Method for forming particles

Abstract

A method for forming particles. The method includes the step of entraining a gas into a precursor material, wherein the gas includes about 50% to about 100% by volume of argon and about 0% to about 50% by volume of other components. The precursor material is deposited onto a moving conveyor. The precursor material is cooled to form a plurality of particles.

Description

Technical Field

[0001] Method for forming particles. Background Art

[0002] Consumers desire products that simplify the process they use to wash their clothes, help them reduce the time they spend handling dirty clothes, and help them achieve a high level of benefits. Consumers are well positioned to understand the amount of fabric care composition required to provide their desired benefits. Therefore, fabric care products that enable consumers to customize the amount of fabric care composition they use are welcomed by many consumers.

[0003] Fabric care products that can be delivered in the wash are particularly easy to use for consumers. For example, a consumer can simply place the fabric care product with the clothes in the tub of a washing machine and start a washing machine cycle.

[0004] Typically, consumers use fabric care detergent compositions containing significant amounts of surfactants and other cleaning ingredients. Such fabric care compositions are typically provided in soluble unit dose bags containing a specified amount of fabric care actives. Fabric care compositions are also provided in liquid or powder form, and consumers are provided with measuring cups to provide a measured amount of fabric care composition. These types of products may be referred to as fully formulated fabric care compositions.

[0005] In order to provide the above fabric care benefits and fabric care benefits beyond those that can be provided by using fully formulated fabric care compositions, fabric care products as additives are welcomed by consumers. Consumers enjoy and feel satisfied by using fabric care additives that are packaged in a manner that enables the consumer to use a customized amount of fabric care additive based on the consumer's judgment of how much fabric care additive is needed to provide the desired benefit. Such fabric care additives are conveniently provided with the fully formulated fabric care composition through the wash, but are metered separately from the fully formulated fabric care composition.

[0006] Fabric care additives in particle form are attractive to many consumers. Some fabric care additive particles are provided with a porous structure. When forming a wash liquor, the particles with a porous structure can float in the water. Compared with sinking particles, floating particles may be easy to dissolve more completely in the wash, because sinking particles may be caught in the wrinkles, creases and pockets of clothing during washing. Undissolved particles tend to incompletely deliver the fabric care beneficial active agents contained in the particles, which may be undesirable to consumers. Floating particles including unencapsulated spices can provide a pleasant fragrance to the head space above the wash liquor and the room where the washing machine is located. In addition, floating particles can better distribute fabric care additives to clothing during the wash cycle.

[0007] Melt processing is a common method for forming particles. A problem with preparing porous particles via a melt process is that when the molten precursor material solidifies, the bubbles in the melt tend to coalesce and rise from the molten material. This can result in larger holes at or near the outer surface of the particle, irregular rough outer surfaces, irregular distribution of pore sizes in the solidified particles, and the ejection of bubbles and molten material from the particle surface when the particles solidify. The durability of such particles may not be as good as particles with a more solid outer surface, and they are easily powdery, messy to use, and appear to be of poor quality. When the molten precursor material solidifies, the tendency of bubbles in the melt to coalesce and rise from the molten material can also effectively limit the volume of holes that can be provided in the particles without these adverse consequences.

[0008] In view of these limitations, there is a continuing unmet need for fabric care additives in particulate form having a uniform pore size distribution throughout the particle. There is also a need for a process for forming such porous particles. Summary of the invention

[0009] A method for forming particles includes the following steps: providing a precursor material to a feed tube; entraining a gas into the precursor material, wherein the gas comprises about 50 volume % to about 100 volume % argon and about 0 volume % to about 100 volume % other components; providing a distributor including a plurality of holes; conveying the precursor material from the feed tube to the distributor; passing the precursor material through the holes; providing a movable conveying device below the holes; depositing the precursor material onto the movable conveying device; and cooling the precursor material to form a plurality of particles. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 A device for forming particles.

[0011] Figure 2 Part of an apparatus for forming particles.

[0012] Figure 3 is an end view of an apparatus for forming particles.

[0013] Figure 4 Part of an apparatus for forming particles. DETAILED DESCRIPTION

[0014] Water soluble carrier

[0015] The particles and thus the precursor material as described below may comprise a water soluble carrier. The water soluble carrier may be a water soluble polymer. The water soluble carrier is used to carry the capsules into the wash liquor. When the water soluble carrier dissolves, the capsules are dispersed into the wash liquor and deposited onto the clothes.

[0016] The water-soluble carrier may be a material that dissolves in the wash liquor within a short period of time, for example, less than about 10 minutes.

[0017] Water soluble means that the material, carrier material or particle is soluble or dispersible in water, and optionally has a water solubility of at least 50%, optionally at least 75% or even at least 95% measured by the method described below, using a glass filter with a maximum pore size of 20 microns: 50 grams ± 0.1 grams of carrier are added to a pre-weighed 400 mL beaker, and 245 mL ± 1 mL of distilled water are added. On a magnetic stirrer set at 600 rpm, it is vigorously stirred for 30 minutes. The mixture is then filtered through a porous glass filter with the above-specified pore size (maximum 20 microns). This step is performed at a temperature of 23°C ± 1.0°C and a relative humidity of 50% ± 2%. The water in the collected filtrate is dried by any conventional method, and the weight of the remaining material (the dissolved or dispersed portion) is determined. Then, the percentage of solubility or dispersibility can be calculated.

[0018] The water-soluble carrier may be selected from water-soluble inorganic alkali metal salts, water-soluble alkaline earth metal salts, water-soluble organic alkali metal salts, water-soluble organic alkaline earth metal salts, water-soluble carbohydrates, water-soluble silicates, water-soluble urea, and any combination thereof.

[0019] The alkali metal salt can be, for example, selected from lithium salts, sodium salts and potassium salts and any combination thereof. Useful alkali metal salts can be, for example, selected from alkali metal fluorides, alkali metal chlorides, alkali metal bromides, alkali metal iodides, alkali metal sulfates, alkali metal hydrogen sulfates, alkali metal phosphates, alkali metal monohydrogen phosphates, alkali metal dihydrogen phosphates, alkali metal carbonates, alkali metal monohydrogen carbonates, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbates and combinations thereof.

[0020] The alkali metal salt can be selected from sodium fluoride, sodium chloride, sodium bromide, sodium iodide, sodium sulfate, sodium bisulfate, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, sodium carbonate, sodium bicarbonate, sodium acetate, sodium citrate, sodium lactate, sodium tartrate, sodium silicate, sodium ascorbate, potassium fluoride, potassium chloride, potassium bromide, potassium iodide, potassium sulfate, potassium bisulfate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, potassium carbonate, potassium monohydrogen carbonate, potassium acetate, potassium citrate, potassium lactate, potassium tartrate, potassium silicate, potassium, ascorbic acid and combinations thereof.

[0021] The alkaline earth metal salt can be selected from magnesium salt, calcium salt, etc. and combinations thereof. The alkaline earth metal salt can be selected from alkali metal fluoride, alkali metal chloride, alkali metal bromide, alkali metal iodide, alkali metal sulfate, alkali metal hydrogen sulfate, alkali metal phosphate, alkali metal monohydrogen phosphate, alkali metal dihydrogen phosphate, alkali metal carbonate, alkali metal monohydrogen carbonate, alkali metal acetate, alkali metal citrate, alkali metal lactate, alkali metal pyruvate, alkali metal silicate, alkali metal ascorbate and combinations thereof. The alkaline earth metal salt can be selected from magnesium fluoride, magnesium chloride, magnesium bromide, magnesium iodide, magnesium sulfate, magnesium phosphate, magnesium monohydrogen phosphate, magnesium dihydrogen phosphate, magnesium carbonate, magnesium monohydrogen carbonate, magnesium acetate, magnesium citrate, magnesium lactate, magnesium tartrate, magnesium silicate, magnesium ascorbate, calcium fluoride, calcium chloride, calcium bromide, calcium iodide, calcium sulfate, calcium phosphate, calcium monohydrogen phosphate, calcium dihydrogen phosphate, calcium carbonate, calcium monohydrogen carbonate, calcium acetate, calcium citrate, calcium lactate, calcium tartrate, calcium silicate, calcium ascorbate and combinations thereof.

[0022] Inorganic salts, such as inorganic alkali metal salts and inorganic alkaline earth metal salts, do not contain carbon. Organic salts, such as organic alkali metal salts and organic alkaline earth metal salts, contain carbon. The organic salt may be an alkali metal salt or an alkaline earth metal salt of sorbic acid (i.e., sorbate). Sorbic acid salts may be selected from sodium sorbate, potassium sorbate, magnesium sorbate, calcium sorbate, and combinations thereof.

[0023] Water-soluble carrier can be or comprise the material selected from the following items: water-soluble inorganic alkali metal salt, water-soluble organic alkali metal salt, water-soluble inorganic alkaline earth metal salt, water-soluble organic alkaline earth metal salt, water-soluble carbohydrate, water-soluble silicate, water-soluble urea and their combination.Water-soluble carrier can be selected from sodium chloride, potassium chloride, calcium chloride, magnesium chloride, sodium sulfate, potassium sulfate, magnesium sulfate, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium acetate, potassium acetate, sodium citrate, potassium citrate, sodium tartrate, potassium tartrate, potassium sodium tartrate, calcium lactate, water glass, sodium silicate, potassium silicate, dextrose, fructose, galactose, isoglucose, glucose, sucrose, raffinose, isomalt, xylitol, candy sugar, raw granulated sugar and their combination.In one embodiment, water-soluble carrier can be sodium chloride.In one embodiment, water-soluble carrier can be salt.

[0024] The water-soluble carrier can be or include a material selected from the group consisting of sodium bicarbonate, sodium sulfate, sodium carbonate, sodium formate, calcium formate, sodium chloride, sucrose, maltodextrin, corn syrup solids, corn starch, wheat starch, rice starch, potato starch, tapioca starch, clay, silicates, carboxymethylcellulose citrate, fatty acids, fatty alcohols, diglycerides of hydrogenated tallow, glycerin, and combinations thereof.

[0025] The water-soluble carrier can be selected from water-soluble organic alkali metal salts, water-soluble inorganic alkaline earth metal salts, water-soluble organic alkaline earth metal salts, water-soluble carbohydrates, water-soluble silicates, water-soluble urea, starch, clay, water-insoluble silicates, citrate carboxymethylcellulose, fatty acids, fatty alcohols, diglycerides of hydrogenated tallow, glycerol, polyethylene glycol, and combinations thereof.

[0026] The water-soluble carrier may be selected from disaccharides, polysaccharides, silicates, zeolites, carbonates, sulfates, citrates, and combinations thereof.

[0027] The water-soluble carrier may be selected from polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxyalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, sodium sulfate, starch, and mixtures thereof.

[0028] The water-soluble carrier may be a water-soluble polymer. The water-soluble polymer may be selected from the group consisting of: a C8-C22 alkyl polyalkoxylate containing more than about 40 alkoxylate units, an ethoxylated nonionic surfactant having an ethoxylation degree greater than about 30, a polyalkylene glycol having a weight average molecular weight of about 2000 to about 15000, and combinations thereof.

[0029] The water-soluble polymer may be a block copolymer having formula (I), (II), (III) or (IV), that is, R 1 O-(EO)x-(PO)yR 2 (I) R 1 O--(PO)x-(EO)yR 2 (II) R 1 O-(EO)o-(PO)p-(EO)qR 2 (III) R 1 O--(PO)o-(EO)p-(PO)qR 2 (IV) or a combination thereof; wherein EO is -CH 2 CH 2 O-group, and PO is -CH(CH 3 )CH 2 O-group; R 1 and R 2 is independently H or a C1-C22 alkyl group; x, y, o, p and q are independently 1-100; provided that the sum of x and y is greater than 35, and the sum of o, p and q is greater than 35; wherein the block copolymer has a molecular weight in the range of about 3000 g / mol to about 15,000 g / mol.

[0030] The water soluble polymer may be one or more block copolymers, such as block copolymers based on ethylene oxide and propylene oxide, selected from the group consisting of PLURONIC-F38, PLURONIC-F68, PLURONIC-F77, PLURONIC-F87, PLURONIC-F88, and combinations thereof. PLURONIC materials are available from BASF.

[0031] The water-soluble polymer can be selected from the group consisting of: polyvinyl alcohol (PVA), modified PVA; polyvinyl pyrrolidone; PVA copolymers, such as PVA / polyvinyl pyrrolidone and PVA / polyvinyl amine; partially hydrolyzed polyvinyl acetate; polyalkylene oxides, such as ethylene oxide; polyethylene glycol; acrylamide; acrylic acid; cellulose, alkyl celluloses, such as methyl cellulose, ethyl cellulose and propyl cellulose; cellulose ethers; cellulose esters; cellulose amides; polyvinyl acetate; polycarboxylic acids and salts; polyamino acids or peptides; polyamides; polyacrylamide; copolymers of maleic acid / acrylic acid; polysaccharides, including starch, modified starch; gelatin; alginates; xyloxylose, other hemicellulose polysaccharides, including xylans, glucuronic acid xylans, arabinoxylans, mannans, glucomannans and galactoglucomannans; natural gums, such as pectin, xanthan gum, carrageenan, locust bean gum, gum arabic, gum tragacanth; and combinations thereof. In one embodiment, the polymer comprises: polyacrylate, especially sulfonated polyacrylate and water-soluble acrylate copolymer; and alkylhydroxycellulose, such as methylcellulose, sodium carboxymethylcellulose, modified carboxymethylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, maltodextrin, polymethacrylate. In another embodiment, the water-soluble polymer can be selected from PVA; PVA copolymer; hydroxypropylmethylcellulose (HPMC); and mixtures thereof.

[0032] The water-soluble polymer can be selected from polyvinyl alcohol, modified polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl alcohol / polyvinyl pyrrolidone, polyvinyl alcohol / polyvinyl amine, partially hydrolyzed polyvinyl acetate, polyalkylene oxide, polyethylene glycol, acrylamide, acrylic acid, cellulose, alkyl cellulose, methyl cellulose, ethyl cellulose, propyl cellulose, cellulose ether, cellulose ester, cellulose amide, polyvinyl acetate, polycarboxylic acids and salts, polyamino acids or peptides, polyamides, polyacrylamides, maleic acid / acrylic acid copolymers, polysaccharides, starch, modified starch, gelatin, alginates, xyloxan, hemicellulose polysaccharides , xylan, glucuronic acid xylan, arabinoxylan, mannan, glucomannan, galactoglucomannan, natural gum, pectin, xanthan gum, carrageenan, locust bean gum, gum arabic, tragacanth gum, polyacrylates, sulfonated polyacrylates, water-soluble acrylate copolymers, alkyl hydroxycellulose, methylcellulose, sodium carboxymethylcellulose, modified carboxymethylcellulose, dextrin, ethylcellulose, propyl cellulose, hydroxyethylcellulose, hydroxypropyl methylcellulose, maltodextrin, polymethacrylates, polyvinyl alcohol copolymers, hydroxypropyl methylcellulose and mixtures thereof.

[0033] The water-soluble polymer may be an organic material. Organic water-soluble polymers may provide the benefit of being readily soluble in water.

[0034] The water-soluble polymer may be selected from the group consisting of polyethylene glycol, polypropylene glycol polyoxyalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, starch, and mixtures thereof.

[0035] The water-soluble polymer may be polyethylene glycol (PEG). PEG may be a convenient material for preparing particles because PEG may have sufficient water solubility to dissolve during the wash cycle when the particles have the mass range disclosed herein. In addition, PEG can be easily processed in melt form. The melting onset temperature of PEG may vary depending on the molecular weight of PEG. The particles may contain about 20% to about 94% PEG by weight, and the PEG has a weight average molecular weight of about 2000 to about 15000. PEG has a lower cost, can be formed into many different shapes and sizes, minimizes the diffusion of unencapsulated fragrances, and is well soluble in water. PEG has a variety of weight average molecular weights. The range of suitable PEG weight average molecular weight includes about 2,000 to about 13,000, or about 4,000 to about 13,000, or about 4,000 to about 12,000, or about 4,000 to about 11,000, or about 5,000 to about 11,000, or about 6,000 to about 10,000, or about 7,000 to about 9,000, or a combination thereof. PEG is available from BASF, such as PLURIOL E 8000, or other PLURIOL products. The water-soluble polymer can be a mixture of two or more polyethylene glycol compositions, one having a first weight average molecular weight (e.g., 9000), and the other having a second weight average molecular weight (e.g., 4000), the second weight average molecular weight being different from the first weight average molecular weight.

[0036] The granules may contain from about 20% to about 99% by weight of a water-soluble carrier. The granules may contain from about 35% to about 95%, optionally from about 50% to about 80%, optionally combinations thereof, and any integer percentage or range of integer percentages within any of the foregoing ranges, of a water-soluble carrier by weight of the granule.

[0037] The plurality of granules may comprise individual granules comprising from about 20% to about 99% by weight of the granule of a water soluble carrier; and from about 0.1% to about 20% by weight of the granule of capsules; wherein the capsules are dispersed in a matrix of a water soluble polymer.

[0038] The particles may comprise from about 20% to about 99% PEG by weight of a single particle. Optionally, a single particle may comprise from about 20% to about 95%, optionally from about 35% to about 95%, optionally from about 50% to about 80%, optionally combinations thereof, and any integer percentage or integer percentage range within any of the foregoing ranges, by weight of the particle.

[0039] The water-soluble polymer may include a material selected from the group consisting of: 2 H 4 O) x -(CH(CH 3 )CH2 O) y -(C 2 H 4 O) z -OH, wherein x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200; Formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 A polyethylene glycol fatty acid ester wherein q is from about 20 to about 200 and r is from about 10 to about 30; the formula HO-(C 2 H 4 O) s -(CH 2 ) t )-CH 3 Polyethylene glycol fatty alcohol ethers, wherein s is from about 30 to about 250 and t is from about 10 to about 30; and mixtures thereof. 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z The polyalkylene polymer of -OH may be a block copolymer or a random copolymer, wherein x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200.

[0040] The water-soluble polymer may include: polyethylene glycol; 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH, wherein x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200; Formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 A polyethylene glycol fatty acid ester of the formula HO-(C 2 H 4 O)s -(CH 2 ) t )-CH 3 A polyethylene glycol fatty alcohol ether wherein s is from about 30 to about 250 and t is from about 10 to about 30.

[0041] The water-soluble polymer may comprise from about 20% to about 95% by weight of the plurality of particles or by weight of an individual particle of the formula H-(C 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z A polyalkylene polymer of -OH wherein x is from about 50 to about 300; y is from about 20 to about 100, and z is from about 10 to about 200.

[0042] The water-soluble polymer may comprise from about 1% to about 20% by weight of the plurality of particles or by weight of the individual particles of the formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 A polyethylene glycol fatty acid ester wherein q is from about 20 to about 200 and r is from about 10 to about 30.

[0043] The water-soluble polymer may comprise from about 1% to about 10% by weight of the plurality of particles or by weight of an individual particle of the formula HO-(C 2 H 4 O) s -(CH 2 ) t )-CH 3 A polyethylene glycol fatty alcohol ether wherein s is from about 30 to about 250 and t is from about 10 to about 30.

[0044] The water-soluble carrier may comprise a plasticizer polyol (0% to 3% by weight of the granule), wherein the plasticizer polymer is optionally liquid at 20° C. and 1 atmosphere; water (1% to 20%, or 1% to 12%, or 6% to 8% by weight of the granule); a sugar alcohol polyol selected from the group consisting of erythritol, xylitol, mannitol, isomalt, maltitol, lactitol, trehalose, lactose, tagatose, sucralose, and mixtures thereof (45% to 80%, or 50% to 70%, or 50% to 60% by weight of the granule); Wherein the granules further comprise: (a) a modified starch having a dextrose equivalent of 15 to 20, and the sugar alcohol polyol and the modified starch are present in a weight ratio of the sugar alcohol polyol to the modified starch of 2:1 to 16:1, or 2:1 to 10:1, or 2:1 to 3:1; or (b) a modified starch having a dextrose equivalent of 4 to less than 15, and the sugar alcohol polyol and the modified starch are present in a weight ratio of the sugar alcohol polyol to the modified starch of 1.5:1 to 16:1, or 1.5:1 to 10:1, or 1.5:1 to 4. The modified starch may have a dextrose equivalent of 15 to 20, and the sugar alcohol polyol and the modified starch may be present in a ratio of 2:1 to 16:1, or 2:1 to 10:1, or 2:1 to 3:1. The modified starch may have a dextrose equivalent of 4 to less than 15, and the sugar alcohol polyol and the modified starch may be present in a weight ratio of the sugar alcohol polyol to the modified starch of 1.5:1 to 16:1, or 1.5:1 to 10:1, or 1.5:1 to 4:1. The modified starch may have a dextrose equivalent of 4 to 12. The modified starch may be maltodextrin. The sugar alcohol polyol may be mannitol. The plasticizer polyol may be selected from the group consisting of glycerol, dipropylene glycol, propylene glycol, and mixtures thereof.

[0045] The granules may contain more than about 20% by weight of a water-soluble carrier. The granules may contain more than about 40% by weight of a water-soluble carrier. The granules may contain from about 20% to about 99% by weight of a water-soluble carrier. Optionally, the granules may contain from about 35% to about 85%, or even from about 50% to about 80% by weight of a water-soluble carrier. The water-soluble carrier may be selected from the group consisting of: 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH, wherein x is 50 to 300, y is 20 to 100, and z is 10 to 200; Formula (C 2 H 4 O)q -C(O)O-(CH 2 ) r -CH 3 Polyethylene glycol fatty acid esters, wherein q is 20 to 200 and r is 10 to 30; Formula HO-(C 2 H 4 O) s -(CH 2 ) t )-CH 3 Polyethylene glycol fatty alcohol ethers, wherein s is 30 to 250 and t is 10 to 30; C8-C22 alkyl polyalkoxy esters containing more than 40 alkoxylate units; polyethylene glycol having a weight average molecular weight of 2000 to 15000; EO / PO / EO block copolymers; PO / EO / PO block copolymers; EO / PO block copolymers; PO / EO block copolymers; polypropylene glycol; ethoxylated nonionic surfactants having a degree of ethoxylation greater than 30; polyvinyl alcohol; polyalkylene glycols having a weight average molecular weight of 2000 to 15000; and mixtures thereof.

[0046] Fabric Care Benefit Actives

[0047] The particle may contain from about 0.1% to about 99% by weight of a fabric care benefit active.A fabric care benefit active is a material provided as part of the particle composition in an amount sufficient to impart a benefit to fabrics treated with the particle.

[0048] Fabric care benefit actives may be selected from the group consisting of amines, surfactant systems, nonionic surfactants, water-binding agents, sulfites, fatty acids and / or salts thereof, enzymes, encapsulated benefit agents, soil release polymers, hueing agents, builders, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleach catalysts, bleach activators, polymeric dispersants, cyclodextrin complex benefit agents, soil removal / anti-redeposition agents, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, foam suppressants, dyes, hueing agents, free perfumes, structural elasticizers, fabric softeners, quaternary amines, soft and hard tallow, carriers, fillers, hydrotropes, organic solvents, antimicrobial agents and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structurants, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof.

[0049] spices

[0050] The fabric care benefit agent may be a perfume. A perfume is an oil or fragrance that includes one or more odorous compounds, such as synthetic products of the ester, ether, aldehyde, ketone, alcohol and hydrocarbon types. Mixtures of various odorous substances may be used that together produce an attractive fragrance. Such perfume oils may also contain natural mixtures of odorous compounds, such as those obtainable from plant sources.

[0051] The fragrance may be a substantially water-insoluble composition comprising fragrance components, optionally mixed with a suitable solvent or diluent. Suitable solvents or diluents include compounds selected from the group consisting of ethanol, isopropanol, diethylene glycol monoethyl ether, dipropylene glycol, diethyl phthalate, triethyl citrate and mixtures thereof.

[0052] The fragrance can be provided as an unencapsulated fragrance. The fragrance can be provided in a fragrance delivery system. Zeolites and cyclodextrins are examples of fragrance delivery systems. The fragrance can be encapsulated in starch. For example, an emulsion of starch and fragrance oil can be spray dried to form starch particles with fragrance droplets dispersed in a starch matrix. The fragrance delivery system can be a granular material or a fine particulate material that may be difficult to handle in a manufacturing environment because the particles may be suspended in the air.

[0053] The fragrance can be an encapsulated fragrance. Encapsulated fragrances are commonly used in clothing products. Encapsulated fragrances contain multiple liquid fragrance droplets, each droplet is encapsulated in an encapsulation shell. The fragrance can be encapsulated in a water-soluble or water-insoluble encapsulation shell. The encapsulation shell can include materials such as melamine-urea-formaldehyde, melamine formaldehyde, urea formaldehyde, starch, etc. The encapsulation shell wall can be a material selected from the following: polyethylene; polyamide; polyvinyl alcohol, optionally containing other comonomers; polystyrene; polyisoprene; polycarbonate; polyester; polyacrylate; polyolefin; polysaccharide, such as alginate and / or deacetylated chitosan; gelatin; shellac; epoxy resin; vinyl polymer; water-insoluble inorganic substance; siloxane; aminoplast; and mixtures thereof. When the encapsulation shell contains aminoplast, the aminoplast can contain polyurea, polyurethane and / or polyureaurethane. Polyurea can include polyoxymethylene urea and / or melamine formaldehyde. Encapsulates with an encapsulation shell containing polysaccharides can be practical. The encapsulating shell may be selected from the group consisting of chitosan, gum arabic, alginate, beta-glucan, starch, starch derivatives, vegetable protein, gelatin, alyssum seed gum, and combinations thereof.

[0054] The encapsulating shell may comprise about 90% to 100%, optionally about 95% to 100%, optionally about 99% to 100%, of an inorganic material by weight of the shell. The inorganic material may be selected from the group consisting of metal oxides, semi-metal oxides, metals, minerals, and mixtures thereof, optionally selected from the group consisting of: SiO 2 、TiO 2、Al 2 O 3 、ZrO 2 、ZnO 2 、CaCO 3 , Ca 2 SiO 4 , Fe 2 O 3 , Fe 3 O 4 , clay, gold, silver, iron, nickel, copper and mixtures thereof, optionally selected from the group consisting of: SiO 2 、TiO 2 、Al 2 O 3 、CaCO 3 and mixtures thereof, optionally SiO 2 The encapsulation shell may include a first shell member and a second shell member, the first shell member including a condensation layer and a nanoparticle layer, wherein the condensation layer includes a condensation product of a precursor, and wherein the nanoparticle layer includes inorganic nanoparticles, and wherein the condensation layer is disposed between the core and the nanoparticle layer, the second shell member surrounds the first shell member, and wherein the second shell member surrounds the nanoparticle layer. The encapsulant may be any of those described in U.S. Patent Publications 2020 / 0330948 A1, 2020 / 0330949 A1, and 2020 / 0330950 A1 and U.S. Patent Application 63 / 092,829.

[0055] The fragrance may include one or more plant-derived fragrances. Plant-derived fragrances are concentrated hydrophobic liquids containing volatile compounds extracted from plants. Plant-derived fragrances may be selected from the group consisting of: allspice berries, angelica seeds, fennel seeds, basil, bay, laurel, bergamot, blood orange, camphor, caraway seeds, cardamom seeds, carrot seeds, cinnamon, nepeta, fir, celery seeds, chamomile, Roman chamomile, cinnamon bark, cinnamon leaves, lemongrass, sage, clove buds, coriander seeds, cypress, elemi, eucalyptus, fennel, fir, frankincense, geranium, ginger, pink grapefruit, helichrysum, hops, hyssop, juniper berries, rock rose, lavender, lemon, lemon Lemongrass, lime, magnolia, citrus, marjoram, lemon balm, artemisia, myrrh, myrtle, neroli, niacinamide, nutmeg, sweet orange, oregano, palmarosa, patchouli, peppermint oil, black pepper, mint, orange leaf, pine needles, radiata, ravensa leaf, rose, rosemary, rosewood, sage, sandalwood, spearmint, spikenard, spruce, star anise, artemisia annua, tangerine, tea tree, thyme red, verbena, vetiver, deer hoof grass, wormwood, yarrow, ylang-ylang extra and ylang-ylang III, and mixtures thereof.

[0056] The granules may comprise from about 0.1% to about 20% fragrance by weight of the granule, optionally from about 0.1% to about 15%, optionally from about 0.1% to about 12%, optionally from about 1% to about 15%, optionally from about 2% to about 20%, optionally from about 8% to about 10% fragrance by weight of the granule.

[0057] Fragrance lotion composition

[0058] The fabric care benefit agent can be a fragrance emulsion composition. The fragrance emulsion composition can include: an amino-functional silicone, wherein the amino-functional silicone includes one or more primary amine moieties, and wherein the amino-functional silicone is characterized by a total amine content of about 0.05 to about 2.2; one or more emulsifiers; one or more fragrance raw materials, wherein the one or more fragrance raw materials include an aldehyde moiety, a ketone moiety, or a combination thereof; and water.

[0059] The fragrance emulsion composition may be any of those described in European Patent Office Application No. 20156010.9 filed on February 7, 2020.

[0060] Amino functional siloxanes may be characterized by:

[0061] (a) a total amine content of from about 0.071 to about 2.14, or from about 0.071 to about 1.78, or from about 0.71 to about 1.43, or from about 0.14 to about 1.07, or from about 0.14 to about 0.71, or from about 0.21 to about 0.71, or from about 0.36 to about 0.71; and / or

[0062] (b) a primary amine content of about 0.05 to about 2.2, preferably about 0.071 to about 2.14, or about 0.071 to about 1.78, or about 0.71 to about 1.43, or about 0.14 to about 1.07, or about 0.14 to about 0.71, or about 0.21 to about 0.71, or about 0.36 to about 0.71; and / or

[0063] (c) The ratio of primary amine content to total amine content is from about 1:2 to about 1:1, preferably about 1.2:2, more preferably about 1.5:2, or even more preferably about 1.8:2.

[0064] The amino-functional siloxane may be characterized by the formula:

[0065] [R 1 R 2 R 3 SiO 1 / 2 ] (j+21+2) [R 4 R 5 SiO 2 / 2 ] m [R6 SiO 3 / 2 ] j [SiO 4 / z ] 1

[0066] in

[0067] j is an integer from 0 to 150, preferably from 0 to 50, more preferably from 0 to 20;

[0068] m is an integer from 10 to 1500, preferably from 10 to 1000, more preferably from 20 to 500;

[0069] l is an integer from 0 to 150, preferably from 1 to 150, more preferably from 0 to 50, most preferably from 0 to 20;

[0070] The prerequisite is that j+m+l is equal to an integer greater than or equal to 50;

[0071] R 1 , R 2 , R 3 , R 4 , R 5 and R 6 Each of the moieties is independently selected from H, OH, C 1 -C 32 Alkyl, C 1 -C 32 Substituted alkyl, C 6 -C 32 Aryl, C 5 -C 32 Substituted aryl, C 6 -C 32 Alkyl aryl, C 6 -C 32 Substituted alkylaryl, C 1 -C 32 Alkoxy and C 1 -C 32 substituted alkoxy, and XZ, wherein the part R 1 To R 6 At least one of = XZ,

[0072] Preferably, each R 1-6 Independently selected from OH, C 1 -C 2 Alkyl, C 1 -C 2 Substituted alkyl, C 1 -C 2 Alkoxy, C 1 -C 2 substituted alkoxy, and XZ;

[0073] wherein each X is independently a substituted or unsubstituted divalent alkylene or alkylidene group containing 2-12 carbon atoms, preferably each X is independently a substituted or unsubstituted divalent alkylene or alkylidene group containing 2-6 carbon atoms, most preferably each X is independently a substituted or unsubstituted divalent alkylene or alkylidene group containing 2-4 carbon atoms;

[0074] wherein each Z is a moiety comprising said one or more primary amine moieties,

[0075] Preferably, each Z is independently selected from the group -NH 2 、-N(H)-X-NH 2 or a mixture thereof.

[0076] The emulsion composition may be characterized by at least one of features (a) to (d):

[0077] (a) comprising from about 10% to about 70%, or from about 25% to about 65%, or from about 50% to about 65%, by weight of the silicone emulsion, of an amino-functional silicone; and / or

[0078] (b) comprises from about 30% to about 90%, or from about 35% to about 75%, or from about 35% to about 50%, by weight of the emulsion, of water; and / or

[0079] (c) characterized by a viscosity measured at 0.1 rad / s and 25° C. of about 10 Pa·s to about 500 Pa·s, preferably about 20 Pa·s to about 400 Pa·s, more preferably about 25 Pa·s to about 300 Pa·s, even more preferably about 100 Pa·s to about 300 Pa·s; and / or

[0080] (d) comprising a plurality of droplets, wherein the plurality of droplets are characterized by an average diameter of about 1 micrometer to about 5 micrometers.

[0081] The one or more fragrance raw materials may comprise materials selected from the group consisting of:

[0082] a.oncidal, methylnonyl acetaldehyde, adoc aldehyde, melon aldehyde, calypsone or mixtures thereof;

[0083] b. cuminaldehyde, benzaldehyde, anisaldehyde, jasmine aldehyde, isocyclic citral, privet aldehyde (triplal / ligustral), 3,6-ivy formaldehyde, privet aldehyde (ligustral), Qingfeng aldehyde or mixtures thereof;

[0084] c. sardinaldehyde (jasmonic acid), otropal, cyclamenaldehyde, cyclamal, lily of the valley aldehyde, consinaldehyde, sea breeze aldehyde, cinnamaldehyde or mixtures thereof;

[0085] d. δ-damascone, β-damascone, α-damascone, damascone or mixtures thereof;

[0086] e. vanillin, ethyl vanillin or mixtures thereof; or

[0087] f. A combination of materials selected from at least two categories of a, b, c, d and e.

[0088] The one or more emulsifiers may comprise a nonionic surfactant, preferably wherein the nonionic surfactant comprises an alkoxylated fatty alcohol, even more preferably wherein the one or more emulsifiers are characterized by an HLB value of from about 5 to about 20, preferably from about 8 to about 16.

[0089] The one or more emulsifiers may include a first emulsifier and a second emulsifier, wherein the second emulsifier is different from the first emulsifier, preferably wherein the first emulsifier is a linear nonionic surfactant, and / or preferably wherein the second emulsifier is a branched nonionic surfactant.

[0090] Fabric softening

[0091] The fabric care active benefit agent may be a fabric softening active. The particles may contain about 5% to about 45% by weight of a quaternary ammonium compound. The quaternary ammonium compound may be an ester quaternary ammonium compound. The quaternary ammonium compound may be those described in U.S. Patent Publications 2019 / 0169538 A1, 2019 / 0169539 A1, 2019 / 0169777 A1, 2019 / 0169532 A1, 2019 / 0169533 A1, and 2019 / 0169534 A1. The quaternary ammonium compound may be di-(tallowyloxyethyl)-N, N-methylhydroxyethyl methyl ammonium sulfate.

[0092] The fabric softening active may be a fatty amine. The particle may contain from about 8% to about 45% by weight of a fatty amine. The fatty amine may be those described in U.S. Patent Publication No. 2020 / 0354652 A1.

[0093] The fabric softening active may be a silicone. The particle may contain from about 1% to about 50% silicone by weight. The silicone may be a silicone as described in U.S. Patent Publication No. 2017 / 0349865.

[0094] Branched polyester

[0095] The fabric care active benefit agent may be a branched polyester. The particle may contain from about 5% to about 45% by weight of a branched polyester. The branched polyester may be those described in U.S. Patent Publication 2019 / 0367841 A1. The branched polyester may be those described and claimed in U.S. Patent Publication 2019 / 0233764 A1.

[0096] Cationic polymers

[0097] The fabric care active benefit agent may be a cationic polymer. The particle may contain from about 0.1% to about 10% by weight of a cationic polymer. The cationic polymer may be selected from the group consisting of a cationic polysaccharide, polyquaternium-4, polyquaternium-6, polyquaternium-7, polyquaternium-10, polyquaternium-22, polyquaternium-67, and mixtures thereof. The cationic polysaccharide may be a polymeric quaternary ammonium salt of hydroxyethyl cellulose that has been reacted with an epoxide substituted with a trimethylammonium group.

[0098] Enzymes

[0099] The fabric care active benefit agent may be an enzyme. The particle may contain from about 0.0001% to about 5% by weight of the enzyme. The enzyme may be selected from the group consisting of: a protease, a xyloglucanase, a mannanase, and a combination thereof. The enzyme may be those described in U.S. Patent Publications 2017 / 0260481 A1 and 2017 / 0260482 A1.

[0100] Graft copolymer

[0101] The fabric care active benefit agent may be a graft copolymer. The particle may contain from about 1% to about 75% by weight of the graft copolymer. The graft copolymer may be those described in U.S. Patent Application 69 / 951,274. The graft copolymer may be those described in U.S. Patent Application 69 / 722,492.

[0102] Antioxidants

[0103] The fabric care active benefit agent may be an antioxidant. The particles may contain from about 0.2% to about 2% by weight of an antioxidant. The antioxidant may be dispersed in the matrix of the water-soluble carrier. The antioxidant may be those antioxidants described in U.S. Patent Application No. 63 / 034,766. The antioxidant may be butylated hydroxytoluene.

[0104] Apparatus and method for forming particles

[0105] exist Figure 1, an apparatus 1 for forming particles is shown in . Precursor material 20 may be a melt of any composition disclosed herein for particles 90. Precursor material 20 may include more than about 20% by weight of a water-soluble carrier. Precursor material 20 may include more than about 20% by weight of a water-soluble polymer. Precursor material 20 may include about 20% to about 99% by weight of a water-soluble carrier. Precursor material 20 may include about 20% to about 99% by weight of a water-soluble polymer.

[0106] Precursor material 20 may comprise greater than about 20%, optionally greater than about 40%, by weight of polyethylene glycol having a weight average molecular weight of about 2000 to about 13000, and from about 0.1% to about 20% by weight of fragrance.

[0107] One or more raw materials may be provided to the batch mixer 10. The batch mixer 10 may have sufficient capacity to maintain a sufficient residence time for a certain volume of raw materials provided thereto, thereby allowing a desired level of raw material mixing and / or reaction to occur. The material leaving the batch mixer 10 may be a precursor material 20. Optionally, the precursor material may be provided to the feed pipe 40 from some other upstream mixing process (e.g., in-line mixing, in-line static mixing, etc.). The precursor material 20 may be a molten product. The batch mixer 10 may be a dynamic mixer. A dynamic mixer is a mixer that applies energy to mix the contents in the mixer. The batch mixer 10 may include one or more impellers to mix the contents in the batch mixer 10.

[0108] Between the batch mixer 10 (optionally present) and the distributor 30, the precursor material 20 may be conveyed through the feed pipe 40. The feed pipe 40 may be in fluid communication with the batch mixer 10. One or more gas feed lines 155 may be provided in fluid communication with the feed pipe 40 downstream of the batch mixer 10. One or more gas feed lines 155 may be provided in fluid communication with the feed pipe 40 between the batch mixer 10 and the distributor 30. The grinder 200 may be provided downstream of the one or more gas feed lines 155 and in series with the feed pipe 40. The grinder 200 may be provided in series with the feed pipe 40 downstream of the one or more gas feed lines 155 and upstream of the distributor 30.

[0109] The precursor material 20 may be provided to the feed pipe 40. The feed pipe 40 is a transport device that carries the precursor material 20. The feed pipe 40 includes a transport device between the elements of the apparatus 1 and a transport device through which the precursor material is carried within the components of the apparatus 1. For example, the grinder 200 may be provided in a unit in which a portion of the transport device is close to the grinder 200 and a portion of the transport device is away from the grinder 200. Each of these portions is a portion of the feed pipe 40. Therefore, the feed pipe 40 may be regarded as the entire transport device between the batch mixer 10 and the distributor 30, and the feed pipe 40 is interrupted by various elements such as one or more gas feed lines 155, the grinder 200, the intermediate mixer 50, and the feed pump 140. In the absence of an intermittent mixer 10 upstream of the feed pipe 40, the feed pipe 40 can be regarded as the entire transmission device upstream of the distributor 30, and the feed pipe 40 is interrupted by various elements (such as one or more gas feed pipelines 155, the grinder 200, the intermediate mixer 50 and the feed pump 140).

[0110] The intermediate mixer 55 may be disposed downstream of the grinder 200 and in series with the feed pipe 40. The intermediate mixer 55 may be a static mixer 50. The intermediate mixer 55 may be in fluid communication with the feed pipe 40 between the grinder 200 and the distributor 30. The intermediate mixer 55 may be a static mixer 50, which may be downstream of the batch mixer 10. In other words, the batch mixer 10 may be upstream of the intermediate mixer 55 or the static mixer 55 (if used). The intermediate mixer 55 may be in series with the feed pipe 40. The intermediate mixer 55 may be a rotor-stator mixer. The intermediate mixer 55 may be a colloid mill. The intermediate mixer 55 may be an inline driven fluid disperser. The intermediate mixer 55 may be an Ultra Turrax disperser, a Dispax-reactor disperser, a ColloidMil MK, or a Cone Mill MKO, available from IKA, Wilmington, North Carolina, United States of America. The intermediate mixer 55 can be a porous disc mill, a toothed colloid mill, or a DIL Inline Homogenizer, available from FrymaKoruma, Rheinfelden, Switzerland. The static mixer 50 can be a spiral static mixer. The static mixer 50 can be a Kenics 1.905 cm inner diameter KMS 6, available from Chemineer, Dayton, OH, USA.

[0111] Without being bound by theory, it is believed that an intermediate mixer 55, such as a static mixer 50, can provide a more uniform temperature of the precursor material 20 within the distributor 30 or the stator 100. At the downstream end of the intermediate mixer 55 or static mixer 50 (if used), the temperature of the precursor material 20 within the feed tube 40 across a cross section of the feed tube 40 orthogonal to the flow direction can vary by less than about 10°C, or less than about 5°C, or less than about 1°C, or less than about 0.5°C.

[0112] In the absence of a static mixer 50, the temperature across the cross-section of the feed tube 40 orthogonal to the flow direction may be non-uniform. The temperature of the precursor material 20 at the centerline of the feed tube 40 may be higher than the temperature of the precursor feed material 20 at the peripheral wall of the feed tube 40. When the precursor material 20 is discharged into the distributor 30 or stator 100, the temperature of the precursor material 20 may change at different locations within the distributor or stator 100. Without being bound by theory, it is believed that by providing a uniform temperature across the entire cross-section of the feed tube 40 using a static mixer 50 as described herein, more uniform particles 90 can be produced compared to the apparatus 1 without a static mixer 50.

[0113] The distributor 30 may be provided with a plurality of holes 60. The precursor material 20 may pass through the holes 60. After passing through the holes 60, the precursor material 20 may be deposited on a moving conveyor 80 disposed below the distributor 30. When the conveyor 80 is moving, the precursor material 20 may be deposited on the moving conveyor 80. The conveyor 80 may be capable of translation relative to the distributor 30. The conveyor 80 may be a continuously moving conveyor 80. The conveyor 80 may be an intermittently moving conveyor 80. The continuously moving conveyor 80 may provide a higher processing speed. The intermittently moving conveyor 80 may provide improved control over the shape of the prepared particles 90.

[0114] The precursor material 20 can be cooled on the moving conveyor 80 to form a plurality of solid particles 90. The cooling can be provided by ambient cooling. Optionally, the cooling can be provided by spraying the underside of the conveyor 80 with water at ambient temperature or cooling water.

[0115] Once the particles 90 have developed sufficient viscosity, the particles 90 may be conveyed from the conveyor 80 to processing equipment downstream of the conveyor 80 for further processing and / or packaging.

[0116] The distributor 30 may be a cylinder 110 rotatably mounted about a stator 100 in fluid communication with the feed tube 40, and the cylinder 110 may have a periphery 120 and may have a plurality of holes 60 in the periphery 120, such as Figure 2Thus, the apparatus 1 may include a stator 100 in fluid communication with a feed tube 40. The feed tube 40 may feed the precursor material 20 into the stator 100 after the precursor material 20 has passed through the grinder 200.

[0117] The apparatus 1 may include a cylinder 110 rotatably mounted about a stator 100. The stator 100 feeds a precursor material through one or both ends 130 of the cylinder 110. The cylinder 110 may have a longitudinal axis L passing through the cylinder 110 about which the cylinder 110 rotates. The cylinder 110 has a periphery 120. There may be a plurality of holes 60 in the periphery 120 of the cylinder 110.

[0118] When the cylinder 110 is driven to rotate about its longitudinal axis L, the hole 60 can be intermittently in fluid communication with the stator 100 when the cylinder 110 rotates around the stator 100. The cylinder 110 can be considered to have a longitudinal direction MD in the direction of movement across the periphery 120 of the stator 100 and a transverse direction orthogonal to the longitudinal direction MD on the periphery 120. The stator 100 can be similarly considered to have a transverse direction CD parallel to the longitudinal axis L. The transverse direction of the stator 100 can be aligned with the transverse direction of the cylinder 110. The stator 100 can have a plurality of dispensing ends 122, which are arranged in the transverse direction CD of the stator 100. The dispensing end 122 is a portion or area of ​​the stator 100 that supplies the precursor material 20.

[0119] Generally, the precursor material 20 may be fed to the stator 100 through the mill 200 and the feed tube 40 via one or more gas feed lines 155. The stator 100 distributes the precursor feed material 20 across the entire operating width of the drum 110. As the drum 110 rotates about its longitudinal axis, the precursor material 20 is fed through the holes 60 as the holes 60 pass through the stator 100. As each hole 60 encounters the stator 100, a non-continuous amount of the precursor material 20 is fed through each hole 60. The amount of the precursor material 20 fed through each hole 60 as each hole 60 passes through the stator 100 can be controlled by controlling one or both of the precursor material pressure within the stator 100 and the rotational speed of the drum 110, or optionally by controlling the viscosity of the precursor material 20 by controlling the temperature of the precursor material 20.

[0120] Droplets of precursor material 20 are deposited on conveyor 80 across the entire operating width of drum 110. Conveyor 80 may be translatable relative to the longitudinal axis of drum 110. The speed of conveyor 80 may be set relative to the tangential speed of drum 110 to control the shape of precursor material 20 once it is deposited on conveyor 80. The speed of conveyor 80 may be approximately the same as the tangential speed of drum 110.

[0121] like Figure 1As shown in , the flow of the precursor material 20 flowing through the feed tube 40 can be provided by gravity driven flow from the batch mixer 10 and the distributor 30. In order to provide more controlled manufacturing, the apparatus 1 can be provided with a feed pump 140, such as Figure 2 . The feed pump 140 may be in series with the feed pipe 40, in series meaning in line with the flow of the precursor material 20. The feed pump 140 may be between the batch mixer 10 and the distributor 30. The feed pump 140 may be upstream of the distributor 30. If a stator 100 is used, the feed pump 140 may be in series with the feed pipe 40, in series meaning in line with the flow of the precursor material 20. If a stator 100 is used, the feed pump 140 may be between the batch mixer 10 and the stator 100. The feed pump 140 may be upstream of the stator 100. When describing the position of the feed pump 140, intermediate is used to describe that the feed pump 140 is in series with the downstream of the batch mixer 10 and the upstream of the distributor 30, or if used, the upstream of the stator 100.

[0122] If used in the apparatus 1 , one or more gas feed lines 155 and a grinder 200 may be positioned in series between the feed pump 140 and the distributor 30 or stator 100 .

[0123] The flow rate of the precursor material 20 may be about 3 L / min. The precursor material 20 may be a molten material comprising any of the compositions described herein for the precursor material 20 or the particles 90.

[0124] The apparatus 1 may include one or more gas feed lines 155. If the gas to be entrained into the precursor material can actually be supplied via a single gas feed line 155, a single gas feed line 155 may be practical. As described herein, a single component gas or a gas containing multiple components may be desirable. A single component gas or a multi-component gas may be provided in a single container 157. For example, a mixture of argon, carbon dioxide, and nitrogen may be provided in a gas cylinder. Optionally, a gas mixture may be continuously provided from the environment via a reaction process or by combining air with another gas from a container. The gas may be pressurized via a compressor.

[0125] The one or more gas feed lines 155 may include a flow regulator 158. The flow regulator 158 may regulate the flow of gas entering the feed line 40. The volume of gas added per unit volume of the precursor material 20 may be controlled by setting the flow regulator 158 to a desired flow rate. The more gas fed into the precursor material 20 in the feed line 40, the more gas will be included in the particles 90. The one or more gas feed lines 155 may be used to entrain gas into the precursor material 20.

[0126] The flow regulator 158 may be a Key Instruments Flo-Rite series GS 65 mm flow meter, part number 60410-R5. The feed tube 40 may be 1 1 / 2 inch stainless steel sanitary pipe. The gas feed line 155 may be a 1 / 4 inch inner diameter polyethylene pipe. The gas may be provided to the gas feed line 155 at a pressure greater than about 4 bar (eg, 5.9 bar).

[0127] If two or more gas feed lines 155 are respectively connected to the feed pipe 40, a flow regulator may be provided along each gas feed line 155 to regulate the gas flow in each respective gas feed line 155. If the gas mixture is introduced into the feed pipe 40 via a single gas feed line 155, a single flow regulator 158 may be practical.

[0128] At the connection between the gas feed line 155 and the feed pipe, an injection bushing device for introducing gas may be provided.

[0129] The gas can be provided at a temperature and pressure such that when the gas reaches ambient temperature and pressure, a desired volume of gas is present in the particles 90. The ideal gas law can be used to determine the desired temperature and pressure for delivery. The gas can also contain water. The water can be in gaseous or liquid form. The amount of water in the gas can be selected to be at a desired level.

[0130] The grinder 200 may be a rotor-stator type grinder. The grinder may be a Quadro Z1 inline mixer with a single stage mid-rotor stator, which operates at about 400 RPM.

[0131] The grinder 200 and the one or more gas feed lines 155 may be combined in a single unit.

[0132] Oakes Foamer (ET Oakes Corporation, 686 Old Willets Path, Hauppauge, NY 11788) 2MT1A continuous foamer can be used to place the gas feed line 155, flow regulator 158 and grinder 200 in a single unit.

[0133] A view of the device 1 in the longitudinal direction MD is shown in Figure 3 In. Figure 3 As shown in , the apparatus 1 may have an operating width W and the cylinder 110 may rotate about a longitudinal axis L.

[0134] The apparatus 1 for forming particles 90 may include: a feed pipe; one or more gas feed lines 155, the one or more gas feed lines being mounted in fluid communication with the feed pipe 40 downstream of the batch mixer 10; a grinder 200, the grinder being located downstream of the one or more gas feed lines 155 and in series with the feed pipe 40; and a distributor 30, the distributor being located downstream of the grinder 200 and in fluid communication with the feed pipe 40, wherein the distributor 30 includes a plurality of holes 60. The apparatus 1 may include a conveyor below the distributor 30 and being translationally movable relative to the distributor 30. The distributor 30 may include a stator 100 in fluid communication with the feed pipe 40. The distributor 30 may include a barrel 110 rotatably mounted about the stator 100 and rotatable about a longitudinal axis L of the barrel 110. The barrel 110 may have a perimeter 120, and the barrel 110 may have a plurality of holes 60 disposed about the perimeter 120. The holes 60 may be intermittently in fluid communication with the stator 100 as the cylinder 110 rotates about the stator 100. The apparatus may include a conveyor 80 below the cylinder 110, and the conveyor 80 may be translationally movable relative to the longitudinal axis L. The apparatus 1 for forming particles 90 may include a batch mixer 10. The feed tube 40 may be in fluid communication with the batch mixer 10.

[0135] The method for forming particles 90 may include the following steps: providing a precursor material 20 to a feed tube 40; entraining a gas into the precursor material 20, wherein the gas comprises about 50 volume % to about 100 volume %, optionally about 55 volume % to about 100 volume %, optionally about 60 volume % to about 100 volume %, optionally about 70 volume % to about 100 volume %, optionally about 80 volume % to about 100 volume %, optionally about 90 volume % to about 100 volume %, optionally 100 volume % argon; providing a distributor 30 having a plurality of holes 60; conveying the precursor material 20 from the feed tube 40 to the distributor 30; passing the precursor material 20 through the holes 60; providing a movable conveying device 80 below the holes 60; depositing the precursor material 20 onto the movable conveying device 80; and cooling the precursor material 20 to form a plurality of particles 90.

[0136] The gas may be entrained in the precursor material 20 as a gas mixture. For example, the gas mixture may be introduced into the precursor material 20 via a single gas feed line 155. The gas mixture may include about 50% to about 100% by volume, optionally about 55% to about 100% by volume, optionally about 60% to about 100% by volume, optionally about 70% to about 100% by volume, optionally about 80% to about 100% by volume, optionally about 90% to about 100% by volume, optionally 100% by volume of argon and about 0% to about 50% by volume of other ingredients. The mixture may be provided from a container 157 containing the gas mixture. For example, the container 157 may be a gas cylinder filled with a desired gas, which is a mixture of different gases.

[0137] Optionally, argon gas may be provided from a primary container 157a, and the other components of the gas may be provided from one or more secondary containers 157b ( Figure 4 ). The primary container 157a and the secondary container 157b may feed into a single gas feed line 155. A flow regulator 158 may control the flow of gas from the primary container 157a and the secondary container 157b into the gas feed line 155. Optionally, an in-line mixer may be provided in or upstream of the gas feed line 155 to mix the gas from the primary container 157a and the secondary container 157b.

[0138] The primary container 157a may contain argon. Other components of the gas may be provided from a secondary container 157b. Other components of the gas may be provided from the secondary container 157b as air or carbon dioxide. Air containers and carbon dioxide containers are readily commercially available. Similarly, argon containers are readily commercially available. An operator of the apparatus 1 may obtain argon cylinders and air cylinders and set a flow regulator 158 to provide the desired gas. The argon and other components of the gas may be combined into a single gas stream before being entrained into the precursor material 20.

[0139] Optionally, primary vessel 157a may feed into a primary gas feed line 155 and secondary vessel 157b may feed into a secondary gas feed line 155. The gas flow rate within each gas feed line 155 may be regulated by a flow regulator 158 dedicated to such gas feed line 155.

[0140] In operation, it is feasible to provide the precursor material 20 in the feed tube at an operating pressure of about 2 bar to about 8 bar. The gas may be fed into the feed tube at a pressure higher than the operating pressure of the feed tube 40. The gas or its argon component may be entrained at a pressure greater than about 3 bar to about 4 bar, or even greater than about 4 bar, or even greater than about 5 bar.

[0141] The solubility of argon gas in the precursor material 20 may be greater than the solubility of the bulk volume of the other components of the gas. When argon gas is fed into the stream of the precursor material 20 at the operating pressure, the argon gas dissolves into the precursor material 20. The other components of the gas may or may not dissolve into the precursor material 20 at the operating pressure. Those components that have a low solubility in the precursor material 20 relative to argon gas are retained in the precursor material 20 primarily as bubbles.

[0142] As the precursor material 20 passes through the hole 60, the pressure drops toward or to atmospheric pressure. The precursor material 20 may also begin to cool. As the precursor material 20 travels from the hole 60 to the movable conveyor 80, the precursor material 20 may continue to cool. The cooling continues after the precursor material 20 is deposited on the movable conveyor 80. Heat is removed from the precursor material 20 by the conveyor, and the belt-facing side of the precursor material 20 in contact with the movable conveyor 80 begins to solidify. Similarly, after the precursor material 20 is deposited on the movable conveyor 80, the surface of the precursor material 20 continues to cool. Therefore, the cooling of the precursor material 20 after being deposited on the movable conveyor 80 is a three-dimensional time-dependent process.

[0143] As the molten precursor material 20 cools, a solidification front develops from the belt-facing side of the precursor material 20, and the solidification front advances over time away from the movable conveyor 80. The air-facing side of the precursor material 20 (which is away from the belt-facing surface of the precursor material) also cools over time. This results in a solidification front that advances from the air-facing surface toward the center of the particle on the movable conveyor 80 as the precursor material 20 cools.

[0144] If the gas entrained in the precursor material 20 is air, which is about 78% nitrogen by volume, about 21% oxygen by volume, about 0.93% argon by volume, and about 0.03% carbon dioxide by volume, most of the gas has limited solubility in the precursor material 20, and the air is retained in the precursor material 20 as bubbles throughout the process of making the particles. This can limit the amount of air that can be entrained in the precursor material 20 and still give the particles the desired stability and appearance. After the precursor material 20 is deposited on the movable belt 40, the buoyancy of the bubbles in the precursor material 20 and the solidification front advancing from the belt-facing side of the precursor material 20 tend to drive some of the bubbles away from the movable conveyor 80. When the bubbles are driven upward, they can coalesce to form larger bubbles. Some bubbles can escape through the air-facing side of the precursor material 20. The escaped bubbles no longer contribute to the porosity of the particles 90. If a skin has formed on the air-facing side of the precursor material 20, gas bubbles can be ejected through the skin, which can result in particles 90 having physically unstable outer surfaces. Physically unstable outer surfaces are undesirable because they can cause the particles to flake and make the particles messy during use.

[0145] A problem with using air as the gas to be entrained is that bubbles are present in the precursor material 20 when it is deposited onto the movable belt 40 and the phenomena described in the previous paragraph occur, which can result in unsatisfactory particles 90. Surprisingly, using a gas comprising about 50% to about 100% by volume, optionally about 55% to about 100% by volume, optionally about 60% to about 100% by volume, optionally about 70% to about 100% by volume, optionally about 80% to about 100% by volume, optionally about 90% to about 100% by volume, optionally 100% by volume argon can improve the ability of the precursor material 20 to retain bubbles as the precursor material 20 is cooled on the movable conveyor 80 to form particles 90. This can result in particles 90 having a higher porosity and fewer large bubbles at or near the air-facing surface of the particles 90.

[0146] Argon may be relatively soluble in the precursor material 20 compared to other gas components. Relatively insoluble gas components in the precursor material 20 may exist as bubbles. When the operating pressure on the precursor material is released to ambient pressure or near ambient pressure, the argon flows out of solution. The process of argon flowing out of the solution of the precursor material 20 is a time-dependent process. Bubbles of relatively insoluble gas components in the precursor material 20, if present, may serve as nucleation sites for argon to flow out of the solution of the precursor material. As the argon flows out of solution, the precursor material 20 is also cooling. As previously described, a solidification front may develop from the tape-facing side of the precursor material 20, and the air-facing side of the precursor material 20 is also solidifying. The solidifying or solidified precursor material 20 forms a barrier to bubbles escaping from the precursor material 20. As the argon gradually flows out of the solution of the precursor material 20, bubbles of argon may form and / or argon may flow out of solution into existing bubbles of relatively insoluble gas components. The delayed formation of argon bubbles, or the expansion of existing bubbles of relatively insoluble gas components as argon nucleates on such bubbles, allows for a larger volume of bubbles to form in the precursor material 20. And these later-formed bubbles are less likely to escape from the precursor material 20. Once the precursor material 20 is fully cured, the formed particles 90 can have a large volume of voids.

[0147] A gas containing about 50% to about 100% by volume, optionally about 55% to about 100% by volume, optionally about 60% to about 100% by volume, optionally about 70% to about 100% by volume, optionally about 80% to about 100% by volume, optionally about 90% to about 100% by volume, optionally 100% by volume argon may be advantageous over air or a gas containing more than about 50% by volume carbon dioxide. For dissolved gases that contribute to the void volume of the solidified particles 90, bubbles flow out of solution and form in a time-dependent process. For bubble formation caused by changes in gas solubility as a function of changes in pressure, or decompression nucleation, the bubble formation rate decreases with solubility. The rate of bubble formation from decompression nucleation using argon that is partially soluble in the precursor material 20 can be much faster than the bubble formation rate when using a relatively more soluble gas such as carbon dioxide. This may be the case when the precursor material 20 comprises more than about 20% by weight of a water-soluble polymer, or more specifically, polyethylene glycol having a weight average molecular weight of about 2,000 to about 13,000.

[0148] If the bubble formation rate of decompression nucleation is slower than the solidification rate, the phase change will drive bubble formation. Bubble formation in the solidified precursor material 20 driven by the phase change can cause the particle surface to rupture and cause the expanded melt to solidify on the particle surface. This is an undesirable aesthetic effect for the particles 90, and can also cause the accumulation of broken particles 90 in the product packaging, which is also undesirable. For the particles formed by the distributor 30 that keeps the molten precursor material 20 under pressure substantially until the molten precursor material is discharged from the distributor 30, an acceptable gas can be a gas that provides partial solubility in the molten precursor material 20 at atmospheric pressure and has a time-dependent nucleation rate faster than the solidification rate of the precursor material 20 that finally forms the particles 90 when the precursor material 20 is deposited. For a polyethylene glycol carrier with a weight average molecular weight of about 2000 to about 13000 and a minimum pressure change of 3 bars through the distributor 30, argon can provide these desired properties. Argon can be superior to a blend of air and carbon dioxide due to its partial solubility in water-soluble polymers such as polyethylene glycol. At the same temperature and pressure, argon is more soluble in polyethylene glycol than air because the nitrogen portion of the air has a relatively low solubility in polyethylene glycol compared to argon. However, argon has a much lower solubility than carbon dioxide because the amount of carbon dioxide injected is almost completely dissolved at only 3 bar pipeline pressure, and the same amount of argon is only partially dissolved at 10 bar. The gas can be entrained at pressures from about 3 bar to about 10 bar.

[0149] Particles

[0150] The particles 90, which can be formed as described herein, can contain from about 25% to about 99% by weight of a water-soluble carrier. The particles 90 can also contain from about 0.1% to about 20% by weight of a fabric care benefit active agent. Each particle can have a mass of from about 5 mg to about 200 mg, preferably from about 10 mg to about 100 mg, preferably from about 20 mg to about 50 mg. The particles can have a hemispherical or compressed hemispherical shape.

[0151] Fabric care benefit actives may be selected from the group consisting of amines, surfactant systems, nonionic surfactants, water-binding agents, sulfites, fatty acids and / or salts thereof, enzymes, encapsulated benefit agents, soil release polymers, hueing agents, builders, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleach catalysts, bleach activators, polymeric dispersants, cyclodextrin complex benefit agents, soil removal / anti-redeposition agents, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, foam suppressants, dyes, hueing agents, free perfumes, structural elasticizers, fabric softeners, quaternary amines, soft and hard tallow, carriers, fillers, hydrotropes, organic solvents, antimicrobial agents and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structurants, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof.

[0152] The fabric care benefit active may be selected from the group consisting of antimicrobial agents, antioxidants, perfumes, fabric conditioners, dyes, dye fixatives, and combinations thereof.The fabric care benefit active may be an unencapsulated perfume or an encapsulated perfume.

[0153] Each of the particles 90 may have a mass of about 5 mg to about 200 mg, optionally about 10 mg to about 100 mg, optionally about 20 mg to about 50 mg. The particles may have a hemispherical or compressed hemispherical shape.

[0154] Granules 90 can be prepared as follows. A batch of 50 kg of precursor material 20 can be prepared in a mixer. Molten PEG8000 can be added to a jacketed mixer maintained at 70° C. and stirred at 125 rpm with a pitched blade paddle stirrer. Butylated hydroxytoluene can be added to the mixer in an amount of about 0.01% by weight of the precursor material 20. A water-based slurry of perfume microcapsules can be added to the mixer in an amount of about 4% by weight of the precursor material 20. Unencapsulated perfume can be added to the mixer in an amount of about 8% by weight of the precursor material 20. Dye can be added to the mixer in an amount of about 0.01% by weight of the precursor material 20. PEG can account for the balance by weight of the precursor material 20. The precursor material 20 can be mixed for 30 minutes.

[0155] The precursor material 20 can be formed into particles 90 on a SANDVIK ROTOFORM 3000 with a belt 750 mm wide and 10 m long. The cylinder 110 can have 2 mm diameter holes 60, which are arranged at a spacing of 10 mm in the cross direction CD and at a spacing of 9.35 mm in the machine direction MD. The cylinder can be set about 3 mm above the belt. The belt speed and the rotation speed of the cylinder 110 can be set to 10 m / min.

[0156] After mixing the precursor material 20, the precursor material 20 can be pumped from the mixer 10 at a constant rate of 3.1 kg / min or even 4 kg / min through a plate and frame heat exchanger that is configured to control the outlet temperature to 50° C. The pressure in the feed pipe 40 downstream of the pump 140 can be about 2 bar to about 7 bar, and alternatively about 5.5 bar or about 5 bar, which is the pressure in the feed pipe 40 downstream of the grinder 200.

[0157] The gas may be entrained in the precursor material 20, wherein the volume flow rate ratio of the precursor material to the gas is about 1.3:1 to about 2.6:1, or even about 1.3:1 to about 1.6:1. The pressure of the gas in the gas feed line 155 must be higher than the pressure in the feed tube 40 to ensure that the gas flows and is entrained in the precursor material 20. The flow rate of the precursor material 20 may be about 4.5 liters / minute, and the gas flow rate may be about 3.4 liters / minute. The gas may be argon, a mixture of argon and carbon dioxide, or a mixture of argon and other relatively insoluble gases.

[0158] The precursor material 20 with the gas entrained therein may be passed through a Quadro Z1 mill with a medium rotor / stator element. After milling, the precursor material may optionally be passed through a Kenics 1.905 cm KMS 6 static mixer 50 mounted 91.44 cm upstream of the stator 100 of the rotary forming apparatus.

[0159] combination :

[0160] A. A method for forming particles, the method comprising the steps of:

[0161] a. providing a precursor material (20) to a feed tube (40);

[0162] b. entraining a gas into the precursor material, wherein the gas comprises from about 50% to about 100% by volume, optionally from about 55% to about 100% by volume, optionally from about 60% to about 100% by volume, optionally from about 70% to about 100% by volume, optionally from about 80% to about 100% by volume, optionally from about 90% to about 100% by volume, optionally about 100% by volume argon and from about 0% to about 50% by volume of other ingredients;

[0163] c. Providing a dispenser (30) comprising a plurality of holes (60);

[0164] d. transferring the precursor material (20) from the feed pipe to the distributor;

[0165] e. passing the precursor material through the hole;

[0166] f. Providing a movable conveying device (80) below the hole;

[0167] g. causing the precursor material to be deposited onto the movable conveyor; and

[0168] h. Cooling the precursor material to form a plurality of particles (90).

[0169] B. The method according to paragraph A, wherein the dispenser comprises:

[0170] a. a stator (100), the stator being in fluid communication with the feed pipe;

[0171] b. A cylinder (110) rotatably mounted about the stator and rotatable about a longitudinal axis (L) of the cylinder, wherein the cylinder has a periphery (120) and the cylinder includes the plurality of holes disposed about the periphery, wherein the holes are intermittently connected to the stator fluid when the cylinder rotates about the stator.

[0172] C. The method according to paragraph A or B, further comprising the step of grinding the precursor material after the step of entraining gas into the precursor material.

[0173] D. The method of paragraph C, wherein the step of grinding the precursor material after the step of entraining gas into the precursor material is performed using an in-line rotor-stator grinder.

[0174] E. The method of any of paragraphs A to D, wherein the gas is entrained as a gas mixture.

[0175] F. The method of paragraph E, wherein the gas mixture is from a container containing the gas mixture.

[0176] G. The method of any of paragraphs A to E, wherein the argon gas is provided from a primary container (157a) and the other components of the gas are provided from one or more secondary containers (157b).

[0177] H. The method of paragraph G, wherein the argon gas and the other components of the gas are combined into a single stream of the gas prior to being entrained into the precursor material.

[0178] I. A method according to paragraph H, wherein the other components of the gas are provided as air from the secondary container.

[0179] J. The method of any of paragraphs A to I, wherein the argon is entrained at a pressure greater than 2 bar at a minimum flow rate of about 0.5 liters / minute.

[0180] K. The method of any of paragraphs A to J, wherein more than 50% by volume of the other ingredients have a solubility in the precursor material that is less than that of argon.

[0181] L The method of any of paragraphs A to K, wherein the precursor material comprises greater than about 20% by weight of a water-soluble polymer.

[0182] M. The method according to paragraph L, wherein the water-soluble polymer is selected from the group consisting of:

[0183] a. Formula H-(C 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH, wherein x is from 50 to 300, y is from 20 to 100, and z is from 10 to 200;

[0184] b. Formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 A polyethylene glycol fatty acid ester, wherein q is 20 to 200, and r is 10 to 30;

[0185] c. Formula HO-(C 2 H 4 O) s -(CH 2 ) t )-CH 3 Polyethylene glycol fatty alcohol ether, wherein s is 30 to 250, and t is 10 to 30;

[0186] d. C8-C22 alkyl polyalkoxylates containing more than 40 alkoxylate units;

[0187] e. polyethylene glycol having a weight average molecular weight of 2000 to 15000;

[0188] f.EO / PO / EO block copolymer:

[0189] g. PO / EO / PO block copolymer;

[0190] h.EO / PO block copolymer;

[0191] i.PO / EO block copolymer;

[0192] j. Polypropylene glycol;

[0193] k. ethoxylated nonionic surfactants having a degree of ethoxylation greater than 30;

[0194] 1. Polyvinyl alcohol;

[0195] m. polyalkylene glycols having a weight average molecular weight of 2000 to 15000; and mixtures thereof.

[0196] N. The method of any of paragraphs A to M, wherein the precursor material comprises polyethylene glycol having a weight average molecular weight of about 2,000 to about 13,000.

[0197] O. The method of any of paragraphs A to N, wherein the precursor material comprises greater than about 40% by weight polyethylene glycol.

[0198] P. The method according to any of paragraphs A to O, wherein the particles have an individual mass between about 0.1 mg and about 2 mg.

[0199] Q. The method of any of paragraphs A to P, wherein the precursor material comprises from about 0.1% to about 20% by weight fragrance.

[0200] R. The method of paragraph Q, wherein the flavorant comprises an encapsulated flavorant.

[0201] S. The method of paragraph Q, wherein the fragrance comprises encapsulated fragrance and unencapsulated fragrance.

[0202] T. The method of any of paragraphs A to S, wherein the precursor material comprises from about 0.1% to about 20% by weight of an encapsulated flavor.

[0203] U. The method of any of paragraphs A to T, wherein the step of cooling the precursor material is performed by ambient cooling.

[0204] V. The method of any of paragraphs A to U, wherein the precursor material is provided to the feed tube from a batch mixer (10).

[0205] W. The method of any of paragraphs A to V, wherein the other component is selected from the group consisting of oxygen, nitrogen, argon, and mixtures thereof.

[0206] X. The method according to any one of paragraphs A to W, wherein the precursor material comprises a fabric care benefit agent selected from the group consisting of: amines, surfactant systems, nonionic surfactants, water binding agents, sulfites, fatty acids and / or salts thereof, enzymes, encapsulated benefit agents, soil release polymers, hueing agents, builders, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalytic substances, bleaching agents, bleach catalysts, bleach activators, polymer dispersants, cyclodextrin complexes. Benefit agents, soil removal / anti-redeposition agents, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, foam suppressants, dyes, hueing agents, free perfumes, structural elasticizers, fabric softeners, quaternary amines, soft and hard tallows, carriers, fillers, hydrotropes, organic solvents, antimicrobial agents and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structurants, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof.

[0207] Y. The method of any of paragraphs A to X, wherein the gas is argon.

[0208] Z. The method of any of paragraphs A to Y, wherein the gas is entrained at a pressure of about 3 bar to about 10 bar.

[0209] The dimensions and values ​​disclosed herein should not be understood as being strictly limited to the exact numerical values ​​cited. Instead, unless otherwise indicated, each such dimension is intended to represent the stated value and a functionally equivalent range around that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".

[0210] Unless expressly excluded or otherwise limited, each document cited herein, including any cross-referenced or related patent or patent application and any patent application or patent to which this application claims priority or the benefit of, is hereby incorporated by reference in its entirety. The citation of any document is not an admission that it is prior art to any of the present invention disclosed or claimed herein, or an admission that it, by itself or in combination with any one or more of the references, proposes, suggests, or discloses any such invention. In addition, to the extent that any meaning or definition of a term in this invention conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this invention shall govern.

[0211] Although specific embodiments of the present invention have been illustrated and described, it will be apparent to those skilled in the art that various other changes and modifications may be made without departing from the spirit and scope of the present invention. Therefore, it is intended that all such changes and modifications within the scope of the present invention be covered in the appended claims.

Claims

1. A method for forming particles, the method comprising the following steps: Providing a precursor material (20) to a feed tube (40); entraining a gas into the precursor material, wherein the gas comprises from about 50% to about 100% argon by volume and from about 0% to about 50% by volume of other ingredients; providing a dispenser (30) comprising a plurality of apertures (60); conveying the precursor material (20) from the feed tube to the dispenser; passing the precursor material through the aperture; providing a movable conveyor (80) below the aperture; depositing the precursor material onto the movable conveyor; as well as The precursor material is cooled to form a plurality of particles (90).

2. The method according to claim 1, wherein the dispenser comprises: a stator (100), the stator being in fluid communication with the feed pipe; A cylinder (110) is rotatably mounted about the stator and is rotatable about a longitudinal axis (L) of the cylinder, wherein the cylinder has a periphery (120) and the cylinder includes the plurality of holes disposed about the periphery, wherein the holes are intermittently in fluid communication with the stator when the cylinder rotates about the stator.

3. The method according to claim 1 or claim 2, further comprising the following steps: The precursor material is milled after the step of entraining a gas into the precursor material.

4. The method of claim 3, wherein the step of grinding the precursor material after the step of entraining gas into the precursor material is performed using an in-line rotor-stator grinder.

5. The method according to any one of claims 1 to 4, wherein the gas is entrained as a gas mixture.

6. The method of claim 5, wherein the gas mixture is from a container containing the gas mixture.

7. A method according to any one of claims 1 to 6, wherein the argon gas is provided from a primary container (157a) and the other components of the gas are provided from one or more secondary containers (157b).

8. The method of claim 7, wherein the other component of the gas is provided as air from the secondary container.

9. The method of any one of claims 1 to 8, wherein the argon and the other components of the gas are combined into a single stream of the gas before being entrained into the precursor material.

10. A method according to any one of claims 1 to 9, wherein the argon is entrained at a pressure greater than 2 bar at a minimum flow rate of about 0.5 litres / minute.

11. The method according to any one of claims 1 to 10, wherein more than 50% by volume of the other components have a solubility in the precursor material that is lower than that of the argon gas.

12. The method of any one of claims 1 to 11, wherein the precursor material comprises greater than about 20% by weight of a water-soluble polymer.

13. The method according to claim 12, wherein the water-soluble polymer is selected from: Formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH, wherein x is from 50 to 300, y is from 20 to 100, and z is from 10 to 200; Formula (C2H4O) q -C(O)O-(CH2) r -CH3 polyethylene glycol fatty acid esters, wherein q is 20 to 200, and r is 10 to 30; Formula HO-(C2H4O) s -(CH2) t )-CH3 polyethylene glycol fatty alcohol ether, wherein s is 30 to 250, and t is 10 to 30; C8-C22 alkyl polyalkoxylates containing more than 40 alkoxylate units; Polyethylene glycol having a weight average molecular weight of 2000 to 15000; EO / PO / EO block copolymer; PO / EO / PO block copolymer: EO / PO block copolymer; PO / EO block copolymer; Polypropylene glycol: Ethoxylated nonionic surfactants with a degree of ethoxylation greater than 30; Polyvinyl alcohol; Polyalkylene glycol having a weight average molecular weight of 2,000 to 15,000; and A mixture of them.

14. The method of any one of claims 1 to 13, wherein the precursor material comprises polyethylene glycol having a weight average molecular weight of about 2,000 to about 13,000.

15. The method according to any one of claims 1 to 14, wherein the other component is selected from the group consisting of oxygen, nitrogen, carbon dioxide and mixtures thereof.

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