Process for forming particles

Abstract

A process for forming particles. The process includes a step of mixing a gas into a precursor material, where the gas contains from about 50 volume % to about 100 volume % argon and from about 0 volume % to about 50 volume % other components. The precursor material is deposited on a moving conveyor. The precursor material is cooled to form a plurality of particles.

Description

[Technical Field]

[0001] A process for forming particles. [Background Art]

[0002] Consumers desire products that can simplify the process they use to do laundry, can help reduce the time spent handling dirty laundry, and can help achieve a high level of benefits. Consumers are well positioned to understand the amount of fabric care composition that is necessary to provide the benefits they desire. As a result, fabric care products that allow consumers to customize the amount of fabric care composition they use are favored by many consumers.

[0003] Fabric care products that can be delivered into a washing liquor are particularly easy to use for consumers. For example, consumers can simply place the fabric care product together with the laundry into the drum of a washing machine and start the washing machine cycle.

[0004] Typically, consumers use fabric care detergent compositions that contain a substantial amount of surfactants and other cleaning ingredients. Such fabric care compositions are often provided in soluble unit dose pouches containing a predetermined amount of fabric care active agent. Fabric care compositions are also provided in liquid or powder form, and consumers are provided with a measuring cup to provide a measured amount of the fabric care composition. These types of products may be referred to as fully formulated fabric care compositions.

[0005] Fabric care additives are popular with consumers because they offer fabric care benefits that go beyond what can be provided by using a complete fabric care composition. Consumers enjoy and are satisfied with using packaged fabric care additives in a way that allows them to use custom amounts of fabric care additives based on their own judgment of how much fabric care additive is needed to provide the desired benefits. Such fabric care additives are conveniently provided through washing together with a complete fabric care composition, but are added separately from the complete fabric care composition.

[0006] Fabric care additives in particle form have become appealing to many consumers. Some fabric care additive particles are offered with a porous structure. Particles with a porous structure can float in water when the wash solution is formed. Floating particles may tend to dissolve more completely in the wash compared to sinking particles, as sinking particles can get trapped in the folds, wrinkles, and pockets of the laundry during the wash. Undissolved particles tend to incompletely deliver the beneficial fabric care activators contained within the particles, which may be undesirable for consumers. Floating particles containing non-encapsulated fragrances can provide a pleasant scent to the headspace above the wash solution and in the room where the washing machine is located. Furthermore, floating particles may distribute the fabric care additive more effectively to the laundry during the wash cycle.

[0007] Melt processing is a common technique for forming particles. One problem associated with making porous particles via a melt process is that as the molten precursor material solidifies, bubbles within the melt tend to coalesce and rise out of the molten material. This can result in large pores at or near the outer surface of the particle, an irregularly rough outer surface, an irregular distribution of pore sizes within the solidified particle, as well as ejection of bubbles and molten material from the particle surface as the particle solidifies. Such particles may have a more accessible outer surface, tend to be dusty, tend to be difficult to use, and are less durable than particles that appear to be of poor quality. The tendency of bubbles in the melt to coalesce and rise out of the molten material as the molten precursor solidifies can also effectively limit the volume of pores that can be provided within the particles without causing these adverse effects. SUMMARY OF THE INVENTION PROBLEM TO BE SOLVED BY THE INVENTION

[0008] In view of these limitations, there continues to be an unmet need for fabric care additives in the form of particles having a uniform distribution of pore sizes throughout the particles. Furthermore, there is a need for a process for forming such porous particles. MEANS FOR SOLVING THE PROBLEM

[0009] A process for forming particles, comprising the steps of: feeding a precursor material to a feed pipe; incorporating a gas into the precursor material, wherein the gas comprises from about 50 volume% to about 100 volume% argon and from 0 volume% to about 100 volume% other components; providing a distributor comprising a plurality of holes; moving the precursor material from the feed pipe to the distributor; passing the precursor material through the holes; providing a movable conveyor below the holes; depositing the precursor material onto the movable conveyor; and cooling the precursor material to form a plurality of particles. BRIEF DESCRIPTION OF DRAWINGS

[0010] [Figure 1] It is a device for forming particles. [Figure 2] It is part of a device used to form particles. [Figure 3] This is an end view of a device for forming particles. [Figure 4] It is part of a device used to form particles. [Modes for carrying out the invention]

[0011] Water-soluble carrier The particles, and by extension the precursor materials described below, may include a water-soluble carrier. The water-soluble carrier may be a water-soluble polymer. The water-soluble carrier acts to transport the capsules into the cleaning solution. Once the water-soluble carrier dissolves, the capsules are dispersed in the cleaning solution and adhere to the laundry.

[0012] The water-soluble carrier may be a material that is soluble in the cleaning solution in a short time, for example, less than about 10 minutes.

[0013] Water solubility means that a material, carrier material, or particle is soluble or dispersible in water and has water solubility of at least 50%, at least 75%, or even at least 95%, as measured by the method described below herein using a glass filter with a maximum pore size of 20 microns. The method is as follows: (50 grams ± 0.1 grams of carrier material are added to a pre-weighed 400 mL beaker, and 245 mL ± 1 mL of distilled water is added. This is vigorously stirred for 30 minutes with a magnetic stirrer set to 600 rpm. The mixture is then filtered through a sintered glass filter with the pore size defined above (maximum 20 micrometers). The process is carried out at a temperature of 23 °C ± 1.0 °C and a relative humidity of 50% ± 2%. The water is dried from the recovered filtrate by any conventional method, and the weight of the remaining material is determined (this is the soluble fraction or dispersion fraction). The percentage of solubility or dispersion can then be calculated.

[0014] The water-soluble carrier may be selected from the group consisting of 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.

[0015] Alkali metal salts can be selected from the group consisting of, for example, salts of lithium, salts of sodium, and salts of potassium, and any combination thereof. Useful alkali metal salts can be selected from the group consisting of, for example, alkali metal fluorides, alkali metal chlorides, alkali metal bromides, alkali metal iodides, alkali metal sulfates, alkali metal bisulfates, alkali metal phosphates, alkali metal monohydrogen phosphates, alkali metal dihydrogen phosphates, alkali metal carbons, alkali metal monohydrogen carbons, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbicates, and combinations thereof.

[0016] Alkali metal salts can be selected from the group consisting of sodium fluoride, sodium chloride, sodium bromide, sodium iodide, sodium sulfate, sodium bicarbonate, sodium phosphate, monohydrogen phosphate, 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 bicarbonate, potassium phosphate, monohydrogen phosphate, dihydrogen phosphate, potassium carbonate, monohydrogen carbonate, potassium acetate, potassium citrate, potassium lactate, potassium tartrate, potassium silicate, potassium, ascorbates, and combinations thereof.

[0017] Alkaline earth metal salts can be selected from the group consisting of magnesium salts, calcium salts, and combinations thereof. Alkaline earth metal salts can be selected from the group consisting of alkali metal fluorides, alkali metal chlorides, alkali metal bromides, alkali metal iodides, alkali metal sulfates, alkali metal bisulfates, alkali metal phosphates, alkali metal monohydrogen phosphates, alkali metal dihydrogen phosphates, alkali metal carbons, alkali metal monohydrogen carbons, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbicates, and combinations thereof. Alkaline earth metal salts can be selected from the group consisting of magnesium fluoride, magnesium chloride, magnesium bromide, magnesium iodide, magnesium sulfate, magnesium phosphate, monohydrogen phosphate, dihydrogen phosphate, magnesium carbonate, 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, monohydrogen phosphate, dihydrogen phosphate, calcium carbonate, monohydrogen carbonate, calcium acetate, calcium citrate, calcium lactate, calcium tartrate, calcium silicate, calcium ascorbate, and combinations thereof.

[0018] 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. Organic salts may be alkali metal salts or alkaline earth metal salts of sorbic acid (i.e., sorbates). Sorbates may be selected from the group consisting of sodium sorbate, potassium sorbate, magnesium sorbate, calcium sorbate, and combinations thereof.

[0019] The water-soluble carrier may be a material selected from the group consisting of water-soluble inorganic alkali metal salts, 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, and combinations thereof, or may contain such materials. The water-soluble carrier may be selected from the group consisting of 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, sodium potassium tartrate, calcium lactate, water glass, sodium silicate, potassium silicate, dextrose, fructose, galactose, isoglucose, glucose, sucrose, raffinose, isomalt, xylitol, rock sugar, granulated sugar, and combinations thereof. In one embodiment, the water-soluble carrier may be sodium chloride. In one embodiment, the water-soluble carrier may be table salt.

[0020] The water-soluble carrier may be a material selected from the group consisting of sodium bicarbonate, sodium sulfate, sodium carbonate, sodium formate, calcium formate, sodium chloride, sucrose, maltodextrin, corn syrup solid, corn starch, wheat starch, rice starch, potato starch, tapioca starch, clay, silicates, carboxymethylcellulose citrate, fatty acids, fatty alcohols, glyceryl diesters of hydrogenated animal fat, glycerol, and combinations thereof, or may contain such materials.

[0021] The water-soluble carrier may be selected from the group consisting of 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, carboxymethylcellulose citrate, fatty acids, fatty alcohols, glyceryl diesters of hydrogenated animal fats, glycerol, polyethylene glycol, and combinations thereof.

[0022] The water-soluble carrier may be selected from the group consisting of disaccharides, polysaccharides, silicates, zeolites, carbonates, sulfates, citrates, and combinations thereof.

[0023] The water-soluble carrier may be selected from the group consisting of polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxoalkylene, polyethylene glycol fatty acid esters, polyethylene glycol ethers, sodium sulfate, starch, and mixtures thereof.

[0024] The water-soluble carrier may be a water-soluble polymer. The water-soluble polymer may be selected from the group consisting of C8-C22 alkyl polyalkoxylates containing more than about 40 alkoxylate units, ethoxylated nonionic surfactants having a degree of ethoxylation of more than about 30, polyalkylene glycols having a weight average molecular weight of from about 2000 to about 15000, and combinations thereof.

[0025] The water-soluble polymer may be of formula (I), (II), (III) or (IV), R 1 O-(EO)x-(PO)y-R 2 (I), R 1 O-(PO)x-(EO)y-R 2 (II), R 1 O-(EO)o-(PO)p-(EO)q-R 2 (III), R 1 O-(PO)o-(EO)p-(PO)q-R 2 (IV), or combinations thereof, wherein EO is a -CH2CH2O- group, PO is a -CH(CH3)CH2O- group, R 1 and R 2 are independently H or a C1-C22 alkyl group, x, y, o, p, and q are independently from 1 to 100, with the proviso that the sum of x and y is greater than 35, the sum of o, p, and q is greater than 35, and the block copolymer has a molecular weight ranging from about 3000 g / mol to about 15,000 g / mol).

[0026] The water-soluble polymer may be a block copolymer or a plurality of block copolymers, for example, an ethylene oxide and propylene oxide-based block copolymer 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.

[0027] Water-soluble polymers include polyvinyl alcohol (polyvinyl A selection may be made from the group consisting of alcohol (PVA), modified PVA; polyvinylpyrrolidone; PVA copolymers such as PVA / polyvinylpyrrolidone and PVA / polyvinylamine; partially hydrolyzed polyvinyl acetate; polyalkylene oxides such as polyethylene oxide; polyethylene glycol; acrylamide; acrylic acid; alkylcellulose materials such as cellulose, e.g., methylcellulose, ethylcellulose, and propylcellulose; cellulose ethers; cellulose esters; celluloseamides; polyvinyl acetate; polycarboxylic acids and salts; polyamino acids or peptides; polyamides; polyacrylamides; maleic acid / acrylic acid copolymers; polysaccharides including starch and modified starch; gelatin; alginates; other hemicellulose polysaccharides including xyloglucan, xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan, and galactoglucomannan; and natural gums such as pectin, xanthan gum, and carrageenan, locus bean, arabic, tragacanth; and combinations thereof. In one embodiment, the polymer includes polyacrylates, particularly sulfonated polyacrylates and water-soluble acrylate copolymers; and alkylhydroxycellulose-based materials, such as methylcellulose, sodium carboxymethylcellulose, modified carboxymethylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, maltodextrin, and polymethacrylate. In yet another embodiment, the water-soluble polymer is selected from the group consisting of PVA; PVA copolymers; hydroxypropyl methylcellulose (HPMC); and mixtures thereof.

[0028] Water-soluble polymers include polyvinyl alcohol, modified polyvinyl alcohol, polyvinylpyrrolidone, polyvinyl alcohol / polyvinylpyrrolidone, polyvinyl alcohol / polyvinylamine, partially hydrolyzed polyvinyl acetate, polyalkylene oxide, polyethylene glycol, acrylamide, acrylic acid, cellulose, alkylcellulose-based materials, methylcellulose, ethylcellulose, propylcellulose, cellulose ether, cellulose ester, celluloseamide, polyvinyl acetate, polycarboxylic acids and salts, polyamino acids or peptides, polyamide, polyacrylamide, maleic acid / acrylic acid copolymer, polysaccharides, starch, modified starch, gelatin, alginate, xyloglucan, hemicellulose-based polysaccharides. The following materials may be selected from the group consisting of xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan, galactoglucomannan, natural gum, pectin, xanthan gum, carrageenan, locus bean, arabic, tragacanth, polyacrylate, sulfonated polyacrylate, water-soluble acrylate copolymer, alkyl hydroxycellulose-based materials, methylcellulose, sodium carboxymethylcellulose, modified carboxymethylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, maltodextrin, polymethacrylate, polyvinyl alcohol polymer, hydroxypropylmethylcellulose, and mixtures thereof.

[0029] Water-soluble polymers can be organic materials. Organic water-soluble polymers can offer the advantage of being readily soluble in water.

[0030] The water-soluble polymer may be selected from the group consisting of polyethylene glycol, polypropylene glycol polyoxoalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, starch, and mixtures thereof.

[0031] The water-soluble polymer may be polyethylene glycol (PEG). PEG can be a convenient material for producing particles because it can be sufficiently water-soluble to dissolve during the washing cycle when the particles have a mass within the range disclosed herein. Furthermore, PEG can be readily handled as a molten material. The onset of the melting temperature of PEG can vary as a function of the molecular weight of PEG. The particles may contain about 20% to about 94% by weight of PEG, with a weight-average molecular weight of about 2000 to about 15000. PEG is relatively low-cost, can be formed into many different shapes and sizes, minimizes the diffusion of non-encapsulated fragrances, and dissolves well in water. PEG is available in a variety of weight-average molecular weights. The preferred weight-average molecular weight range for PEG 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 combinations thereof. PEG is available from BASF, for example, as PLURIOL E 8000, or other PLURIOL products. The water-soluble polymer may 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), wherein the second weight-average molecular weight is different from the first weight-average molecular weight.

[0032] The particles may contain approximately 20% to 99% by weight of a water-soluble carrier. The particles may also contain approximately 35% to 95% by weight of the particles, optionally approximately 50% to 80% by weight, optionally a combination thereof, and any total percentage or total percentage within any of the aforementioned ranges of a water-soluble carrier.

[0033] Multiple particles may include individual particles containing approximately 20% to 99% by weight of a water-soluble carrier and approximately 0.1% to 20% by weight of a particle capsule, the capsules dispersed in a matrix of a water-soluble polymer.

[0034] The particles may contain approximately 20% to 99% by weight of PEG. Optionally, each particle may contain approximately 20% to 95% by weight of PEG, optionally approximately 35% to 95% by weight, optionally approximately 50% to 80% by weight, optionally a combination thereof, and any total percentage or total percentage within any of the aforementioned ranges.

[0035] Water-soluble polymers are given by formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (where x is approximately 50 to 300, y is approximately 20 to 100, and z is approximately 10 to 200) polyalkylene polymer; formula (C2H4O) q -C(O)O-(CH2) r -CH3 (wherein q is approximately 20 to approximately 200 and r is approximately 10 to approximately 30) polyethylene glycol fatty acid ester; formula HO-(C2H4O) s -CH2) t Polyethylene glycol fatty alcohol ethers of the formula H-CH3 (wherein s is about 30 to about 250 and t is about 10 to about 30); and materials selected from the group consisting of mixtures thereof. Formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z Polyalkylene polymers of -OH (where x is approximately 50 to approximately 300, y is approximately 20 to approximately 100, and z is approximately 10 to approximately 200) can be block copolymers or random copolymers.

[0036] The water-soluble polymer is polyethylene glycol; formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (where x is approximately 50 to 300, y is approximately 20 to 100, and z is approximately 10 to 200) polyalkylene polymer; formula (C2H4O) q -C(O)O-(CH2) r-CH3 (wherein q is approximately 20 to approximately 200 and r is approximately 10 to approximately 30) polyethylene glycol fatty acid esters; and formula HO-(C2H4O) s -(CH2) t It may contain polyethylene glycol fatty alcohol ether of )-CH3 (wherein s is about 30 to about 250 and t is about 10 to about 30).

[0037] The water-soluble polymer is composed of approximately 20% to 95% by weight of multiple particles or individual particles, with the formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z It may contain polyalkylene polymers of -OH (wherein x is approximately 50 to approximately 300, y is approximately 20 to approximately 100, and z is approximately 10 to approximately 200).

[0038] The water-soluble polymer is present in a concentration of approximately 1% to 20% by weight of multiple particles or individual particles, and is of the formula (C2H4O). q -C(O)O-(CH2) r It may contain polyethylene glycol fatty acid esters of -CH3 (wherein q is about 20 to about 200 and r is about 10 to about 30).

[0039] The water-soluble polymer is present in a concentration of approximately 1% to 10% by weight of multiple particles or individual particles, with the formula HO-(C2H4O) s -CH2) t It may contain polyethylene glycol fatty alcohol ethers of )-CH3 (wherein s is about 30 to about 250 and t is about 10 to about 30).

[0040] The water-soluble carrier may consist of a plasticizer polyol (0% to 3% by weight of the particles), wherein the plasticizer polymer is optionally liquid at 20°C and 1 atm, water (1% to 20% by weight of the particles, or 1% to 12% by weight, or 6% to 8% by weight), and 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% by weight of the particles, or 50% to 70% by weight, or 50% to 60% by weight), and the particles are (a) Modified starch having 15 to 20 dextrose equivalents, wherein the sugar alcohol polyol and the modified starch are present in a weight ratio of 2:1 to 16:1, or 2:1 to 10:1, or 2:1 to 3:1; or (b) Modified starch having 4 to less than 15 dextrose equivalents, wherein the sugar alcohol polyol and the modified starch are present in a weight ratio 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 15 to 20 dextrose equivalents, 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 4 to less than 15 dextrose equivalents, and the sugar alcohol polyol and the modified starch may exist in a weight ratio 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 4 to 12 dextrose equivalents. The modified starch may be maltodextrin. The sugar alcohol polyol may be mannitol. The plasticizer polyol may be selected from the group consisting of glycerin, dipropylene glycol, propylene glycol, and mixtures thereof.

[0041] The particles may contain more than approximately 20% by weight of a water-soluble carrier. The particles may contain more than approximately 40% by weight of a water-soluble carrier. The particles may contain approximately 20% to approximately 99% by weight of a water-soluble carrier. Optionally, the particles may contain approximately 35% to approximately 85% by weight, or even more, approximately 50% to approximately 80% by weight of a water-soluble carrier. The water-soluble carrier has the formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (where x is 50-300, y is 20-100, and z is 10-200) polyalkylene polymer; formula (C2H4O) q -C(O)O-(CH2) r -CH3 (wherein q is 20-200 and r is 10-30) polyethylene glycol fatty acid ester; formula HO-(C2H4O) s -(CH2) t Polyethylene glycol aliphatic alcohol ethers of the formula )-CH3 (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 copolymers; PO / EO / PO block copolymers; EO / PO block copolymers; PO / EO block copolymers; polypropylene glycols; ethoxylated nonionic surfactants having a degree of ethoxylation greater than 30; polyvinyl alcohols; polyalkylene glycols having a weight-average molecular weight of 2000 to 15000; and mixtures thereof may be selected from the group.

[0042] Fabric care beneficial activators The particles may contain approximately 0.1% to 99% by weight of a fabric care beneficial activator. The fabric care beneficial activator is a substance provided as part of the particle composition in an amount sufficient to impart beneficial properties to the fabric being treated with the particles.

[0043] Fabric care beneficial activators may be selected from the group consisting of amines, surfactants, nonionic surfactants, water-binding agents, sulfites, fatty acids and / or salts thereof, enzymes, encapsulation beneficial agents, stain-releasing polymers, colorants, builders, chelating agents, stain transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleaching catalysts, bleaching activators, polymer dispersants, cyclodextrin complex beneficial agents, stain removers / anti-redeposition agents, encapsulation fragrances, polymer dispersants, polymer grease cleaners, whitening agents, antifoaming agents, dyes, colorants, free fragrances, structural elasticizers, fabric softeners, quaternary amines, cured and softened tallows, carriers, fillers, hydrotropes, organic solvents, antimicrobial agents and / or preservatives, neutralizing agents and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structuring agents, opacifiers, pearl essences, pigments, corrosion inhibitors and / or colorfast agents, and mixtures thereof.

[0044] fragrance Fabric care beneficial agents may be fragrances. Fragrances are oils or air fresheners containing one or more fragrant compounds, such as esters, ethers, aldehydes, ketones, alcohols, and hydrocarbon-type synthetic products. Mixtures of various fragrant substances that work together to produce an attractive aromatic note may be used. Such fragrance oils may also include natural mixtures of fragrant compounds, such as those available from plant sources.

[0045] The fragrance may be a substantially water-insoluble composition comprising fragrance components 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.

[0046] Fragrances may be supplied as non-encapsulated fragrances. Fragrances may be supplied in a fragrance delivery system. Zeolites and cyclodextrins are examples of fragrance delivery systems. Fragrances may be encapsulated in starch. For example, an emulsion of starch and fragrance oil may be spray-dried to form starch particles having droplets of fragrance dispersed within a starch matrix. Fragrance delivery systems may be particulate materials or fine particulate materials that may be difficult to handle in the manufacturing environment due to the possibility that the particles may become airborne.

[0047] The fragrance may be an encapsulated fragrance. Encapsulated fragrances are commonly used in laundry products. An encapsulated fragrance contains multiple droplets of liquid fragrance, each encapsulated in an encapsulation shell. The fragrance may be encapsulated in a water-soluble or water-insoluble encapsulation shell. The encapsulation shell may include melamine-urea-formaldehyde, melamine-formaldehyde, urea-formaldehyde, starch, and similar materials. The encapsulation shell may be a material selected from polyethylene; polyamide; polyvinyl alcohol containing other comonomers; polystyrene; polyisoprene; polycarbonate; polyester; polyacrylate; polyolefin; polysaccharides, e.g., alginate and / or chitosan; gelatin; shellac; epoxy resin; vinyl polymer; water-insoluble inorganic materials; silicone; aminoplast; and mixtures thereof. If the inclusion shell contains an aminoplast, the aminoplast may contain polyurea, polyurethane, and / or polyurea urethane. The polyurea may contain polyoxymethylene urea and / or melamine formaldehyde. Inclusion bodies having an inclusion shell containing polysaccharides may be practical. The inclusion shell may be selected from the group consisting of chitosan, gum arabic, alginate, β-glucan, starch, starch derivatives, plant proteins, gelatin, alyssum homolocarpum seed gum, and combinations thereof.

[0048] The inclusion shell may contain approximately 90% to 100% by weight, optionally approximately 95% to 100% by weight, or optionally approximately 99% to 100% by weight of inorganic material. The inorganic material is selected from the group consisting of metal oxides, metalloid oxides, metals, minerals, and mixtures thereof, and may optionally consist of SiO2, TiO2, Al2O3, ZrO2, ZnO2, CaCO3, Ca2SiO4, Fe2O3, Fe3O4, clay, gold, silver, iron, nickel, copper, and mixtures thereof, or optionally selected from the group consisting of SiO2, TiO2, Al2O3, CaCO3, and mixtures thereof, and may optionally be SiO2. The inclusion shell is a first shell component comprising a condensation layer and a nanoparticle layer, wherein the condensation layer comprises a precursor condensation product, and the nanoparticle layer comprises inorganic nanoparticles, and the condensation layer may comprise a second shell component disposed between the core and the nanoparticle layer and surrounding the first shell component, wherein the second shell component surrounds the nanoparticle layer. The inclusion may be any of the inclusions described in U.S. Patent Application Publications 2020 / 0330948(A1), 2020 / 0330949(A1), and 2020 / 0330950(A1), and U.S. Patent Application No. 63 / 092,829.

[0049] The fragrance may contain one or more plant-derived fragrances. Plant-derived fragrances are concentrated hydrophobic liquids containing volatile chemical compounds extracted from plants. Plant-derived fragrances include allspice berry, angelica seed, anise seed, basil, bay laurel, bay, bergamot, blood orange, camphor, caraway seed, cardamom seed, carrot seed, cassia, catnip, cedarwood, celery seed, German chamomile, Roman chamomile, cinnamon bark, cinnamon leaf, citronella, clary sage, clove bud, coriander seed, cypress, elemi, eucalyptus, fennel, fir needle, frankincense, geranium, ginger, pink grapefruit, helichrysum, hops, hyssop, juniper berry, labdanum, lavender, lemon, and lemongrass. The following may be selected: lime, magnolia, mandarin, marjoram, melissa, mugwort, myrrh, myrtle, neroli, niaouli, nutmeg, sweet orange, oregano, palmarosa, patchouli, pennyroyal, pepper black, peppermint, petit green, pine needles, radiata, ravensara, rose, rosemary, rosewood, sage, sandalwood, spearmint, spikenard, spruce, star anise, sweet annie, tangerine, tea tree, thyme red, verbena, vetiver, wintergreen, wormwood, yarrow, ylang-ylang extra, and ylang-ylang III, as well as mixtures thereof.

[0050] The particles may contain approximately 0.1% to 20% by weight of fragrance, optionally approximately 0.1% to 15% by weight, optionally approximately 0.1% to 12% by weight, optionally approximately 1% to 15% by weight, optionally approximately 2% to 20% by weight, or optionally approximately 8% to 10% by weight of fragrance.

[0051] Fragrance emulsion composition The fabric care beneficial agent may be a fragrance emulsion composition. The fragrance emulsion composition may comprise an amino-functional silicone having one or more primary amine moieties and a total amine content of about 0.05 to about 2.2, one or more emulsifiers, one or more fragrance raw materials having aldehyde moieties, ketone moieties, or a combination thereof, and water.

[0052] The fragrance emulsion composition may be one of those described in European Patent Office application No. 20156010.9, filed on February 7, 2020.

[0053] Amino-functional silicones are as follows: (a) Total amine content of approximately 0.071 to approximately 2.14, or approximately 0.071 to approximately 1.78, or approximately 0.71 to approximately 1.43, or approximately 0.14 to approximately 1.07, or approximately 0.14 to approximately 0.71, or approximately 0.21 to approximately 0.71, or approximately 0.36 to approximately 0.71, and / or (b) 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 (c) The ratio of primary amine content to total amine content may be approximately 1:2 to approximately 1:1, preferably approximately 1.2:2, more preferably approximately 1.5:2, or even more preferably approximately 1.8:2.

[0054] Amino-functional silicones are defined by the following formula: [R1R2R3SiO 1 / 2 ] (j+2l+2) [R4R5SiO 2 / 2 ] m [R6SiO 3 / 2 ] j [SiO 4 / 2 ] l (In the formula, j is an integer between 0 and 150, preferably between 0 and 50, more preferably between 0 and 20. m is an integer between 10 and 1500, preferably between 10 and 1000, more preferably between 20 and 500. l is an integer between 0 and 150, preferably between 1 and 150, more preferably between 0 and 50, and most preferably between 0 and 20. However, j+m+l is equal to an integer greater than or equal to 50. Each of the R1, R2, R3, R4, R5, and R6 sections independently contains H, OH, and C1-C. 32 Alkyl, C1-C 32 Substitutive alkyl groups, C6-C 32 Aryl, C5~C 32 Substituting aryls, C6~C 32 Alkylaryl, C6~C 32 Substituted alkylaryls, C1-C 32 Alkoxy, and C1-C 32 A substituted alkoxy and XZ are selected from the group, and at least one of the subgroups R1 to R6 is XZ. Preferably, each R 1~6 However, independently selected from the group consisting of OH, C1-C2 alkyl, C1-C2 substituted alkyl, C1-C2 alkoxy, C1-C2 substituted alkoxy, and XZ, In the formula, each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing 2 to 12 carbon atoms, preferably each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing 2 to 6 carbon atoms, most preferably each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing 2 to 4 carbon atoms. In the formula, each Z is a part containing one or more primary amine moieties, Preferably, each Z may be independently selected from the group -NH2, -N(H)-X-NH2, or a mixture thereof.

[0055] The emulsion composition has the following properties (a) to (d): (a) The silicone emulsion contains approximately 10% to 70% by weight, or approximately 25% to 65% by weight, or approximately 50% to 65% by weight of an amino-functionalized silicone, and / or (b) The emulsion contains approximately 30% to 90% by weight of water, or approximately 35% to 75% by weight, or approximately 35% to 50% by weight, and / or (c) characterized by a viscosity of about 10 to about 500 Pa·s, preferably about 20 to about 400 Pa·s, more preferably about 25 to about 300 Pa·s, and / or, measured at 0.1 rad / s and 25°C, and / or (d) The plurality of droplets may be characterized by at least one of the following: the plurality of droplets having an average diameter of about 1 micron to about 5 microns.

[0056] One or more flavoring ingredients are as follows: a. Oncidal, methyl nonylacetaldehyde, adoxal, melanal, calypsone, or mixtures thereof; b. Cumin aldehyde, benzaldehyde, anisaldehyde, heliotropin, isocyclocitral, tripral / ligustral, 3,6-ivy carbaldehyde, ligustral, centenal, or mixtures thereof; c. Satinaldehyde (jasmorange), otropal, cyclamen homoaldehyde, cyclamen aldehyde (cyclamal), lilial, canthoxal, floralozone, cinnamic aldehyde, or mixtures thereof; d. Delta-damascone, beta-damascone, alpha-damascone, nectaril, or mixtures thereof; e. Vanillin, ethyl vanillin, or a mixture thereof; or The materials may include a combination of materials selected from at least two categories of fa, b, c, d, and e.

[0057] One or more emulsifiers may include a nonionic surfactant, preferably the nonionic surfactant includes an alkoxylated fatty alcohol, and more preferably the one or more emulsifiers are characterized by an HLB value of about 5 to about 20, preferably about 8 to about 16.

[0058] One or more emulsifiers include a first emulsifier and a second emulsifier different from the first emulsifier, preferably the first emulsifier is a linear nonionic surfactant and / or preferably the second emulsifier is a branched nonionic surfactant.

[0059] Fabric softening The fabric care active beneficial agent may be a fabric softening active substance. 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 one described in U.S. Patent Application 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-(tall-oiloxyethyl)-N,N-methylhydroxyethylammonium methyl sulfate.

[0060] The fabric softening activating agent may be an aliphatic amine. The particles may contain about 8% to about 45% by weight of an aliphatic amine. The aliphatic amine may be one of those described in U.S. Patent Application Publication 2020 / 0354652(A1).

[0061] The fabric softening activating agent may be silicone. The particles may contain about 1% to about 50% by weight of silicone. The silicone may be one described in U.S. Patent Application Publication No. 2017 / 0349865.

[0062] Branched polyester The fabric care active beneficial agent may be branched polyester. The particles may contain about 5% to about 45% by weight of branched polyester. The branched polyester may be the one described in U.S. Patent Application Publication 2019 / 0367841(A1). The branched polyester may be the one described and claimed in U.S. Patent Application Publication 2019 / 0233764(A1).

[0063] Cationic polymers The fabric care active beneficial agent may be a cationic polymer. The particles may contain about 0.1% to about 10% by weight of the cationic polymer. The cationic polymer may be selected from the group consisting of cationic polysaccharides, 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 hydroxyethylcellulose reacted with an epoxide substituted with a trimethylammonium group.

[0064] enzyme The fabric care active beneficial agent may be an enzyme. The particles may contain about 0.0001% to about 5% by weight of enzyme. The enzyme may be selected from the group consisting of proteases, xyloglucanases, mannanases, and combinations thereof. The enzyme may be one of those described in U.S. Patent Application Publications 2017 / 0260481(A1) and 2017 / 0260482(A1).

[0065] Graft copolymer The fabric care active beneficial agent may be a graft copolymer. The particles may contain about 1% to about 75% by weight of the graft copolymer. The graft copolymer may be one described in U.S. Patent Application No. 69 / 951,274. The graft copolymer may be one described in U.S. Patent Application No. 69 / 722,492.

[0066] Antioxidant Fabric care beneficial agents may be antioxidants. The particles may contain about 0.2% to about 2% by weight of antioxidants. The antioxidants can be dispersed in the matrix of the water-soluble carrier. The antioxidants may be those described in U.S. Patent Application No. 63 / 034,766. The antioxidants may be butylated hydroxytoluene.

[0067] Apparatus and process for forming particles An apparatus 1 for forming particles is shown in Figure 1. The precursor material 20 may be a melt of any of the compositions disclosed herein for the particles 90. The precursor material 20 may contain more than about 20% by weight of a water-soluble carrier. The precursor material 20 may contain more than about 20% by weight of a water-soluble polymer. The precursor material 20 may contain about 20% to about 99% by weight of a water-soluble carrier. The precursor material 20 may contain about 20% to about 99% by weight of a water-soluble polymer.

[0068] The precursor material 20 may contain polyethylene glycol having a weight-average molecular weight of approximately 2000 to approximately 13000 in more than approximately 20% by weight, optionally more than approximately 40% by weight, and a fragrance in an amount of approximately 0.1% to approximately 20% by weight.

[0069] Raw materials may be supplied to a batch mixer 10. The batch mixer 10 may have sufficient capacity to hold the volume of supplied raw materials for a residence time sufficient to allow for a desired level of mixing or reaction of the raw materials. Materials leaving the batch mixer 10 may be precursor materials 20. Optionally, precursor materials may be supplied to the feed pipe 40 from some other upstream mixing process, such as in-line mixing or in-line static mixing. The precursor materials 20 may be a molten material. The batch mixer 10 may be a dynamic mixer. A dynamic mixer is a mixer to which energy is applied to mix the contents of the mixer. The batch mixer 10 may include one or more impellers for mixing the contents within the batch mixer 10.

[0070] Between the batch mixer 10 and the distributor 30, which may be present if desired, the precursor material 20 may move through the supply pipe 40. The supply pipe 40 may be in fluid communication with the batch mixer 10. One or more gas supply lines 155 may be provided to be in fluid communication with the supply pipe 40 downstream of the batch mixer 10. One or more gas supply lines 155 may be provided to be in fluid communication with the supply pipe 40 between the batch mixer 10 and the distributor 30. A mill 200 may be provided downstream of one or more gas supply lines 155 and in the line of the supply pipe 40. A mill 200 may be provided downstream of one or more gas supply lines 155 and in the line of the supply pipe 40 upstream of the distributor 30.

[0071] The precursor material 20 can be supplied to the supply pipe 40. The supply pipe 40 is a transport means for carrying the precursor material 20. The supply pipe 40 includes a transport means between the elements of the apparatus 1 and the transport means for carrying the precursor material within the elements of the apparatus 1. For example, a mill 200 may be located within a unit comprising a portion of the transport means entering the mill 200 and a portion of the transport means exiting the mill 200. Each of these portions is part of the supply pipe 40. Thus, the supply pipe 40 can be considered as the entire transport means between the batch mixer 10 and the distributor 30, with various elements along the supply pipe 40, such as one or more gas supply lines 155, the mill 200, the intermediate mixer 50, and the supply pump 140. If there is no batch mixer 10 upstream of the supply pipe 40, the supply pipe 40 can be considered as the entire transport system upstream of the distributor 30, and along the supply pipe 40 there are various elements such as one or more gas supply lines 155, a mill 200, an intermediate mixer 50, and a supply pump 140.

[0072] The intermediate mixer 55 may be located downstream of the mill 200 and in the line of the supply pipe 40. The intermediate mixer 55 may be a static mixer 50. The intermediate mixer 55 may be in fluid communication with the supply pipe 40 between the mill 200 and the distributor 30. The intermediate mixer 55, which may be a static mixer 50, may be located downstream of the batch mixer 10. In other words, if used, the batch mixer 10 may be located upstream of the intermediate mixer 55 or the static mixer 55. The intermediate mixer 55 may be in the line of the supply 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 a driven in-line fluid disperser. The intermediate mixer 55 may be an Ultra Turrax disperser, Dispax-reactor disperser, Colloid Mill MK, or Cone Mill MKO, available from IKA (Wilmington, North Carolina, United States of America). The intermediate mixer 55 may be a perforated disc mill, a toothed colloid mill, or a DIL inline homogenizer available from FrymaKoruma (Rheinfelden, Switzerland). The static mixer 50 may be a helical static mixer. The static mixer 50 may be a Kenics KMS 6 (1.905 cm inner diameter) available from Chemineer (Dayton, OH, USA).

[0073] While not bound by theory, it is conceivable that an intermediate mixer 55, such as a static mixer 50, can provide a more uniform temperature of precursor material 20 within the distributor 30 or stator 100. At the downstream end of the intermediate mixer 55 or, if used, the static mixer 50, the temperature of the precursor material 20 in the supply pipe 40 across the entire cross-section of the supply pipe 40 perpendicular to the direction of flow may vary by less than approximately 10°C, or less than approximately 5°C, or less than approximately 1°C, or less than approximately 0.5°C.

[0074] If a static mixer 50 is not present, the temperature across the entire cross-section of the supply pipe 40 perpendicular to the flow direction may be non-uniform. The temperature of the precursor material 20 at the centerline of the supply pipe 40 may be higher than the temperature of the precursor supply material 20 at the circumferential wall of the supply pipe 40. When the precursor material 20 is discharged to the distributor 30 or stator 100, the temperature of the precursor material 20 may vary at different locations within the distributor or stator 100. Although not bound by theory, it is believed that by using a static mixer 50 as described in this specification, a uniform temperature can be provided across the entire cross-section of the supply pipe 40, thereby enabling the production of more uniform particles 90 compared to apparatus 1 without a static mixer 50.

[0075] The distributor 30 may be provided with a plurality of holes 60. The precursor material 20 can pass through the holes 60. After passing through the holes 60, the precursor material 20 may be deposited on a moving conveyor 80 located below the distributor 30. The precursor material 20 may be deposited on the moving conveyor 80 as the conveyor 80 moves. The conveyor 80 may be translationally movable relative to the distributor 30. The conveyor 80 may be a continuous moving conveyor 80. The conveyor 80 may be an intermittent moving conveyor 80. A continuous moving conveyor 80 may provide a higher processing speed. An intermittent moving conveyor 80 may allow for better control over the shape of the particles 90 produced.

[0076] The precursor material 20 can be cooled on the moving conveyor 80 to form a plurality of solid particles 90. Cooling can be provided by ambient cooling. If desired, cooling can be provided by spraying room temperature water or cold water on the underside of the conveyor 80.

[0077] Once the particles 90 have achieved sufficiently high cohesiveness, they may be transferred from the conveyor 80 to a processing device located downstream of the conveyor 80 for further processing and / or packaging.

[0078] The distributor 30 may be a cylinder 110 rotatably mounted around the stator 100 (which is in fluid communication with the supply pipe 40), but the cylinder 110 may have an outer surface 120, the outer surface 120 may have a plurality of holes 60 as shown in Figure 2. Thus, the apparatus 1 may include a stator 100 that is in fluid communication with the supply pipe 40. After the precursor material 20 has passed through the mill 200, the supply pipe 40 can supply the precursor material 20 to the stator 100.

[0079] The apparatus 1 may include a cylinder 110 rotatably mounted around a stator 100. The stator 100 is supplied with precursor material through one or both ends 130 of the cylinder 110. The cylinder 110 may have a longitudinal axis L passing through it, but the cylinder 110 rotates around it. The cylinder 110 has an outer surface 120. The outer surface 120 of the cylinder 110 may have a plurality of holes 60.

[0080] Since the cylinder 110 is rotationally driven around its longitudinal axis L, the bore 60 can intermittently fluidize the stator 100 as the cylinder 110 rotates around the stator 100. The cylinder 110 can be considered to have a mechanical direction MD in the direction of movement of the outer surface portion 120 that spans the stator 100, and a mechanical transverse direction on the outer surface portion 120 perpendicular to the mechanical direction MD. The stator 100 can similarly be considered to have a mechanical transverse direction CD parallel to its longitudinal axis L. The mechanical transverse direction of the stator 100 can be aligned with the mechanical transverse direction of the cylinder 110. The stator 100 may have a plurality of distribution ports 122 located in the mechanical transverse direction CD of the stator 100. The distribution ports 122 are portions or regions of the stator 100 to which the precursor material 20 is supplied.

[0081] Generally, the precursor material 20 can be supplied to the stator 100 by passing it through one or more gas supply lines 155 via the mill 200 and the supply pipe 40. The stator 100 distributes the precursor material 20 across the entire operating width of the cylinder 110. As the cylinder 110 rotates around its longitudinal axis, the precursor material 20 is supplied through the holes 60 as they pass the stator 100. Individual chunks of precursor material 20 are supplied through each hole 60 as each hole 60 encounters the stator 100. The chunks of precursor material 20 supplied through each hole 60 as each hole 60 passes the stator 100 can be controlled by controlling the viscosity of the precursor material 20 by controlling either or both the pressure of the precursor material in the stator 100 and / or the rotational speed of the cylinder 110, or by controlling the temperature of the precursor material 20.

[0082] A small amount of precursor material 20 is deposited onto the conveyor 80 across the entire operating width of the cylinder 110. The conveyor 80 may be movable parallel to the longitudinal axis of the cylinder 110. The speed of the conveyor 80 can be set relative to the tangential speed of the cylinder 110 to control the shape of the precursor material 20 when it is deposited on the conveyor 80. The speed of the conveyor 80 may be approximately the same as the tangential speed of the cylinder 110.

[0083] As shown in Figure 1, the flow rate of precursor material 20 through the supply pipe 40 may be provided by the flow rate provided by gravity from the batch mixer 10 and the distributor 30. To improve the controllability of the production, the apparatus 1 may be provided with a supply pump 140, as shown in Figure 2. The supply pump 140 may be located in the line of the supply pipe 40, where "in the line" means in the flow line of the precursor material 20. The supply pump 140 may be between the batch mixer 10 and the distributor 30. The supply pump 140 may be upstream of the distributor 30. If a stator 100 is used, the supply pump 140 may be located in the line of the supply pipe 40, where "in the line" means in the flow line of the precursor material 20. If a stator 100 is used, the supply pump 140 may be between the batch mixer 10 and the stator 100. The supply pump 140 may be upstream of the stator 100. When describing the location of the supply pump 140, the phrase "between" is used to indicate that the supply pump 140 is located downstream of the batch mixer 10 in the line and upstream of the distributor 30, or upstream of the stator 100 if one is used.

[0084] One or more gas supply lines 155 and mills 200 may be located in the line between the supply pump 140 and the distributor 30 or stator 100 (if used in device 1).

[0085] The flow rate of the precursor material 20 may be approximately 3 L / min. The precursor material 20 may be a molten material containing either the precursor material 20 or any of the compositions described herein for the particles 90.

[0086] Apparatus 1 may include one or more gas supply lines 155. A single gas supply line 155 may be practical if the gas to be mixed with the precursor material can actually be supplied through a single gas supply line 155. 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 can be supplied within a single container 157. For example, a mixture of argon, carbon dioxide, and nitrogen can be supplied within a gas cylinder. Optionally, the gas mixture can be supplied continuously from the environment via a reaction process or by combining air with another gas supplied from the container. The gas can be pressurized via a compressor.

[0087] One or more gas supply lines 155 may include a flow regulator 158. The flow regulator 158 can adjust the flow rate of gas to the supply line 40. The volume of added gas per unit volume of precursor material 20 can be controlled by setting the flow regulator 158 to a desired flow rate. Supplying more gas to the precursor material 20 in the supply line 40 will result in more gas being contained in the particles 90. One or more gas supply lines 155 may be provided to mix gas with the precursor material 20.

[0088] The flow regulator 158 may be a Key Instruments Flo-Rite Series GS 65mm (part number 60410-R5). The supply line 40 may be a 1 1 / 2 inch stainless steel sanitary pipe. The gas supply line 155 may be a 1 / 4 inch inner diameter polyethylene pipe. The gas may be supplied through the gas supply line 155 at a pressure greater than approximately 4 bar, for example, 5.9 bar.

[0089] If two or more gas supply lines 155 are connected separately to the supply pipe 40, flow regulators may be provided along each gas supply line 155 to adjust the flow rate of gas in each gas supply line 155. If a mixture of gases is introduced into the supply pipe 40 via a single gas supply line 155, a single flow regulator 158 may be practical.

[0090] An injection quill device for introducing gas may be provided at the connection point between the gas supply line 155 and the supply pipe.

[0091] The gas may be supplied at a temperature and pressure such that a desired volume of the gas is present within the particle 90 when the gas reaches ambient temperature and pressure. The desired delivery temperature and pressure may be determined using the law of ideal gases. The gas may also contain water. The water may be in gaseous or liquid form. The amount of water in the gas may be selected to reach a desired level.

[0092] The Mill 200 could be a rotor-stator type mill. The mill could be a Quadro Z1 inline mixer with a single-stage medium rotor-stator operating at approximately 400 RPM.

[0093] The mill 200 and one or more gas supply lines 155 may be incorporated into a single unit.

[0094] The gas supply line 155, flow regulator 158, and mill 200 may be provided as a single unit using an Oakes Foamer (2MT1A continuous former manufactured by ETOakes Corporation (686 Old Willets Path Hauppauge, NY 11788)).

[0095] The apparatus 1 as seen from the machine direction MD is shown in Figure 3. As shown in Figure 3, the apparatus 1 may have an operating width W, and the cylinder 110 may rotate around the longitudinal axis L.

[0096] The apparatus 1 for forming particles 90 may include a supply pipe, one or more gas supply lines 155 installed to be in fluid communication with a supply pipe 40 located downstream of a batch mixer 10, a mill 200 located downstream of one or more gas supply lines 155 and in the line of the supply pipe 40, and a distributor 30 located downstream of the mill 200 and in fluid communication with the supply pipe 40, the distributor 30 comprising a plurality of holes 60. The apparatus 1 may include a conveyor located below the distributor 30 and translatable relative to the distributor 30. The distributor 30 may include a stator 100 in fluid communication with the supply pipe 40. The distributor 30 may include a cylinder 110 that is rotatably mounted around the stator 100 and rotatable around the longitudinal axis L of the cylinder 110. The cylinder 110 may have an outer surface 120, and the cylinder 110 may have a plurality of holes 60 arranged around the outer surface 120. The hole 60 can intermittently communicate fluidly with the stator 100 as the cylinder 110 rotates around the stator 100. The apparatus may include a conveyor 80 below the cylinder 110, which may be translationally translatable with respect to the longitudinal axis L. The apparatus 1 for forming the particles 90 may include a batch mixer 10. The supply pipe 40 can communicate fluidly with the batch mixer 10.

[0097] The process for forming particles 90 may include the steps of: supplying a precursor material 20 to a supply pipe 40; mixing a gas into the precursor material 20, wherein the gas contains approximately 50% to approximately 100% by volume, optionally approximately 55% to approximately 100% by volume, optionally approximately 60% to approximately 100% by volume, optionally approximately 70% to approximately 100% by volume, optionally approximately 80% to approximately 100% by volume, optionally approximately 90% to approximately 100% by volume, or optionally 100% by volume of argon; providing a distributor 30 having a plurality of holes 60; moving the precursor material 20 from the supply pipe 40 to the distributor 30; passing the precursor material 20 through the holes 60; providing a movable conveyor 80 below the holes 60; accumulating the precursor material 20 on the movable conveyor 80; and cooling the precursor material 20 to form a plurality of particles 90.

[0098] The gas can be mixed with the precursor material 20 as a mixture of gases. For example, the gas mixture can be directed to the precursor material 20 via a single gas supply line 155. The gas mixture may contain 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 components. The mixture can be supplied from a container 157 containing the gas mixture. For example, the container 157 may be a gas cylinder filled with the desired gas, which is a mixture of different gases.

[0099] Optionally, argon may be supplied from a primary container 157a, and other components of the gas may be supplied from one or more secondary containers 157b (Figure 4). The primary container 157a and secondary containers 157b can be supplied to a single gas supply line 155. A flow regulator 158 can control the flow of gas from the primary container 157a and secondary containers 157b into the gas supply line 155. Optionally, an in-line mixer may be provided in or upstream of the gas supply line 155 to mix the gases from the primary container 157a and secondary containers 157b.

[0100] The primary container 157a may contain argon. Other components of the gas may be supplied from the secondary container 157b. Other components of the gas may be supplied from the secondary container 157b as air or carbon dioxide. Air containers and carbon dioxide containers are readily available commercially. Similarly, argon containers are readily available commercially. The operator of apparatus 1 can obtain argon cylinders and air cylinders and set the flow regulator 158 to supply the desired gas. The argon and other components of the gas may be combined before being mixed with the precursor material 20 to form a single flow of gas.

[0101] Optionally, the primary container 157a can supply gas to the primary gas supply line 155, and the secondary container 157b can supply gas to the secondary gas supply line 155. The gas flow in each gas supply line 155 can be regulated by a flow regulator 158 dedicated to such gas supply line 155.

[0102] During operation, it may be practical to supply the precursor material 20 into the supply pipe at an operating pressure of approximately 2 bar to approximately 8 bar. The gas can be supplied to the supply pipe 40 at a pressure higher than the operating pressure of the supply pipe 40. The gas or its argon component can be mixed in at a pressure of approximately 3 to approximately 4 bar, or even more than approximately 4 bar, or even more than approximately 5 bar.

[0103] The solubility of argon in the precursor material 20 can be greater than the solubility of most of the volume of the other components of the gas. When argon gas is supplied to a flow of precursor material 20 at the operating pressure, the argon is solubilized in the precursor material 20. The other components of the gas may or may not be solubilized in the precursor material 20 at the operating pressure. Those components that have low solubility in the precursor material 20 relative to argon mainly remain in the precursor material 20 as bubbles.

[0104] As the precursor material 20 passes through the hole 60, the pressure decreases toward or to atmospheric pressure. The precursor material 20 may also begin to cool. The precursor material 20 may continue to cool as it moves from the hole 60 to the movable conveyor 80. Cooling continues after the precursor material 20 is deposited on the movable conveyor 80. The conveyor removes heat from the precursor material 20, and the belt-facing side of the precursor material 20 in contact with the movable conveyor 80 begins to solidify. Similarly, the surface of the precursor material 20 continues to cool even after the precursor material 20 is deposited on the movable conveyor 80. Thus, once deposited on the movable conveyor 80, the cooling of the precursor material 20 is a three-dimensional time-dependent process.

[0105] As the molten precursor material 20 cools, a solidified forefront develops from the belt-facing side of the precursor material 20, and this solidified forefront moves forward away from the movable conveyor 80 over time. The air-facing side of the precursor material 20, away from the belt-facing surface, also cools as a function of time. This results in a solidified forefront that moves forward from the air-facing surface towards the center of the particles formed on the movable conveyor 80 as the precursor material 20 cools.

[0106] If the gas mixed into the precursor material 20 is air, consisting of approximately 78 vol% nitrogen, 21 vol% oxygen, 0.93 vol% argon, and 0.03 vol% carbon dioxide, then the majority of the gas has limited solubility in the precursor material 20, and the air remains as bubbles in the precursor material 20 throughout the particle-forming process. This limits the amount of air that can be mixed into the precursor material 20, while still allowing for the production of particles with 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 forward solidification portion 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 bubbles are driven upward, they can coalesce to form larger bubbles. Some bubbles may 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 layer is formed on the air-facing side of the precursor material 20, bubbles may be ejected through the skin layer, resulting in particles 90 with a physically unstable outer surface. A physically unstable outer surface is undesirable because it can cause the particles to detach easily and make them difficult to use.

[0107] A problem associated with using air as the mixing gas is that when the precursor material 20 is deposited on the movable belt 40, bubbles are present within the precursor material 20, causing the phenomenon described in the preceding paragraph, which can result in the production of insufficient particles 90. Surprisingly, by using a gas containing argon in amounts of approximately 50% to 100% by volume, optionally approximately 55% to 100% by volume, optionally approximately 60% to 100% by volume, optionally approximately 70% to 100% by volume, optionally approximately 80% to 100% by volume, optionally approximately 90% to 100% by volume, and optionally 100% by volume, the ability of the precursor material 20 to retain bubbles can be improved when the precursor material 20 is cooled on the movable conveyor 80 to form particles 90. This can result in particles 90 with higher porosity and fewer large bubbles on or near the air-facing surface of the particles 90.

[0108] Argon may be relatively soluble in the precursor material 20 compared to other gas components. Gas components that are relatively insoluble in the precursor material 20 may exist as bubbles. When the working pressure on the precursor material is released to or toward ambient pressure, argon exits the solution. The process of argon exiting the solution from the precursor material 20 is a time-dependent process. Bubbles of gas components that are relatively insoluble in the precursor material 20, if present, can act as nucleation sites for argon exiting the solution from the precursor material. While argon exits the solution, the precursor material 20 is also cooled. As previously described, the leading edge of solidification may develop from the side of the precursor material 20 facing the belt, and the side of the precursor material 20 facing the air is also solidified. The solidified or solidified precursor material 20 forms a barrier against bubbles escaping from the precursor material 20. As argon gradually emerges from the precursor material 20 and out of the solution, argon bubbles may form, and / or argon may emerge from the solution and enter existing bubbles of the relatively insoluble gaseous component. The delayed formation of argon bubbles, or the expansion of existing bubbles of the relatively insoluble gaseous component as argon nucleates on such bubbles, allows for the formation of larger volume bubbles in the precursor material 20, and these subsequently formed bubbles are less likely to escape from the precursor material 20. Once the precursor material 20 has completely solidified, the formed particles 90 may have large volume voids.

[0109] Gases containing argon in amounts of approximately 50% to 100% by volume, optionally approximately 55% to 100% by volume, optionally approximately 60% to 100% by volume, optionally approximately 70% to 100% by volume, optionally approximately 80% to 100% by volume, optionally approximately 90% to 100% by volume, and optionally 100% by volume, may be more favorable than air or gases containing more than approximately 50% by volume of carbon dioxide. Bubbles escape from the solution and form in a time-dependent process as the dissolved gas contributes to the void volume of the solidified particles 90. In the case of bubble formation caused by changes in gas solubility as a function of pressure changes or depressurization nucleation, the rate of bubble formation decreases with solubility. The rate of bubble formation from depressurization using argon, which is partially soluble in the precursor material 20, can be much faster than the rate of bubble formation when using a relatively more soluble gas such as carbon dioxide. This may occur if the precursor material 20 contains more than about 20% by weight of a water-soluble polymer, or more specifically, polyethylene glycol having a weight-average molecular weight of about 2000 to about 13000.

[0110] If the rate of bubble formation from reduced-pressure nucleation is slower than the rate of solidification, a phase change will result in bubble formation. Bubble formation within the solidification precursor material 20 resulting from the phase change can cause the particle surface to burst, solidifying the expanding molten material on the particle surface. This is an undesirable aesthetic for the particles 90 and may also lead to the accumulation of broken particles 90 within the product package, which is also undesirable. With respect to particles formed by the distributor 30, which essentially keeps the molten precursor material 20 under pressure until the molten precursor material 20 is released from the distributor 30, an acceptable gas may be one that provides partial solubility to the molten precursor material 20 at atmospheric pressure and has a time-dependent nucleation rate during deposition of the precursor material 20 that is faster than the solidification rate of the precursor material 20 that ultimately forms the particles 90. For polyethylene glycol carriers having a weight-average molecular weight of about 2000 to about 13000 and where the pressure change through the distributor 30 is at least 3 bar, argon can provide these desired properties. Argon may be more advantageous than a blend of air and carbon dioxide because it partially dissolves in water-soluble polymers such as polyethylene glycol. Since the nitrogen portion of air has relatively low solubility in polyethylene glycol compared to argon, argon is far more soluble in polyethylene glycol than air at the same temperature and pressure. However, compared to carbon dioxide, argon has much lower solubility; the same amount of injected carbon dioxide dissolves almost completely at a line pressure of only 3 bar, while the same amount of argon only partially dissolves at 10 bar. The gases can be mixed at pressures of approximately 3 bar to approximately 10 bar.

[0111] particle The particles 90 may be formed as described herein and may contain about 25% to about 99% by weight of a water-soluble carrier. The particles 90 may further contain about 0.1% to about 20% by weight of a fabric care beneficial activator. Each particle may have a mass of about 5 mg to about 200 mg, preferably about 10 mg to about 100 mg, preferably about 20 mg to about 50 mg. The particles may have a hemispherical or compressed hemispherical shape.

[0112] Fabric care beneficial activators may be selected from the group consisting of amines, surfactants, nonionic surfactants, water binders, sulfites, fatty acids and / or salts thereof, enzymes, encapsulation beneficial agents, stain-releasing polymers, colorants, builders, chelating agents, stain transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleaching catalysts, bleaching activators, polymer dispersants, cyclodextrin complex beneficial agents, stain removers / anti-redeposition agents, encapsulation fragrances, polymer dispersants, polymer grease cleaners, whitening agents, antifoaming agents, dyes, colorants, free fragrances, structural elastochemicals, fabric softeners, quaternary amines, cured and softened tallows, carriers, fillers, hydrotropes, organic solvents, antimicrobial agents and / or preservatives, neutralizing agents and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structuring agents, opacifiers, pearl essences, pigments, corrosion inhibitors and / or colorfast agents, and mixtures thereof.

[0113] Fabric care beneficial activators may be selected from the group consisting of antimicrobial agents, antioxidants, fragrances, fabric conditioning agents, dyes, dyeing agents, and combinations thereof. Fabric care beneficial activators may be non-encapsulated or encapsulated fragrances.

[0114] Each of the particles 90 may have a mass of approximately 5 mg to approximately 200 mg, optionally approximately 10 mg to approximately 100 mg, or optionally approximately 20 mg to approximately 50 mg. The particles may have a hemispherical or compressed hemispherical shape.

[0115] Particles 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 using a pitch blade agitator. Butylated hydroxytoluene may be added to the mixer in an amount of about 0.01% by weight of the precursor material 20. An aqueous slurry of fragrance microcapsules may be added to the mixer in an amount of about 4% by weight of the precursor material 20. Unencapsulated fragrance may be added to the mixer in an amount of about 8% by weight of the precursor material 20. Dyes may be added to the mixer at a concentration of about 0.01% by weight of the precursor material 20. PEG may constitute the weight percentage of the remaining portion of the precursor material 20. The precursor material 20 may be mixed for 30 minutes.

[0116] The precursor material 20 may be formed into particles 90 using a SANDVIK ROTOFORM 3000 having a belt with a width of 750 mm and a length of 10 m. The cylinder 110 may have holes 60 with a diameter of 2 mm, set at a pitch of 10 mm in the machine transverse direction CD and at a pitch of 9.35 mm in the machine direction MD. The cylinder can be set approximately 3 mm above the belt. The belt speed and the rotation speed of the cylinder 110 can be set to 10 m / min.

[0117] After mixing the precursor material 20, the precursor material 20 can be extruded from the mixer 10 through the plate and flame heat exchanger set at a constant speed of 3.1 kg / min or even 4 kg / min, and the outlet temperature can be controlled to 50°C. The pressure in the feed pipe 40 downstream of the pump 140 can be about 2 to about 7 bar, or about 5.5 bar or about 5 bar, and this pressure is that in the feed pipe 40 downstream of the mill 200.

[0118] The gas may be mixed into the precursor material 20 at a volume flow rate ratio of precursor material to gas of approximately 1.3:1 to approximately 2.6:1, or even more precisely, approximately 1.3:1 to approximately 1.6:1. The gas pressure in the gas supply line 155 must be higher than the pressure in the supply pipe 40 to ensure the flow and mixing of the gas into the precursor material 20. The flow rate of the precursor material 20 may be approximately 4.5 liters / min, and the gas flow rate may be approximately 3.4 liters / min. The gas may be argon, a mixture of argon and carbon dioxide, or a mixture of argon and other relatively insoluble gases.

[0119] The precursor material 20 containing the mixed gas can be passed through a Quadro Z1 mill equipped with a medium rotor / stator element. After grinding, the precursor material can optionally be passed through a Kenics 1.905 cm KMS 6 static mixer 50 installed 91.44 cm upstream of the stator 100 of the rotoforming device.

[0120] combination: A. A process for forming particles, a. A step of supplying precursor material (20) to the supply pipe (40), b. A step of mixing a gas into the precursor material, wherein the gas contains approximately 50% to approximately 100% by volume, optionally approximately 55% to approximately 100% by volume, optionally approximately 60% to approximately 100% by volume, optionally approximately 70% to approximately 100% by volume, optionally approximately 80% to approximately 100% by volume, optionally approximately 90% to approximately 100% by volume, and optionally approximately 100% by volume of argon and approximately 0% to approximately 50% by volume of other components. c. A step of providing a distributor (30) having multiple holes (60), d. A step of moving the precursor material (20) from the supply pipe to the distributor, e. A step of passing the precursor material through the hole, f. A step of installing a movable conveyor (80) below the hole, g. A step of accumulating the precursor material on the movable conveyor, h. A process comprising the step of cooling the precursor material to form a plurality of particles (90). B. The said distributor a. A stator (100) that is in fluid communication with the supply pipe, b. The process according to paragraph A, comprising a cylinder (110) rotatably mounted around the stator and rotatable around the longitudinal axis (L) of the cylinder, wherein the cylinder has an outer surface (120), and the cylinder comprises a plurality of holes arranged around the outer surface, the holes intermittently fluidly communicating with the stator as the cylinder rotates around the stator. C. The process according to paragraph A or B, further comprising the step of grinding the precursor material after the step of mixing the gas with the precursor material. D. The process described in paragraph C, wherein the step of crushing the precursor material after the step of mixing gas into the precursor material is performed using an inline rotor stator mill. E. A process described in any one of paragraphs A to D, wherein the gas is introduced as part of a gas mixture. F. The process described in paragraph E, wherein the mixture of gases is from a container containing the mixture of gases. G. The process described in any one of paragraphs A to E, wherein the argon is supplied from a primary vessel (157a) and the other components of the gas are supplied from one or more secondary vessels (157b). H. The process described in paragraph G, wherein the argon and the other components of the gas are combined into a single flow of the gas before being mixed with the precursor material. I. The process described in paragraph H, wherein the other components of the gas are supplied as air from the secondary container. J. The process described in any one of paragraphs A to I, wherein the argon is mixed in at a pressure greater than 2 bar and at a minimum flow rate of approximately 0.5 liters / minute. The process described in any one of paragraphs A to J, wherein the other component present in an amount exceeding 50% by volume is less soluble in the precursor material than the argon. L. The process according to any one of paragraphs A to K, wherein the precursor material further comprises more than approximately 20% by weight of a water-soluble polymer. M. The water-soluble polymer is a. Formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (wherein x is 50-300, y is 20-100, and z is 10-200) polyalkylene polymer; b.Formula (C2H4O) q -C(O)O-(CH2) r -CH3 (wherein q is 20 to 200 and r is 10 to 30) polyethylene glycol fatty acid ester; c.Formula HO-(C2H4O) s -(CH2) t -CH3 (wherein s is 30-250 and t is 10-30) polyethylene glycol aliphatic alcohol ether; d. C8-C22 alkyl polyalkoxylates containing more than 40 alkoxylate units; e. Polyethylene glycol having a weight-average molecular weight of 2000 to 15000; f.EO / PO / EO block copolymer; g.PO / EO / PO block copolymer; h.EO / PO block copolymer; i.PO / EO block copolymer; j. Polypropylene glycol; Ethoxylated nonionic surfactants having an ethoxylation degree greater than k.30; l. Polyvinyl alcohol; The process described in paragraph L, selected from the group consisting of polyalkylene glycols having a weight-average molecular weight of 2000 to 15000, and mixtures thereof. N. The process according to any one of paragraphs A to M, wherein the precursor material comprises polyethylene glycol having a weight-average molecular weight of about 2000 to about 13000. O. The process according to any one of paragraphs A to N, wherein the precursor material contains more than approximately 40% by weight of polyethylene glycol. P. The process described in any one of paragraphs A to O, wherein the particles have an individual mass of approximately 0.1 mg to approximately 2 g. Q. The process described in any one of paragraphs A to P, wherein the precursor material contains approximately 0.1% to approximately 20% by weight of fragrance. R. The process described in paragraph Q, wherein the fragrance includes encapsulated fragrance. S. The process described in paragraph Q, wherein the fragrance includes encapsulated fragrances and unencapsulated fragrances. T. The process described in any one of paragraphs A to S, wherein the precursor material comprises about 0.1% to about 20% by weight of encapsulated fragrance. U. The process described in any one of paragraphs A to T, wherein the step of cooling the precursor material is performed by ambient cooling. V. The process described in any one of paragraphs A to U, wherein the precursor material is supplied from a batch mixer (10) to the supply pipe. W. The process described in any one of paragraphs A to V, wherein the other component is selected from the group consisting of oxygen, nitrogen, argon, and mixtures thereof. X. The precursor material may include amines, surfactants, nonionic surfactants, water binders, sulfites, fatty acids and / or their salts, enzymes, encapsulation beneficial agents, stain-releasing polymers, colorants, builders, chelating agents, stain transfer inhibitors, dispersants, enzyme stabilizers, catalyst materials, bleaching agents, bleaching catalysts, bleaching activators, polymer dispersants, cyclodextrin complex beneficial agents, stain removers / anti-redeposition agents, encapsulation fragrances, polymer dispersants, polymer grease-cleaning agents, whitening agents, antifoaming agents, and dyes. A process according to any one of paragraphs A to W, comprising a fabric care beneficial agent selected from the group consisting of colorants, free fragrances, structural elastochemicals, fabric softeners, quaternary amines, cured and softened animal fats, carriers, fillers, hydrotropes, organic solvents, antimicrobial agents and / or preservatives, neutralizing agents and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structuring agents, opacifiers, pearl essences, pigments, corrosion inhibitors and / or colorfast agents, and mixtures thereof. Y. The process described in any one of paragraphs A to X, wherein the gas is argon. Z. A process described in any one of paragraphs A to Y, wherein the gas is mixed in at a pressure of approximately 3 bar to approximately 10 bar.

[0121] The dimensions and values ​​disclosed herein should not be understood as being strictly limited to the exact numerical values ​​listed. Instead, unless otherwise specified, each such dimension is intended to mean both the listed value and the functionally equivalent range encompassing that value. For example, a dimension disclosed as "40 mm" is intended to mean "approximately 40 mm."

[0122] All documents referenced herein, including all patents or patent applications that are cross-referenced or related, and all patent applications or patents on which this application claims priority or benefit thereof, are incorporated herein by reference in their entirety unless expressly excluded or otherwise limited. No citation of any document shall be deemed prior art to any invention disclosed or claimed herein, nor shall it be deemed to teach, suggest or disclose any such invention, either alone or in combination with any one or more other references. Furthermore, in the event of any conflict between the meaning or definition of any term in this document and any meaning or definition of the same term in any document incorporated by reference, the meaning or definition given to the term in this document shall prevail.

[0123] While 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 can be made without departing from the spirit and scope of the invention. Therefore, it is intended that all such changes and modifications within the scope of the invention be covered in the appended claims. [1] A process for forming particles, A process of supplying precursor material (20) to a supply pipe (40), A step of mixing a gas into the precursor material, wherein the gas contains about 50% to about 100% by volume of argon and about 0% to about 50% by volume of other components. A step of providing a distributor (30) having multiple holes (60), A step of moving the precursor material (20) from the supply pipe to the distributor, The process of passing the aforementioned precursor material through the hole, A step of installing a movable conveyor (80) below the hole, A step of accumulating the aforementioned precursor material on the movable conveyor, A process comprising the step of cooling the precursor material to form a plurality of particles (90). [2] The aforementioned distributor, A stator (100) that is in fluid communication with the aforementioned supply pipe, The process according to [1], comprising a cylinder (110) rotatably mounted around the stator and rotatable around a longitudinal axis (L) of the cylinder, wherein the cylinder has an outer surface (120), the cylinder comprises the plurality of holes disposed around the outer surface, and the holes intermittently fluidly communicate with the stator as the cylinder rotates around the stator. [3] The process according to [1] or [2], further comprising the step of mixing gas with the precursor material, followed by the step of grinding the precursor material. [4] The process according to [3], wherein the step of crushing the precursor material after the step of mixing gas into the precursor material is performed using an inline rotor stator mill. [5] The process according to any one of [1] to [4], wherein the gas is mixed in as a mixture of gases. [6] The process according to [5], wherein the mixture of gases is from a container containing the mixture of gases. [7] The process according to any one of [1] to [6], wherein the argon is supplied from a primary vessel (157a) and the other components of the gas are supplied from one or more secondary vessels (157b). [8] The process according to [7], wherein the other components of the gas are supplied as air from the secondary container. [9] The process according to any one of [1] to [8], wherein the argon and the other components of the gas are combined into a single flow of the gas before being mixed with the precursor material.

[10] The process according to any one of [1] to [9], wherein the argon is mixed in at a pressure greater than 2 bar and at a minimum flow rate of about 0.5 liters / minute.

[11] The process according to any one of [1] to

[10] , wherein the other component in an amount exceeding 50% by volume is less soluble in the precursor material than the argon.

[12] The process according to any one of [1] to

[11] , wherein the precursor material comprises more than about 20% by weight of a water-soluble polymer.

[13] The aforementioned water-soluble polymer 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 50-300, y is 20-100, and z is 10-200) polyalkylene polymer; Formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 Polyethylene glycol fatty acid ester (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 aliphatic 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 having an ethoxylation degree greater than 30; Polyvinyl alcohol; A process described in

[12] , selected from polyalkylene glycols having a weight-average molecular weight of 2000 to 15000, and mixtures thereof.

[14] The process according to any one of [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 process according to any one of [1] to

[14] , wherein the other component is selected from oxygen, nitrogen, carbon dioxide, and mixtures thereof.

Claims

1. A process for forming particles, A step of supplying precursor material (20) to a supply pipe (40), A step of mixing a gas into the precursor material, wherein the gas contains 50% to 100% by volume of argon and 0% to 50% by volume of other components, and the mixed argon gas is solubilized. A step of providing a distributor (30) having multiple holes (60), A step of moving the precursor material (20) from the supply pipe to the distributor, A step of passing the precursor material through the hole, wherein the pressure of the precursor material that has passed through the hole of the distributor (30) decreases and the dissolved argon comes out, The steps include providing a movable conveyor (80) below the hole, A step of accumulating the aforementioned precursor material on the movable conveyor, A step of cooling the precursor material to form a plurality of particles (90), wherein the plurality of particles include the argon bubbles that have been released as voids, A process wherein the precursor material contains more than 20% by weight of a water-soluble polymer, and the water-soluble polymer is polyethylene glycol having a weight-average molecular weight of 2,000 to 13,000.

2. The aforementioned distributor, A stator (100) that is in fluid communication with the supply pipe, The process according to claim 1, comprising a cylinder (110) rotatably mounted around the stator and rotatable around its longitudinal axis (L), wherein the cylinder has an outer surface (120), the cylinder comprises the plurality of holes disposed around the outer surface, and the holes intermittently fluidly communicate with the stator as the cylinder rotates around the stator.

3. The process according to claim 1 or 2, further comprising the step of crushing the precursor material after the step of mixing the gas with the precursor material.

4. The process according to claim 3, wherein the step of crushing the precursor material after the step of mixing gas into the precursor material is performed using an inline rotor stator mill.

5. The process according to claim 1 or 2, wherein the gas is mixed in as a mixture of gases.

6. The process according to claim 5, wherein the mixture of gases is from a container containing the mixture of gases.

7. The process according to claim 1 or 2, wherein the argon is supplied from a primary container (157a), and the other components of the gas are supplied from one or more secondary containers (157b).

8. The process according to claim 7, wherein the other components of the gas are supplied as air from the secondary container.

9. The process according to claim 1 or 2, wherein the argon and the other components of the gas are combined into a single flow of the gas before being mixed with the precursor material.

10. The process according to claim 1 or 2, wherein the argon is mixed in at a pressure greater than 2 bar and at a minimum flow rate of 0.5 liters / minute.

11. The process according to claim 1 or 2, wherein the other component has lower solubility in the precursor material than the argon.

12. The process according to claim 1 or 2, wherein the other component is selected from oxygen, nitrogen, carbon dioxide, and mixtures thereof.

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