cooled 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 quench cooled softener particles is about 15% by weight of the total coated particle.
  • the par­ticles are resized through 12 on 20 mesh and are then ready for use "as is” or for blending into detergent granules.
  • Quench cooled softener core particles prepared as in Example I are coated with ethyl cellulose based coating instead of fatty alcohol.
  • the particles are coated with a 10% solution of Ethocel in methanol.
  • the coating is applied in an 18 inch Wurster Coater (Coating Place, Inc., P.O. Box 248, Verona, Wisconsin 53593).
  • the ethyl cellulose used is Ethocel Std. 10 (Dow Chemical Co., Midland, Michigan 48640), which has an Ubbelohde viscosity of 9.0-11.0, measured at 25°C as a 5% solution in 80% toluene/20% ethanol.
  • the amount of ethyl cellulose solids coated onto the particles is about 3% by weight of the total coated particle weight.
  • the softener particles are resized through 11 on 26 Mesh U.S. Standard screens and are then ready for use "as is” or for blending into detergent granules.
  • a granular detergent/softener composition is prepared by mixing 4 parts of the quench cooled softener particles of either Example I, II or III with 96 parts of the following granular detergent composition.
  • Ingredient Wt.% Sodium C13 linear alkylbenzene sulfonate 16.5 Sodium C14-C15 linear fatty alcohol sulfate 16.5 Sodium sulfate 23.8 Sodium silicate 9.2
  • Polyacrylic acid 1.3
  • Sodium tripolyphosphate 13.7 Sodium carbonate 4.8 Methyl cellulose 3.6
  • Optical brightener 1.3
  • Protease enzyme 1.6 Moisture and miscellaneous 6.8 Total 100.0
  • a granular bleach/softener composition is prepared by mixing 4 parts of the quench cooled softener particles of either 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/quench cooled softener composition of Example III and the four pouches in between containing about 15.5 grams each of the detergent/­quench cooled 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 approximately 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 III and the four pouches in between are filled with about 15.5 grams of the detergent/ethylcellulose coated softener composition of Example III.
  • 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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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
EP19890200662 1988-03-24 1989-03-16 Abgeschreckte Weichspülerteilchenzusammensetzung Withdrawn EP0334430A3 (de)

Applications Claiming Priority (2)

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US17268188A 1988-03-24 1988-03-24
US172681 1988-03-24

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008009521A1 (de) * 2006-07-20 2008-01-24 Henkel Ag & Co. Kgaa Verfahren zur herstellung einer festen, textil-weichmachenden zusammensetzung
US10301575B2 (en) 2015-04-14 2019-05-28 The Procter & Gamble Company Consumer product composition comprising a polyethylene glycol carrier with silicone particles dispersed therein
US10329519B2 (en) 2016-10-19 2019-06-25 The Procter & Gamble Company Consumer product composition comprising a polyethyleneglycol carrier, silicone conditioner, and particulate spacer material

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4196104A (en) * 1977-09-26 1980-04-01 The Procter & Gamble Company Process for producing antistatic, fabric-softening detergent composition
US4395342A (en) * 1980-06-06 1983-07-26 The Procter & Gamble Company Granular fabric softening composition
US4638907A (en) * 1984-11-28 1987-01-27 The Procter & Gamble Company Laminated laundry product
EP0269179A1 (de) * 1986-11-24 1988-06-01 The Procter & Gamble Company Verträgliches Detergens, beim Trocknen freigesetzte, Gewebe weichmachende/antistatische Mittel
US4889643A (en) * 1988-05-05 1989-12-26 The Procter & Gamble Company Quench cooled particulate fabric softening composition
US5002681A (en) * 1989-03-03 1991-03-26 The Procter & Gamble Company Jumbo particulate fabric softner composition

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008009521A1 (de) * 2006-07-20 2008-01-24 Henkel Ag & Co. Kgaa Verfahren zur herstellung einer festen, textil-weichmachenden zusammensetzung
US10301575B2 (en) 2015-04-14 2019-05-28 The Procter & Gamble Company Consumer product composition comprising a polyethylene glycol carrier with silicone particles dispersed therein
US10329519B2 (en) 2016-10-19 2019-06-25 The Procter & Gamble Company Consumer product composition comprising a polyethyleneglycol carrier, silicone conditioner, and particulate spacer material

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