Process for forming particles

Abstract

A process for forming particles, comprising: mixing a gas into a precursor material, the gas comprising about 50% to about 75% by volume carbon dioxide and about 25% to about 50% by volume of other components; depositing the precursor material on a moving conveyor; and cooling the precursor material to form a plurality of particles.

Description

[Technical field]

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

[0002] Consumers want products that can simplify the process of using to do laundry, can help reduce the time spent on handling dirty laundry, and can help achieve high levels of benefits.Consumers are in a good position to understand the amount of fabric care composition that is needed to provide the benefits they desire.As a result, fabric care products that allow consumers to customize the amount of fabric care composition used are favored by many consumers.

[0003] Fabric care products that can be dispensed in the wash liquor are particularly easy for the consumer to use: for example, a consumer can simply place the fabric care product in the washing machine tub along with the laundry and start the washing machine cycle.

[0004] Typically, consumers use fabric care detergent compositions that contain significant amounts of surfactants and other cleaning ingredients. Such fabric care compositions are often provided in soluble unit dose pouches with a predetermined amount of fabric care actives. 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 can be referred to as fully formulated fabric care compositions.

[0005] Additive fabric care products are popular with consumers to provide fabric care benefits beyond those that can be provided by using fully formulated fabric care compositions.Consumers enjoy and are satisfied with using packaged fabric care additives in a manner that allows consumers to use custom amounts of fabric care additives based on the consumer's judgment of how much fabric care additive is needed to provide the desired benefits.Such fabric care additives are conveniently provided throughout the wash with the fully formulated fabric care composition, but are dispensed separately from the fully formulated fabric care composition.

[0006] Fabric care additives in the form of particles have become attractive to many consumers. Some fabric care additive particles are provided with a porous structure. Particles with a porous structure can float in water when the washing liquor is formed. Floating particles may tend to dissolve more completely in the wash compared to sinking particles, since sinking particles may be trapped in the folds, wrinkles, and pockets of laundry during washing. Undissolved particles tend to incompletely deliver the fabric care benefit actives contained in the particles, which may be undesirable for consumers. Floating, non-encapsulated perfume-containing particles can provide a pleasant scent to the head space above the washing liquor and the room where the washing machine is located. Furthermore, floating particles can better distribute the fabric care additive to the laundry during the wash cycle.

[0007] Melt processing is a common technique for forming particles. One problem with creating porous particles via a melting process is that as the molten precursor material solidifies, gas bubbles in 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 irregular rough outer surface, an irregular distribution of pore sizes within the solidified particle, and bubbles and molten material erupting from the surface of the particle as it solidifies. Such particles may be less durable than particles that have a more competent outer surface, are more prone to becoming dusty and difficult to use, and appear to be of poor quality. The tendency of gas bubbles in the melt to coalesce and rise out of the molten material as the molten precursor material solidifies can also effectively limit the volume of pores that can be provided in the particle without these adverse effects. Summary of the Invention [Problem to be solved by the invention]

[0008] In view of these limitations, there is a continuing unmet need for fabric care additives in the form of particles that have a uniform distribution of pore sizes throughout the particle. Additionally, there is a need for processes for forming such porous particles. [Means for solving the problem]

[0009] 1. A process for forming particles, the process comprising: supplying a precursor material to a supply tube; mixing a gas with the precursor material, the gas comprising about 50% to about 75% by volume carbon dioxide and about 25% to about 50% by volume of other components; providing a distributor having a plurality of holes; moving the precursor material from the supply tube to the distributor; passing the precursor material through the holes; providing a moving conveyor below the holes; depositing the precursor material on the moving conveyor; and cooling the precursor material to form a plurality of particles. [Brief description of the drawings]

[0010] [Figure 1] An apparatus for forming particles. [Diagram 2] A portion of an apparatus for forming particles. [Diagram 3] FIG. 2 is an end view of an apparatus for forming particles. [Figure 4] Part of an apparatus for forming particles. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0011] Water-soluble carrier The particles, and thus 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 carry the capsules to the wash liquor. When the water-soluble carrier dissolves, the capsules are dispersed in the wash liquor and adhere to the laundry.

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

[0013] Water soluble means that the material, carrier substance, or particle is soluble or dispersible in water and optionally has at least 50%, optionally at least 75%, or even at least 95% water solubility as measured by the method hereafter presented using a glass filter with a maximum pore size of 20 micrometers: 50 grams ± 0.1 grams of carrier are added to a pre-weighed 400 mL beaker and 245 mL ± 1 mL of distilled water are added. This is vigorously stirred for 30 minutes with a magnetic stirrer set at 600 rpm. The mixture is then filtered through a sintered glass filter with a pore size (maximum 20 micrometers) as defined above. 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 collected filtrate by any conventional method and the weight of the remaining material is determined (this is the dissolved or dispersed fraction). The solubility or dispersion percentage 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] The alkali metal salt may be selected from the group consisting of, for example, lithium salts, sodium salts, and potassium salts, and any combination thereof. Useful alkali metal salts may 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 carbonates, alkali metal monohydrogen carbonates, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbates, and combinations thereof.

[0016] The alkali metal salt may be selected from the group consisting of sodium fluoride, sodium chloride, sodium bromide, sodium iodide, sodium sulfate, sodium bisulfate, sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, sodium carbonate, sodium bicarbonate, sodium acetate, sodium citrate, sodium lactate, sodium tartrate, sodium silicate, sodium ascorbate, potassium fluoride, potassium chloride, potassium bromide, potassium iodide, potassium sulfate, potassium bisulfate, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, potassium carbonate, potassium monohydrogen carbonate, potassium acetate, potassium citrate, potassium lactate, potassium tartrate, potassium silicate, potassium, ascorbate, and combinations thereof.

[0017] The alkaline earth metal salt may be selected from the group consisting of magnesium salts, calcium salts, and the like, and combinations thereof. The alkaline earth metal salt may 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 carbonates, alkali metal monohydrogen carbonates, alkali metal acetates, alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal silicates, alkali metal ascorbates, and combinations thereof. The alkaline earth metal salt may be selected from the group consisting of magnesium fluoride, magnesium chloride, magnesium bromide, magnesium iodide, magnesium sulfate, magnesium phosphate, magnesium monohydrogen phosphate, magnesium dihydrogen phosphate, magnesium carbonate, magnesium monohydrogen carbonate, magnesium acetate, magnesium citrate, magnesium lactate, magnesium tartrate, magnesium silicate, magnesium ascorbate, calcium fluoride, calcium chloride, calcium bromide, calcium iodide, calcium sulfate, calcium phosphate, calcium monohydrogen phosphate, calcium dihydrogen phosphate, calcium carbonate, calcium monohydrogen carbonate, calcium acetate, calcium citrate, calcium lactate, calcium tartrate, calcium silicate, calcium ascorbate, and combinations thereof.

[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, do contain carbon. The organic salt can be an alkali metal salt or an alkaline earth metal salt of sorbic acid (i.e., a sorbate salt). The sorbate salt can 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 or may include 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.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, potassium sodium tartrate, calcium lactate, water glass, sodium silicate, potassium silicate, dextrose, fructose, galactose, isoglucose, glucose, sucrose, raffinose, isomalt, xylitol, crystal 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 or include a material selected from the group consisting of sodium bicarbonate, sodium sulfate, sodium carbonate, sodium formate, calcium formate, sodium chloride, sucrose, maltodextrin, corn syrup solids, corn starch, wheat starch, rice starch, potato starch, tapioca starch, clays, silicates, carboxymethyl cellulose citrate, fatty acids, fatty alcohols, glyceryl diesters of hydrogenated tallow, glycerol, and combinations thereof.

[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 tallow, 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 polyoxoalkylenes, 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, which may be selected from the group consisting of C8-C22 alkyl polyalkoxylates containing more than about 40 alkoxylate units, ethoxylated nonionic surfactants having an ethoxylation degree of more than about 30, polyalkylene glycols having a weight average molecular weight of about 2000 to about 15000, and combinations thereof.

[0025] The water-soluble polymer may be represented by the formula (I), (II), (III) or (IV), R 1 O-(EO)x-(PO)yR 2 (I), R 1 O--(PO)x-(EO)yR 2 (II), R 1 O-(EO)o-(PO)p-(EO)qR 2 (III), R 1 O--(PO)o-(EO)p-(PO)qR 2 (IV), or a combination thereof, 2 CH 2 O-group, PO is -CH(CH 3 )CH 2 is an O-group; R 1 and R 2 are independently H or a C1-C22 alkyl group; x, y, o, p, and q are independently 1 to 100; provided that the sum of x and y is greater than 35 and the sum of o, p, and q is greater than 35; The block copolymer can be a block copolymer having a molecular weight ranging from about 3000 g / mol to about 15,000 g / mol.

[0026] The water soluble polymer can be a block copolymer or multiple block copolymers, such as ethylene oxide and propylene oxide based block copolymers 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] The water-soluble polymer may be selected from the group consisting of polyvinyl 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; alkylcellulosic materials such as cellulose, methylcellulose, ethylcellulose, and propylcellulose; cellulose ethers; cellulose esters; cellulose amides; polyvinyl acetate; polycarboxylic acids and salts; polyamino acids or peptides; polyamides, polyacrylamides; maleic acid / acrylic acid copolymers; polysaccharides including starch, modified starch; gelatin; alginates; other hemicellulosic polysaccharides including xyloglucan, xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan, and galactoglucomannan; and natural gums such as pectin, xanthan, and carrageenan, locust bean, arabic, and tragacanth; and combinations thereof. In one embodiment, the polymer comprises polyacrylates, particularly sulfonated polyacrylates and water-soluble acrylate copolymers; and alkyl hydroxycellulose-based materials, such as methylcellulose, sodium carboxymethylcellulose, modified carboxymethylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, maltodextrin, polymethacrylates. In yet another embodiment, the water-soluble polymer may be selected from the group consisting of PVA; PVA copolymers; hydroxypropyl methyl cellulose (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 ethers, cellulose esters, cellulose amides, polyvinyl acetate, polycarboxylic acids and salts, polyamino acids or peptides, polyamides, polyacrylamides, maleic acid / acrylic acid copolymers, polysaccharides, starches, modified starches, gelatin, alginates, xyloglucans, hemicellulosic polysaccharides, The polysaccharide may be selected from the group consisting of xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan, galactoglucomannan, natural gums, pectin, xanthan, carrageenan, locust bean, arabic, tragacanth, polyacrylates, sulfonated polyacrylates, water soluble acrylate copolymers, alkylhydroxycellulose-based materials, methylcellulose, sodium carboxymethylcellulose, modified carboxy-methylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethylcellulose, hydroxypropylmethylcellulose, maltodextrin, polymethacrylates, polyvinyl alcohol polymers, hydroxypropylmethylcellulose, and mixtures thereof.

[0029] The water-soluble polymer may be an organic material. Organic water-soluble polymers may 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 esters, polyethylene glycol ethers, starch, and mixtures thereof.

[0031] The water-soluble polymer can be polyethylene glycol (PEG). PEG can be a convenient material to use in making the particles because it can be water-soluble enough to dissolve during the wash cycle when the particles have a mass in the range disclosed herein. Furthermore, PEG can be easily processed as a melt. The onset of the melting temperature of PEG can vary as a function of the molecular weight of the PEG. The particles can include about 20% to about 94% by weight of PEG having 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 diffusion of unencapsulated fragrance, and is well soluble in water. PEG is provided in a variety of weight average molecular weights. Suitable weight average molecular weight ranges for PEG include about 2,000 to about 13,000, alternatively about 4,000 to about 13,000, alternatively about 4,000 to about 12,000, alternatively about 4,000 to about 11,000, alternatively about 5,000 to about 11,000, alternatively about 6,000 to about 10,000, alternatively about 7,000 to about 9,000, or combinations thereof. PEG is available, for example, from BASF as PLURIOL E8000, 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 another having a second weight average molecular weight (e.g., 4000), the second weight average molecular weight being different from the first weight average molecular weight.

[0032] The particles may comprise from about 20% to about 99% by weight of the water-soluble carrier. The particles may comprise from about 35% to about 95% by weight of the particle, optionally from about 50% to about 80% by weight, any combination thereof, and any total percentage or range of total percentages within any of the aforementioned ranges.

[0033] The plurality of particles can include individual particles comprising about 20% to about 99% by weight of the particle of a water-soluble carrier and about 0.1% to about 20% by weight of a particle capsule, the capsule being dispersed in a matrix of a water-soluble polymer.

[0034] The particles may comprise from about 20% to about 99% PEG by weight of the individual particle. Optionally, the individual particles may comprise from about 20% to about 95% PEG by weight of the particle, optionally from about 35% to about 95% PEG by weight, optionally from about 50% to about 80% PEG by weight, optionally combinations thereof, and any total percentage or range of total percentages within any of the foregoing ranges.

[0035] The water soluble polymer may comprise a material selected from the group consisting of: 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH, wherein x is about 50 to about 300, y is about 20 to about 100, and z is about 10 to about 200; 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 (wherein q is about 20 to about 200, and r is about 10 to about 30); 2 H 4 O) s -CH 2 ) t )-CH 3 wherein s is from about 30 to about 250 and t is from about 10 to about 30; and mixtures thereof. 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z The polyalkylene polymer of -OH, where x is about 50 to about 300, y is about 20 to about 100, and z is about 10 to about 200, can be a block copolymer or a random copolymer.

[0036] The water soluble polymer may include: polyethylene glycol; 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH, where x is about 50 to about 300, y is about 20 to about 100, and z is about 10 to about 200; 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 (wherein q is from about 20 to about 200, and r is from about 10 to about 30); and 2 H 4 O) s -(CH 2 ) t )-CH 3 (wherein s is from about 30 to about 250, and t is from about 10 to about 30).

[0037] The water-soluble polymer is from about 20% to about 95% by weight of the plurality of particles or individual particles, and is represented by the formula H-(C 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH, where x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200.

[0038] The water-soluble polymer may be from about 1% to about 20% by weight of the plurality of particles or of each individual particle, 2 H 4 O) q -C(O)O-(CH2 ) r -CH 3 (wherein q is about 20 to about 200, and r is about 10 to about 30) may be included.

[0039] The water-soluble polymer may be from about 1% to about 10% by weight of the plurality of particles or individual particles, and may be a polymer having the formula HO-(C 2 H 4 O) s -CH 2 ) t )-CH 3 (wherein s is from about 30 to about 250, and t is from about 10 to about 30)

[0040] The water-soluble carrier may comprise a plasticizer polyol (0% to 3% by weight of the particles), optionally a plasticizer polymer that is liquid at 20° C. and 1 atmosphere, water (1% to 20% by weight of the particles, or 1% to 12% by weight, or 6% to 8% by weight of the particles), 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 of the particles), wherein the particles comprise (a) 15 to 20% by weight of the particles, or (b) a modified starch having a dextrose equivalent of 4 to less than 15, wherein the sugar alcohol polyol and the modified starch are present in a weight ratio of the sugar alcohol polyol to the modified starch of 1.5:1 to 16:1, or 1.5:1 to 10:1, or 1.5:1 to 4. The modified starch may have a dextrose equivalent of 15 to 20, and the sugar alcohol polyol and the modified starch may be present in a ratio of 2:1 to 16:1, or 2:1 to 10:1, or 2:1 to 3:1. The modified starch may have a dextrose equivalent of 4 to less than 15, and the sugar alcohol polyol and the modified starch may be present in a weight ratio of the sugar alcohol polyol to the modified starch of 1.5:1 to 16:1, or 1.5:1 to 10:1, or 1.5:1 to 4:1. The modified starch may have a dextrose equivalent of 4 to 12. The modified starch may be maltodextrin. The sugar alcohol polyol may be mannitol. The plasticizer polyol may be selected from the group consisting of glycerin, dipropylene glycol, propylene glycol, and mixtures thereof.

[0041] The particles may comprise greater than about 20% by weight of the water-soluble carrier. The particles may comprise greater than about 40% by weight of the water-soluble carrier. The particles may comprise from about 20% to about 99% by weight of the water-soluble carrier. Optionally, the particles may comprise from about 35% to about 85%, or even from about 50% to about 80% by weight of the water-soluble carrier, by weight of the particle. The water-soluble carrier may be selected from the group consisting of: 2 H 4 O) x -(CH(CH 3 )CH 2 O) y -(C 2 H 4 O) z -OH (wherein x is 50 to 300, y is 20 to 100, and z is 10 to 200); 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 (wherein q is 20 to 200 and r is 10 to 30); 2 H 4 O) s -(CH 2 ) t -CH 3 wherein s is 30 to 250 and t is 10 to 30; C8 to C22 alkyl polyalkoxylates containing more than 40 alkoxylate units; polyethylene glycols 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.

[0042] Fabric Care Beneficial Actives The particles may comprise from about 0.1% to about 99% fabric care benefit active by weight of the particle. A fabric care benefit active is a material provided as part of the composition of the particle in an amount sufficient to impart a benefit to fabrics treated with the particle.

[0043] Fabric care benefit actives include amines, surfactant systems, non-ionic surfactants, water-binding agents, sulfites, fatty acids and / or their salts, enzymes, encapsulated benefit agents, soil release polymers, hueing agents, builders, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleach catalysts, bleach activators, polymeric dispersants, cyclodextrin complex benefit agents, stain removal / anti-redeposition agents, non-encapsulated fragrances, polymeric dispersants, polymeric grease cleaners, brighteners, suds suppressors, dyes, hueing agents, free fragrances, The additives may be selected from the group consisting of: ethylhexyl ether, ...

[0044] fragrance Fabric care benefit agent can be perfume.Fragrance is oil or fragrance that contains one or more odoriferous compounds, such as ester, ether, aldehyde, ketone, alcohol, and hydrocarbon type synthetic products.Mixtures of various odoriferous substances that combine to produce attractive fragrance notes can be used.Such perfume oils can also include natural mixtures of odoriferous compounds, such as those available from plant sources.

[0045] The perfume may be a substantially water-insoluble composition comprising perfume components optionally mixed with a suitable solvent or diluent, such as a compound selected from the group consisting of ethanol, isopropanol, diethylene glycol monoethyl ether, dipropylene glycol, diethyl phthalate, triethyl citrate, and mixtures thereof.

[0046] Perfume can be provided as non-encapsulated perfume. Perfume can be provided in perfume delivery system. Zeolite and cyclodextrin are examples of perfume delivery system. Perfume can be encapsulated in starch. For example, starch and perfume oil emulsion can be spray dried to form starch particles with perfume droplets dispersed in starch matrix. Perfume delivery system can be particulate material or fine particulate material that can be difficult to handle in manufacturing environment due to the possibility that particles can become airborne.

[0047] The perfume may be an encapsulated perfume. Encapsulated perfumes are commonly used in laundry products. An encapsulated perfume comprises multiple droplets of liquid perfume, each of which is encapsulated in an encapsulation shell. The perfume may be encapsulated in a water-soluble or water-insoluble encapsulation shell. The encapsulation shell may comprise melamine-urea-formaldehyde, melamine formaldehyde, urea formaldehyde, starch, and similar materials. The encapsulation shell may be a material selected from polyethylene; polyamide; polyvinyl alcohol, optionally containing other co-monomers; polystyrene; polyisoprene; polycarbonate; polyester; polyacrylate; polyolefin; polysaccharides, such as alginate and / or chitosan; gelatin; shellac; epoxy resin; vinyl polymer; water-insoluble inorganic material; silicone; aminoplast; and mixtures thereof. When the encapsulation shell comprises an aminoplast, the aminoplast may comprise a polyurea, a polyurethane, and / or a polyurea urethane. The polyurea may comprise polyoxymethylene urea and / or melamine formaldehyde. Encapsulations having an encapsulation shell comprising a polysaccharide may be practical. The encapsulation shell may be selected from the group consisting of chitosan, gum arabic, alginate, beta-glucan, starch, starch derivatives, vegetable proteins, gelatin, Alyssum Homolocarpum seed gum, and combinations thereof.

[0048] The encapsulation shell may comprise about 90% to 100%, optionally about 95% to 100%, optionally about 99% to 100% inorganic material by weight of the shell. The inorganic material is selected from the group consisting of metal oxides, metalloid oxides, metals, minerals, and mixtures thereof, and optionally SiO. 2 , TiO 2 , Al 2 O 3 , ZrO 2 , ZnO 2 , CaCO 3 , Ca 2 SiO 4 , Fe 2 O 3 , Fe 3 O 4 , clay, gold, silver, iron, nickel, copper, and mixtures thereof, optionally SiO 2 , TiO 2 , Al 2 O 3 , CaCO 3 and mixtures thereof, optionally containing SiO 2 The encapsulation shell may include a first shell component including a condensation layer and a nanoparticle layer, the condensation layer including a condensation product of precursors, the nanoparticle layer including inorganic nanoparticles, the condensation layer being disposed between the core and the nanoparticle layer, and a second shell component surrounding the first shell component, the second shell component surrounding the nanoparticle layer. The encapsulation body may be any of the encapsulations described in U.S. Patent Publication Nos. 2020 / 0330948(A1), 2020 / 0330949(A1), and 2020 / 0330950(A1), and U.S. Patent Application No. 63 / 092,829.

[0049] The fragrance may include one or more botanical fragrances. Botanical fragrances are concentrated hydrophobic liquids containing volatile chemical compounds extracted from plants. Botanical 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, grapefruit pink, helichrysum, hops, hyssop, juniper berry, labdanum, lavender, lemon, Lemongrass, lime, magnolia, mandarin, marjoram, melissa, mugwort, myrrh, myrtle, neroli, niauli, nutmeg, orange sweet, oregano, palmarosa, patchouli, pepper black, peppermint, petitgreen, pine needle, 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, and mixtures thereof.

[0050] The particles may comprise from about 0.1% to about 20% perfume by weight of the particle, optionally from about 0.1% to about 15%, optionally from about 0.1% to about 12%, optionally from about 1% to about 15%, optionally from about 2% to about 20%, optionally from about 8% to about 10% perfume by weight of the particle.

[0051] Fragrance emulsion composition The fabric care benefit agent can be a perfume emulsion composition comprising an amino-functional silicone, the amino-functional silicone comprising one or more primary amine moieties and characterized by a total amine content of about 0.05 to about 2.2, one or more emulsifiers, one or more perfume raw materials, the one or more perfume raw materials comprising an aldehyde moiety, a ketone moiety, or a combination thereof, and water.

[0052] The fragrance emulsion composition can be any of those described in European Patent Office Application No. 20 / 156010.9, filed February 7, 2020.

[0053] The amino-functional silicones include the following: (a) a total amine content of from about 0.071 to about 2.14, or from about 0.071 to about 1.78, or from about 0.71 to about 1.43, or from about 0.14 to about 1.07, or from about 0.14 to about 0.71, or from about 0.21 to about 0.71, or from about 0.36 to about 0.71, and / or (b) a primary amine content of about 0.05 to about 2.2, preferably about 0.071 to about 2.14, or about 0.071 to about 1.78, or about 0.71 to about 1.43, or about 0.14 to about 1.07, or about 0.14 to about 0.71, or about 0.21 to about 0.71, or about 0.36 to about 0.71, and / or (c) a ratio of primary amine content to total amine content of about 1:2 to about 1:1, preferably about 1.2:2, more preferably about 1.5:2, or even more preferably about 1.8:2.

[0054] The amino-functional silicone has the following formula: [R 1 R 2 R 3 SiO 1 / 2 ] (j+2l+2) [R 4 R 5 SiO 2 / 2 ] m [R 6 SiO 3 / 2 ] j [SiO4 / 2 ] l (In the formula, j is an integer of 0 to 150, preferably 0 to 50, and more preferably 0 to 20; m is an integer of 10 to 1500, preferably 10 to 1000, more preferably 20 to 500; l is an integer of 0 to 150, preferably 1 to 150, more preferably 0 to 50, and most preferably 0 to 20; However, j+m+l is equal to an integer greater than or equal to 50, R 1 , R 2 , R 3 , R 4 , R 5 , and R 6 Each of the moieties is independently H, OH, C 1 ~C 32 Alkyl, C 1 ~C 32 Substituted alkyl, C 6 ~C 32 Aryl, C 5 ~C 32 Substituted Aryl, C 6 ~C 32 Alkylaryl, C 6 ~C 32 Substituted alkylaryl, C 1 ~C 32 Alkoxy and C 1 ~C 32 substituted alkoxy, and XZ; 1 ~R 6 At least one of is XZ, Preferably, each R 1~6 However, independently, OH, C 1 ~C 2 Alkyl, C 1 ~C 2 Substituted alkyl, C 1 ~C 2 Alkoxy, C 1 ~C 2 substituted alkoxy, and XZ; wherein each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing from 2 to 12 carbon atoms, preferably each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing from 2 to 6 carbon atoms, and most preferably each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing from 2 to 4 carbon atoms; wherein each Z is a moiety that contains one or more primary amine moieties; Preferably, each Z is independently a group -NH 2 , -N(H)-X-NH 2 or a mixture thereof).

[0055] The emulsion composition has the following characteristics (a) to (d): (a) comprising from about 10% to about 70%, or from about 25% to about 65%, or from about 50% to about 65% amino-functional silicone by weight of the silicone emulsion; and / or (b) the emulsion contains from about 30% to about 90% by weight, or from about 35% to about 75% by weight, or from about 35% to about 50% by weight of water; and / or (c) characterized by a viscosity, measured at 0.1 rad / s and 25° C., 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 even more preferably about 100 to about 300 Pa s; and / or (d) the plurality of droplets comprises a plurality of droplets characterized by an average diameter of from about 1 micron to about 5 microns.

[0056] One or more of the following flavouring ingredients: a. Oncidal, methylnonylacetaldehyde, adoxal, melanal, calypsone, or mixtures thereof; b. Cuminaldehyde, benzaldehyde, anisaldehyde, heliotropin, isocyclocitral, triplamine / ligustral, 3,6-ibcarbaldehyde, ligustral, centenal, or mixtures thereof; c. Satinaldehyde (Jasmolani), Otropal, Cyclamen Homoaldehyde, Cyclamen Aldehyde (Cyclamal), Lilial, Canthoxal, Floralozone, Cinnamaldehyde, or mixtures thereof; d. delta-damascone, beta-damascone, alpha-damascone, nectaryl, or mixtures thereof; e. vanillin, ethyl vanillin, or a mixture thereof; or and a combination of materials selected from at least two of categories fa, b, c, d, and e.

[0057] The one or more emulsifiers may comprise a non-ionic surfactant, preferably the non-ionic surfactant comprises an alkoxylated fatty alcohol, and even more preferably the one or more emulsifiers are characterized by an HLB value of from about 5 to about 20, preferably from about 8 to about 16.

[0058] The 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 softener The fabric care active benefit agent can be a fabric softening active. The particles can include about 5% to about 45% by weight of a quaternary ammonium compound. The quaternary ammonium compound can be an ester quaternary ammonium compound. The quaternary ammonium compound can be those described in U.S. Patent Publication Nos. 2019 / 0169538(A1), 2019 / 0169539(A1), 2019 / 0169777(A1), 2019 / 0169532(A1), 2019 / 0169533(A1), and 2019 / 0169534(A1). The quaternary ammonium compound can be di-(tallowoyloxyethyl)-N,N-methylhydroxyethyl ammonium methyl sulfate.

[0060] The fabric softening active may be an aliphatic amine. The particles may include about 8% to about 45% by weight of an aliphatic amine. The aliphatic amine may be one described in U.S. Patent Application Publication No. 2020 / 0354652(A1).

[0061] The fabric softening active can be a silicone. The particles can include about 1% to about 50% by weight of silicone. The silicone can be one described in U.S. Patent Application Publication No. 2017 / 0349865.

[0062] Branched Polyester The fabric care active benefit agent can be a branched polyester. The particles can include about 5% to about 45% by weight of a branched polyester. The branched polyester can be one described in U.S. Patent Application Publication No. 2019 / 0367841(A1). The branched polyester can be one described and claimed in U.S. Patent Application Publication No. 2019 / 0233764(A1).

[0063] Cationic Polymer The fabric care active benefit agent may be a cationic polymer. The particles may comprise 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 hydroxyethyl cellulose reacted with an epoxide substituted with trimethylammonium groups.

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

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

[0066] Antioxidants The fabric care benefit agent can be an antioxidant. The particles can include about 0.2% to about 2% by weight of the antioxidant. The antioxidant can be dispersed in a matrix of the water-soluble carrier. The antioxidant can be one described in U.S. Patent Application Serial No. 63 / 034,766. The antioxidant can be butylated hydroxytoluene.

[0067] Apparatus and process for forming particles An apparatus 1 for forming particles is shown in FIG. Precursor material 20 can be a melt including any of the compositions disclosed herein for particles 90. Precursor material 20 can include greater than about 20% by weight of the water-soluble carrier. Precursor material 20 can include greater than about 20% by weight of the water-soluble polymer. Precursor material 20 can include from about 20% to about 99% by weight of the water-soluble carrier. Precursor material 20 can include from about 20% to about 99% by weight of the water-soluble carrier.

[0068] Precursor material 20 may include greater than about 20% by weight, optionally greater than about 40% by weight, of polyethylene glycol having a weight average molecular weight of about 2000 to about 13000, and about 0.1% to about 20% by weight of a fragrance.

[0069] Raw materials may be fed into the batch mixer 10. The batch mixer 10 may have sufficient capacity to hold a large amount of the raw materials fed therein for a sufficient residence time to allow for a desired level of mixing or reaction of the raw materials. The material leaving the batch mixer 10 may be a precursor material 20. Optionally, the precursor material may be fed into the feed tube 40 from some other upstream mixing process, such as, for example, in-line mixing, in-line static mixing, etc. The precursor material 20 may be a melt. The batch mixer 10 may be a dynamic mixer. A dynamic mixer is a mixer in which energy is added to mix the contents of the mixer. The batch mixer 10 may include one or more impellers that mix the contents of the batch mixer 10.

[0070] Between the optional batch mixer 10 and the distributor 30, the precursor material 20 may travel through a feed tube 40. The feed tube 40 may be in fluid communication with the batch mixer 10. One or more gas supply lines 155 may be provided in fluid communication with the feed tube 40 downstream of the batch mixer 10. One or more gas supply lines 155 may be provided in fluid communication with the feed tube 40 between the batch mixer 10 and the distributor 30. A mill 200 may be provided downstream of the one or more gas supply lines 155 and in line with the feed tube 40. A mill 200 may be provided downstream of the one or more gas supply lines 155 and in line with the feed tube 40 upstream of the distributor 30.

[0071] The precursor material 20 may be fed into the feed pipe 40. The feed pipe 40 is a transport that carries the precursor material 20. The feed pipe 40 includes transport between the elements of the apparatus 1 and the transport that carries the precursor material within the components of the apparatus 1. For example, the mill 200 may be provided in a unit with a portion of the transport that enters the mill 200 and a portion of the transport that exits the mill 200. Each of these portions is a part of the feed pipe 40. The feed pipe 40 may thus be considered as the entire transport between the batch mixer 10 and the distributor 30, with various elements along the way, such as one or more gas supply lines 155, the mill 200, the intermediate mixer 50, and the feed 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 means upstream of the distributor 30, with various elements along the supply pipe 40, 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 provided downstream of the mill 200 and in line with the feed tube 40. The intermediate mixer 55 may be a static mixer 50. The intermediate mixer 55 may be in fluid communication with the feed tube 40 between the mill 200 and the distributor 30. The intermediate mixer 55, which may be a static mixer 50, may be downstream of the batch mixer 10. In other words, the batch mixer 10, if used, may be upstream of the intermediate mixer 55 or the static mixer 55. The intermediate mixer 55 may be in line with the feed tube 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, a Dispax-reactor disperser, a Colloid Mil MK, or a Cone Mill MKO available from IKA, Wilmington, North Carolina, United States of America. Intermediate mixer 55 may be a perforated disk mill, a toothed colloid mill, or a DIL in-line homogenizer available from FrymaKoruma, Rheinfelden, Switzerland. Static mixer 50 may be a helical static mixer. Static mixer 50 may be a Kenics KMS 6 (1.905 cm inner diameter) available from Chemineer, Dayton, Ohio, USA.

[0073] Without wishing to be bound by theory, it is believed that an intermediate mixer 55, such as static mixer 50, may result in a more uniform temperature of precursor 20 within distributor 30 or stator 100. At the downstream end of intermediate mixer 55, or static mixer 50, if used, the temperature of precursor 20 within feed tube 40 across a cross section of feed tube 40 perpendicular to the direction of flow may vary by less than about 10° C., or less than about 5° C., or less than about 1° C., or less than about 0.5° C.

[0074] In the absence of the static mixer 50, the temperature across the cross section of the feed tube 40 perpendicular to the direction of flow may be non-uniform. The temperature of the precursor material 20 at the centerline of the feed tube 40 may be higher than the temperature of the precursor feed material 20 at the periphery of the feed tube 40. When the precursor material 20 is discharged into the distributor 30 or stator 100, the temperature of the precursor material 20 may vary at different locations within the distributor or stator 100. Without being bound by theory, it is believed that the use of the static mixer 50 as described herein may produce more uniform particles 90 compared to the apparatus 1 without the static mixer 50 by providing a uniform temperature across the cross section of the feed tube 40.

[0075] The distributor 30 may be provided with a number of holes 60. The precursor material 20 may pass through the holes 60. After passing through the holes 60, the precursor material 20 may be deposited on a moving conveyor 80 disposed below the distributor 30. The precursor material 20 may be deposited on the moving conveyor 80 as the conveyor 80 moves. The conveyor 80 may be translatable relative to the distributor 30. The conveyor 80 may be a continuously moving conveyor 80. The conveyor 80 may be an intermittently moving conveyor 80. The continuously moving conveyor 80 may provide a higher processing speed. The intermittently moving conveyor 80 may provide better control over the shape of the particles 90 produced.

[0076] The precursor material 20 may be cooled on the moving conveyor 80 to form a plurality of solid particles 90. Cooling may be provided by ambient cooling. Optionally, cooling may be provided by spraying the underside of the conveyor 80 with warm or cold water.

[0077] Once the particles 90 have become sufficiently cohesive, the particles 90 may be transferred from the conveyor 80 to processing equipment downstream of the conveyor 80 for further processing and / or packaging.

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

[0079] The apparatus 1 may include a cylinder 110 rotatably mounted around a stator 100. The stator 100 is supplied with precursor material via one or both ends 130 of the cylinder 110. The cylinder 110 may have a longitudinal axis L passing through the cylinder 110 about which the cylinder 110 rotates. The cylinder 110 has an exterior surface 120. A plurality of holes 60 may be present in the exterior surface 120 of the cylinder 110.

[0080] The cylinder 110 is driven to rotate about its longitudinal axis L, so that the bores 60 may be in intermittent fluid communication with the stator 100 as the cylinder 110 rotates about the stator 100. The cylinder 110 may be considered to have a machine direction MD in the direction of movement of the outer surface 120 across the stator 100, and a cross machine direction on the outer surface 120 perpendicular to the machine direction MD. The stator 100 may also be considered to have a cross machine direction CD parallel to the longitudinal axis L. The cross machine direction of the stator 100 may be aligned with the cross machine direction of the cylinder 110. The stator 100 may have a number of distribution ports 122 disposed in the cross machine direction CD of the stator 100. The distribution ports 122 are portions or regions of the stator 100 that are supplied with the precursor material 20.

[0081] In general, precursor material 20 can be fed to the stator 100 by passing it through one or more gas supply lines 155, through the mill 200 and through the feed tube 40. The stator 100 distributes the precursor feed material 20 across the working width of the cylinder 110. As the cylinder 110 rotates about its longitudinal axis, the precursor material 20 is fed through the holes 60 as they pass the stator 100. Individual chunks of precursor material 20 are fed through each hole 60 as it encounters the stator 100. The chunks of precursor material 20 fed through each hole 60 as it passes the stator 100 can be controlled by controlling one or both of the pressure of the precursor in the stator 100 and the rotational speed of the cylinder 110, or optionally controlling the viscosity of the precursor material 20 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 working width of the cylinder 110. The conveyor 80 may be translatable relative to the longitudinal axis of the cylinder 110. The speed of the conveyor 80 may be set relative to the tangential velocity of the cylinder 110 to control the shape that the precursor material 20 has once deposited on the conveyor 80. The speed of the conveyor 80 may be approximately the same as the tangential velocity of the cylinder 110.

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

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

[0085] The flow rate of the precursor material 20 can be about 3 L / min. The precursor material 20 can be a melt including any of the compositions described herein for the precursor material 20 or particles 90.

[0086] The apparatus 1 may include one or more gas supply lines 155. A single gas supply line 155 may be practical if the gases to be mixed into the precursor can be practically supplied through a single gas supply line 155. As described herein, gases containing multiple components may be desirable. A multi-component gas may be supplied in a single container 157. For example, a mixture of carbon dioxide and nitrogen may be supplied in a gas cylinder. Optionally, a mixture of gases may be provided continuously from the environment, either through a reaction process or by combining air with another gas supplied from a container. The gas may be pressurized through a compressor.

[0087] The one or more gas supply lines 155 may include a flow regulator 158. The flow regulator 158 may regulate the flow rate of gas into the supply line 40. The amount of gas added per unit volume of precursor material 20 may be controlled by setting the flow regulator 158 to a desired flow rate. The more gas is supplied to the precursor material 20 in the supply line 40, the more gas will be included in the particles 90. The one or more gas supply lines 155 may be provided to mix gas into the precursor material 20.

[0088] Flow regulator 158 can be a Key Instruments Flo-Rite Series GS 65 mm (part number 60410-R5). Supply line 40 can be 1 1 / 2 inch stainless steel sanitary tubing. Gas supply line 155 can be 1 / 4 inch inside diameter polyethylene tubing. Gas can be supplied in gas supply line 155 at a pressure greater than about 4 bar, for example, 5.9 bar.

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

[0090] At the connection between the gas supply line 155 and the supply pipe, an injection quill device may be provided for introducing the gas.

[0091] The gas may be supplied at a temperature and pressure such that a desired amount of gas is present within the particles 90 when the gas reaches ambient temperature and pressure. The ideal gas law may be used to determine the desired delivery temperature and pressure. The gas may also include water. The water may be in gaseous or liquid form. The amount of water in the gas may be selected to be at a desired level.

[0092] The mill 200 can be a rotor-stator type mill. The mill can be a Quadro Z1 in-line mixer with a single medium-sized rotor-stator stage operating at about 400 RPM.

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

[0094] An Oakes Foamer (ET Oakes Corporation, 686 Old Willets Path Hauppauge, NY 11788, 2MT1A continuous former) may be used to provide the gas supply lines 155, flow regulator 158, and mill 200 in a single unit.

[0095] A view of the apparatus 1 in the machine direction MD is shown in Figure 3. As shown in Figure 3, the apparatus 1 can have a working width W and the cylinder 110 can rotate about a longitudinal axis L.

[0096] The apparatus 1 for forming particles 90 may include a feed pipe, one or more gas supply lines 155 mounted in fluid communication with the feed pipe 40 downstream of the batch mixer 10, a mill 200 downstream of the one or more gas supply lines 155 and in line with the feed pipe 40, and a distributor 30 downstream of the mill 200 and in line with the feed pipe 40, the distributor 30 including a plurality of holes 60. The apparatus 1 may include a conveyor below the distributor 30 and translatable relative to the distributor 30. The distributor 30 may include a stator 100 in fluid communication with the feed pipe 40. The distributor 30 may include a cylinder 110 rotatably mounted around the stator 100 and rotatable around a 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 disposed around the outer surface 120. The holes 60 may be in intermittent fluid communication with the stator 100 as the cylinder 110 rotates therearound. The apparatus may include a conveyor 80 below the cylinder 110, which may be translatable about a longitudinal axis L. The apparatus 1 for forming particles 90 may include a batch mixer 10. The feed tube 40 may be in fluid communication with the batch mixer 10.

[0097] A process for forming the particles 90 may include the steps of: supplying precursor material 20 to a supply tube 40; mixing a gas with the precursor material 20, the gas comprising about 50% to about 75% by volume carbon dioxide and about 25% to about 50% by volume of other components; providing a distributor 30 having a plurality of holes 60; moving the precursor material 20 from the supply tube 40 to the distributor 30; passing the precursor material 20 through the holes 60; providing a moving conveyor 80 below the holes 60; depositing the precursor material 20 on the moving conveyor 80; and cooling the precursor material 20 to form a plurality of particles 90.

[0098] The gases may be mixed into the precursor material 20 as a mixture of gases. For example, the mixture of gases may be directed to the precursor material 20 via a single gas supply line 155. The mixture of gases may include about 50% to about 75% by volume carbon dioxide and about 25% to about 50% by volume of other components. The mixture may be provided from a container 157 containing the mixture of gases. For example, the container 157 may be a gas cylinder filled with the desired gas, which is a mixture of different gases.

[0099] Optionally, carbon dioxide may be supplied from a primary container 157a and other components of the gas may be supplied from one or more secondary containers 157b (FIG. 4). The primary containers 157a and secondary containers 157b may be supplied to a single gas supply line 155. A flow regulator 158 may 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 carbon dioxide. The other components of the gas may be provided from the secondary container 157b. The other components of the gas may be provided as air from the secondary container 157b. Containers of air are readily available commercially. Similarly, containers of carbon dioxide are readily available commercially. An operator of the apparatus 1 may obtain a cylinder of carbon dioxide and a cylinder of air and set the flow regulator 158 to provide the desired gas. The carbon dioxide and other components of the gas may be combined into a single stream of gas before being mixed into the precursor material 20.

[0101] Optionally, the primary container 157a can feed into a primary gas supply line 155 and the secondary container 157b can feed into a 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 provide the precursor material 20 in the supply pipe at an operating pressure of about 2 bar to about 8 bar. The gas may be supplied to the supply pipe at a pressure higher than the operating pressure of the supply pipe 40. The gas or its carbon dioxide component may be entrained at a pressure of about 3 to above about 4 bar, or even above about 4 bar, or even above about 5 bar.

[0103] The solubility of carbon dioxide in precursor material 20 can be greater than the solubility of the bulk volume of the other components of the gas. When carbon dioxide gas is provided to the precursor material 20 stream at the operating pressure, the carbon dioxide solubilizes in precursor material 20. The other components of the gas may or may not solubilize in precursor material 20 at the operating pressure. Those components that have a low solubility in precursor material 20 relative to carbon dioxide remain primarily as gas bubbles in precursor material 20.

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

[0105] As the molten precursor material 20 cools, a solidification front develops from the belt-facing side of the precursor material 20, which advances away from the moving conveyor 80 over time. The air-facing side of the precursor material 20, away from the belt-facing surface of the precursor material, also cools as a function of time. This results in a solidification front advancing from the air-facing surface toward the center of the particles being formed on the moving conveyor 80 as the precursor material 20 cools.

[0106] If the gas entrained in the precursor material 20 is air, which is about 78% by volume nitrogen, about 21% by volume oxygen, about 0.93% by volume argon, and about 0.03% by volume carbon dioxide, most of the gas has limited solubility in the precursor material 20 and the air remains as bubbles in the precursor material 20 throughout the process of making the particles. This limits the amount of air that can be entrained in the precursor material 20 and still make particles with the desired stability and appearance. After the precursor material 20 is deposited on the moving belt 40, the buoyancy of the air bubbles in the precursor material 20 and the solidification front advancing from the belt-facing side of the precursor material 20 tend to drive some of the air bubbles away from the moving conveyor 80. As the air bubbles are driven upward, they may coalesce to form larger air bubbles. Some of the air bubbles may escape through the air-facing side of the precursor material 20. The escaped air bubbles no longer contribute to the porosity of the particles 90. If a skin layer were to form on the air-facing side of precursor material 20, air bubbles could erupt through the skin layer, resulting in particles 90 with a physically unstable outer surface. A physically unstable outer surface is undesirable because it can make the particle prone to flaking off, making the particle difficult to use.

[0107] A problem with using air as the entrained gas is that air bubbles may be present within the precursor material 20 as it is deposited on the moving belt 40, causing the phenomenon described in the preceding paragraph, resulting in poorly formed particles 90. Surprisingly, using a gas containing about 50% to about 75% carbon dioxide by volume can improve the ability of the precursor material 20 to retain the air bubbles as it cools on the moving conveyor 80 to form particles 90. This can result in particles 90 with greater porosity and fewer large air bubbles at or near the air-facing surfaces of the particles 90.

[0108] Carbon dioxide 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 be present as gas bubbles. When the operating pressure on the precursor material is released to or toward ambient pressure, the carbon dioxide comes out of solution. The process of carbon dioxide coming out of solution from the precursor material 20 is a time-dependent process. Bubbles of gas components that are relatively insoluble in the precursor material 20 may act as nucleation sites for carbon dioxide to come out of solution from the precursor material. While carbon dioxide is coming out of solution, the precursor material 20 is also cooled. As explained above, a solidification front may develop from the belt-facing side of the precursor material 20, and the air-facing side of the precursor material 20 is also solidifying. The solidified or solidified precursor material 20 forms a barrier to gas bubbles escaping from the precursor material 20. As the carbon dioxide gradually comes out of solution from the precursor material 20, bubbles of carbon dioxide may form, and / or the carbon dioxide may come out of solution and enter existing bubbles of the relatively insoluble gas component. The delayed formation of carbon dioxide bubbles, or the expansion of existing bubbles of the relatively insoluble gas component as the carbon dioxide nucleates on such bubbles, allows a larger volume of bubbles to form in the precursor material 20. And, these later formed bubbles are less likely to escape the precursor material 20. Once the precursor material 20 is fully solidified, the formed particles 90 may have a large volume of voids.

[0109] particle The particles 90 may be formed as described herein and may comprise from about 25% to about 99% by weight of a water soluble carrier. The particles 90 may further comprise from about 0.1% to about 20% by weight of a fabric care benefit active. Each of the particles may have a mass of from about 5 mg to about 200 mg, preferably from about 10 mg to about 100 mg, preferably from about 20 mg to about 50 mg. The particles may have a hemispherical or compressed hemispherical shape.

[0110] Fabric care benefit actives include amines, surfactant systems, non-ionic surfactants, water-binding agents, sulfites, fatty acids and / or their salts, enzymes, encapsulated benefit agents, soil release polymers, hueing agents, builders, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleach catalysts, bleach activators, polymeric dispersants, cyclodextrin complex benefit agents, stain removal / anti-redeposition agents, non-encapsulated fragrances, polymeric dispersants, polymeric grease cleaners, brighteners, suds suppressors, dyes, hueing agents, free fragrances, The additives may be selected from the group consisting of: ethylhexyl ether, ...

[0111] The fabric care benefit actives may be selected from the group consisting of antimicrobial agents, antioxidants, fragrances, fabric conditioning agents, dyes, dye process agents, and combinations thereof. The fabric care benefit actives may be non-encapsulated perfumes or encapsulated perfumes.

[0112] Particles 90 may each have a mass of from about 5 mg to about 200 mg, optionally from about 10 mg to about 100 mg, optionally from about 20 mg to about 50 mg. The particles may have a hemispherical or compressed hemispherical shape.

[0113] The particles 90 can be manufactured as follows: A batch of 50 kg of precursor material 20 may be prepared in a mixer. Molten PEG 8000 may be added to a jacketed mixer maintained at 70° C. and stirred at 125 rpm with a pitch blade agitator. Butylated hydroxytoluene may be added to the mixer in an amount of about 0.01% by weight of precursor material 20. An aqueous slurry of perfume microcapsules may be added to the mixer in an amount of about 4% by weight of precursor material 20. Non-encapsulated perfume may be added to the mixer in an amount of about 8% by weight of precursor material 20. A dye may be added to the mixer in an amount of about 0.01% by weight of precursor material 20. PEG may make up the balance of the weight percent of precursor material 20. Precursor material 20 may be mixed for 30 minutes.

[0114] The precursor material 20 may be formed into particles 90 on a SANDVIK ROTOFORM 3000 with a 750 mm wide, 10 m long belt. The cylinder 110 may have 2 mm diameter holes 60 set at a 10 mm pitch in the cross machine direction CD and a 9.35 mm pitch in the machine direction MD. The cylinder may be set approximately 3 mm above the belt. The belt speed and rotational speed of the cylinder 110 may be set at 10 m / min.

[0115] After mixing the precursor material 20, it can be extruded from the mixer 10 through a plate and frame heat exchanger set at a constant rate of 3.1 kg / min or even 4 kg / min with an outlet temperature controlled at 50° C. The pressure in the feed pipe 40 downstream of the pump 140 can be from about 2 to about 7 bar, or about 5.5 bar or about 5 bar, the pressure being in the feed pipe 40 downstream of the mill 200.

[0116] The gas may be entrained into the precursor material 20 at a precursor to gas volumetric flow ratio of about 1.3:1 to about 2.6:1, or even about 1.3:1 to about 1.6:1. The pressure of the gas in the gas supply line 155 must be higher than the pressure in the supply pipe 40 to ensure flow and entrainment of the gas into the precursor material 20. The flow rate of the precursor material 20 may be about 4.5 liters / min and the gas flow rate may be about 3.4 liters / min. The gas may be a mixture of carbon dioxide and other insoluble gases.

[0117] The precursor material 20 with the entrained gas can be passed through a Quadro Z1 mill equipped with a medium rotor / stator element. After milling, the precursor material can optionally be passed through a Kenics 1.905 cm KMS 6 static mixer 50 located 91.44 cm upstream of the stator 100 of the rotoforming device.

[0118] combination: A. A process for forming particles, comprising: a. supplying a precursor material (20) to a supply tube (40); b. mixing a gas into the precursor material, the gas comprising about 50% to about 75% by volume carbon dioxide and about 25% to about 50% by volume of other components; c. providing a distributor (30) having a plurality of holes (60); d. transferring the precursor material (20) from the supply tube to the distributor; e. passing the precursor material through the holes; f. providing a moving conveyor (80) below the hole; g. depositing the precursor material onto the moving conveyor; h. cooling the precursor material to form a plurality of particles (90). B. The distributor is: a. a stator (100) in fluid communication with the supply line; b. The process of paragraph A comprising: a cylinder (110) rotatably mounted about the stator and rotatable about a longitudinal axis (L) of the cylinder, the cylinder having an outer surface (120), the cylinder comprising the plurality of holes disposed about the outer surface, the holes being in intermittent fluid communication with the stator as the cylinder rotates about the stator. C. The process of paragraph A or B, further comprising the step of milling the precursor material after the step of mixing a gas with the precursor material. D. The process of paragraph C, wherein the step of milling the precursor material after the step of entraining a gas therein is performed using an in-line rotor stator mill. E. The process of any one of paragraphs A-D, wherein the gas is entrained as a mixture of gases. F. The process of paragraph E, wherein the mixture of gases is from a vessel containing the mixture of gases. G. The process of any one of paragraphs A-E, wherein the carbon dioxide is provided from a primary vessel (157a) and the other components of the gas are provided from one or more secondary vessels (157b). H. The process of paragraph G, wherein the carbon dioxide and the other components of the gas are combined into a single stream of the gas before being mixed with the precursor material. I. The process of paragraph H, wherein the other component of the gas is supplied as air from the secondary container. J. The process of any one of paragraphs AI, wherein the carbon dioxide is mixed at a pressure greater than 2 bar and a minimum flow rate of about 0.5 liters / minute. K. The process of any one of paragraphs A-J, wherein greater than 50% by volume of the other component is less soluble in the precursor material than the carbon dioxide. L. The process of any one of paragraphs A-K, wherein the precursor material further comprises greater than about 20% by weight of a water soluble polymer. H. The water-soluble polymer a.Formula H-(C 2 H 4 O)x-(CH(CH 3 )CH 2 O)y-(C 2 H 4 O) a polyalkylene polymer of z-OH (wherein x is 50 to 300, y is 20 to 100, and z is 10 to 200); b.Formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 (wherein q is 20 to 200, and r is 10 to 30), c. Formula HO-(C 2 H 4 O) s -(CH 2 ) t -CH 3 (wherein s is 30 to 250, and t is 10 to 30), d. C8 to C22 alkyl polyalkoxylates containing more than 40 alkoxylate units; e. polyethylene glycol having a weight average molecular weight of 2,000 to 15,000; 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; k. Ethoxylated nonionic surfactants having an ethoxylation degree of more than 30; l. Polyvinyl alcohol; m. polyalkylene glycols having a weight average molecular weight of 2,000 to 15,000; and mixtures thereof. N. The process of any one of paragraphs A through M, wherein the precursor material comprises polyethylene glycol having a weight average molecular weight of about 2,000 to about 13,000. O. The process of any one of paragraphs A-N, wherein the particles comprise greater than about 40% by weight polyethylene glycol. P. The process of any one of paragraphs A through O, wherein the particles have an individual mass of from about 0.1 mg to about 2 g. Q. The process of any one of paragraphs A-P, wherein the precursor material comprises from about 0.1% to about 20% by weight of fragrance. R. The process of paragraph Q, wherein the fragrance comprises an encapsulated fragrance. S. The process of paragraph Q, wherein the fragrance comprises an encapsulated fragrance and a non-encapsulated fragrance. T. The process of any one of paragraphs A through S, wherein the precursor material comprises from about 0.1% to about 20% by weight of encapsulated fragrance. U. The process of any one of paragraphs A-T, wherein cooling the precursor material is performed by ambient cooling. V. The process of any one of paragraphs A-U, wherein the precursor materials are fed to the feed pipe from a batch mixer (10). W. The process of any one of paragraphs AV, wherein the other component is selected from the group consisting of oxygen, nitrogen, argon, and mixtures thereof. X. The process of any one of paragraphs A-W, wherein the precursor material comprises a fabric care benefit agent selected from the group consisting of surfactant systems, water binding agents, sulfites, fatty acids and / or salts thereof, enzymes, encapsulated benefit agents, soil release polymers, hueing agents, builders, chelating agents, dye transfer inhibitors, dispersants, enzyme stabilizers, catalytic materials, bleaching agents, bleach catalysts, bleach activators, polymeric dispersants, soil removal / anti-redeposition agents, polymeric dispersants, polymeric grease cleaners, whitening agents, suds suppressors, dyes, hueing agents, free fragrances, structure elastifiers, fabric softeners, carriers, fillers, hydrotropes, organic solvents, antimicrobials and / or preservatives, neutralizing agents and / or pH adjusters, processing aids, fillers, rheology modifiers or structuring agents, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof.

[0119] Dimensions and values ​​disclosed herein should not be understood as being strictly limited to the exact numerical values ​​recited. Instead, unless otherwise indicated, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm."

[0120] All documents cited herein, including any cross-referenced or related patents or patent applications, and any patent applications or patents to which this application claims priority or benefit, are incorporated herein by reference in their entirety, unless expressly stated to the contrary. The citation of any document shall not be deemed to be prior art to any invention disclosed or claimed herein, or to teach, suggest or disclose any such invention, either alone or in combination with any other reference(s). Furthermore, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition given to that term in this document shall govern.

[0121] While particular embodiments of the present invention have been illustrated and described, it would be obvious 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. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims

1. 1. A process for forming particles comprising: Supplying a precursor material (20) to a supply tube (40); mixing a gas into the precursor material, the gas comprising 50% to 75% by volume carbon dioxide and 25% to 50% by volume of other components; Providing a distributor (30) having a plurality of holes (60); transferring precursor material (20) from the supply tube to the distributor; passing the precursor material through the holes; providing a moving conveyor (80) below said hole; depositing the precursor material on the moving conveyor; and cooling the precursor material to form a plurality of particles (90); The process wherein said particles are porous and are used as a fabric care additive, with the proviso that carbon dioxide contained in said other ingredients is not included in said 50% to 75% by weight carbon dioxide by volume.

2. The distributor, a stator (100) in fluid communication with said supply pipe; 2. The process of claim 1, comprising: a cylinder (110) rotatably mounted about the stator and rotatable about a longitudinal axis (L) of the cylinder, the cylinder having an outer surface (120), the cylinder comprising the plurality of holes disposed about the outer surface, the holes being in intermittent fluid communication with the stator as the cylinder rotates about the stator.

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

4. The process of any one of claims 1 to 3, wherein the gas is entrained as a mixture of gases.

5. The process of claim 4 , wherein the mixture of gases is from a vessel containing the mixture of gases.

6. The process of any one of claims 1 to 4, wherein the carbon dioxide is supplied from a primary vessel (157a) and the other components of the gas are supplied from one or more secondary vessels (157b).

7. 7. The process of claim 6, wherein the carbon dioxide and the other components of the gas are combined into a single stream of the gas before being mixed with the precursor material.

8. 8. The process of claim 7, wherein the other component of the gas is supplied as air from the secondary vessel.

9. A process according to any one of claims 1 to 8, wherein the carbon dioxide is admixed at a pressure above 2 bar and at a minimum flow rate of 0.5 litres / min.

10. The process of any one of claims 1 to 9, wherein more than 50% by volume of the other components are less soluble in the precursor material than the carbon dioxide.

11. The process of any one of claims 1 to 10, wherein the precursor material comprises more than 20% by weight of a water-soluble polymer.

12. The water-soluble polymer is Formula H-(C 2 H 4 O) x -(CH(CH 3 ) CH 2 O) y - (C 2 H 4 O) z -OH, wherein x is from 50 to 300, y is from 20 to 100, and z is from 10 to 200; Formula (C 2 H 4 O) q -C(O)O-(CH 2 ) r -CH 3 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 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 2,000 to 15,000; EO / PO / EO block copolymers; PO / EO / PO block copolymers; EO / PO block copolymer; PO / EO block copolymer; Polypropylene glycol; ethoxylated nonionic surfactants having a degree of ethoxylation greater than 30; Polyvinyl alcohol; 12. The process of claim 11, wherein the polyalkylene glycol is selected from the group consisting of polyalkylene glycols having a weight average molecular weight of from 2,000 to 15,000; and mixtures thereof.

13. The process of any one of claims 1 to 12, wherein the precursor material comprises polyethylene glycol having a weight average molecular weight of 2,000 to 13,000.

14. The process according to any one of claims 1 to 13, wherein the precursor material comprises from 0.1% to 20% by weight of perfume.

15. The process of any one of claims 1 to 14, wherein the step of cooling the precursor material is performed by ambient cooling.

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