Laundry care particles with small variations in average pore radius

Abstract

A composition is provided that includes a plurality of individual particles. The individual particles include a water-soluble carrier and a fabric care benefit active. Each individual particle has a flat bottom, a rounded top, and a maximum height. Each individual particle has a porous bottom third, a porous middle third, and a porous top third. The average pore radius of the bottom third and the average pore radius of the top third differ by less than about 15 μm.

Description

[Technical Field]

[0001] The present invention relates to laundry care particles. [Background technology]

[0002] Consumers want products that can simplify the process used to do laundry, can help reduce the time spent on handling dirty laundry, and can help achieve a high level 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 delivered in the wash liquor are particularly easy for the consumer to use: for example, the 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 a significant amount of surfactants and other cleaning ingredients. Such fabric care compositions are often provided in soluble unit dose pouches that contain a predetermined amount of fabric care actives. Fabric care compositions are also provided in liquid or powder form, and consumers are provided with measuring cups to provide a measured amount of 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 because they provide fabric care benefits beyond those that can be provided by using fully formulated fabric care compositions. Consumers enjoy and appreciate using packaged fabric care additives in a manner that allows them to use custom amounts of fabric care additives based on their 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 wash liquor is formed. Floating particles may tend to dissolve more completely in the wash compared to sinking particles because sinking particles may become trapped in folds, wrinkles, and pockets of laundry during washing. Undissolved particles tend to incompletely deliver the fabric care benefit actives contained therein, which may be undesirable for consumers. Floating particles containing non-encapsulated perfumes can provide a pleasant scent to the headspace above the wash 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 through a melting process is that as the molten precursor material solidifies, gas bubbles within the melt tend to coalesce and rise from the molten material. This can result in large pores at or near the outer surface of the particle, an irregular, rough outer surface, an excessively 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 with a more resistant outer surface, and may be more prone to becoming dusty, difficult to use, and appearing to be of poor quality. The tendency of gas bubbles within the melt to coalesce and rise from the molten material as it solidifies can also effectively limit the volume of pores that can be provided within the particle without these adverse effects occurring. Summary of the Invention [Problem to be solved by the invention]

[0008] Given 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. [Means for solving the problem]

[0009] A composition is provided that includes a plurality of discrete particles, the discrete particles comprising about 20% to about 99% by weight of a water soluble carrier and about 0.1% to about 45% by weight of a fabric care benefit active, each discrete particle having a flat bottom, a rounded top, and a maximum height perpendicular to the flat bottom, each discrete particle having a porous bottom third extending from the flat bottom to a bottom third section height above the flat bottom that is one third of the maximum height, the bottom third having a bottom third average pore radius, and each discrete particle having a porous middle third above the bottom third. and each of the individual particles has a porous top third above the middle third, extending from the middle third to a section height of a middle third above the bottom third that is one-third of the maximum height, the top third having an average pore radius in the top third, the average pore radius in the bottom third differing from the average pore radius in the top third by less than about 15 μm, and each of the particles having a mass of about 5 mg to about 200 mg, optionally about 10 mg to about 100 mg, and optionally about 20 mg to about 50 mg. [Brief explanation of the drawings]

[0010] [Figure 1] It is an apparatus for forming particles. [Figure 2] Part of an apparatus for forming particles. [Figure 3] FIG. 1 is an end view of an apparatus for forming particles. [Figure 4] Part of an apparatus for forming particles. [Figure 5] FIG. 2 is a cross-sectional view of a particle. [Figure 6] FIG. 1 is an exploded view of a particle. [Figure 7] 10 is a micro-CT image and graph of the average pore radius (radius profile in millimeters) of particles formed using a process where the included gas is air. [Figure 8]1 is a micro-CT image and a graph of the average pore radius (radius profile in millimeters) of particles formed using a process in which the gas involved is a mixture of air and carbon dioxide. [Figure 9] A container that contains a plurality of individual particles. DETAILED DESCRIPTION OF THE INVENTION

[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 fabric care benefit active into the wash liquor. When the water-soluble carrier dissolves, the fabric care benefit active is dispersed in the wash liquor and deposited on the laundry.

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

[0013] Water solubility means that the material, carrier substance, or particle is soluble or dispersible in water, optionally at least 50%, optionally at least 75%, or even at least 95% water solubility, as measured by the method set forth herein below using a glass filter with a maximum pore size of 20 micrometers. The method involves adding (50 grams ± 0.1 grams of carrier) to a pre-weighed 400 mL beaker and adding 245 mL ± 1 mL of distilled water. 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 the pore size (maximum 20 micrometers) defined above. The above steps are 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 (this is the dissolved or dispersed fraction) is determined. The solubility or dispersion rate 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, etc., 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, contain carbon. The organic salt may be an alkali metal salt or an alkaline earth metal salt of sorbic acid (i.e., a sorbate). The sorbate 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 or may include a substance 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, 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 or may 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 polyoxoalkylene, polyethylene glycol fatty acid esters, polyethylene glycol ethers, sodium sulfate, starch, and mixtures thereof.

[0024] The water-soluble carrier can be a water-soluble polymer 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 greater than about 30, polyalkylene glycols having a weight average molecular weight of about 2000 Da to about 15000 Da, optionally about 2000 Da to about 13000 Da, and combinations thereof.

[0025] The water-soluble polymer may be a polymer having 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 (wherein EO is a —CH2CH2O— group, PO is a —CH(CH3)CH2O— group, and R 1 and R 2 are independently H or a C1-C22 alkyl group, and x, y, o, p, and q are independently 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 in the range of about 3000 Da to about 15,000 Da.

[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 is polyvinyl alcohol (polyvinyl 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; cellulose, alkylcellulosic materials such as methylcellulose, ethylcellulose, and propylcellulose; cellulose ethers; cellulose esters; cellulose amides; polyvinyl acetate; polycarboxylic acids and salts; polyamino acids or peptides; polyamides; polyacrylamide; 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, tragacanth, and the like; 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 polymethacrylates. In yet another embodiment, the water-soluble polymer may be 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, methyl cellulose, ethyl cellulose, propyl cellulose, cellulose ethers, cellulose esters, cellulose amides, polyvinyl acetate, polycarboxylic acids and salts, polyamino acids or peptides, polyamides, polyacrylamides, maleic acid / acrylic acid copolymers, polysaccharides, starch, modified starch, gelatin, alginates, xyloglucans, hemicellulosic polysaccharides, xylose The sugars may be selected from the group consisting of glutamic acid, glutamic acid esters ...

[0029] The water-soluble polymer can be an organic material. 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 can be polyethylene glycol (PEG). PEG can be a convenient material to use in making particles because it can be sufficiently water-soluble to dissolve during the wash cycle when the particles have a mass within 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 contain about 20% to about 94% by weight of PEG having a weight-average molecular weight of about 2,000 Da to about 15,000 Da. PEG is relatively low cost, can be formed into many different shapes and sizes, minimizes diffusion of non-encapsulated fragrance, and is highly soluble in water. PEG is available in a variety of weight-average molecular weights. Suitable weight average molecular weight ranges for PEG include about 2,000 Da to about 13,000 Da, alternatively about 4,000 Da to about 13,000 Da, alternatively about 4,000 Da to about 12,000 Da, alternatively about 4,000 Da to about 11,000 Da, alternatively about 5,000 Da to about 11,000 Da, alternatively about 6,000 Da to about 10,000 Da, alternatively about 7,000 Da to about 9,000 Da, 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 Da) and another having a second weight average molecular weight (e.g., 4000 Da), the second weight average molecular weight being different from the first weight average molecular weight.

[0032] The particles can comprise from about 20% to about 99% by weight of the water-soluble carrier. The particles can comprise from about 35% to about 95% by weight of the particle, optionally from about 40% to about 90% by weight, optionally from about 50% to about 80% by weight, optionally combinations thereof, and any total percentage or range of total percentages within any of the aforementioned ranges.

[0033] The plurality of particles may comprise individual particles comprising from about 20% to about 99% by weight of the particle of a water soluble carrier and from about 0.1% to about 45% by weight of particles of fabric care benefit active(s), wherein the fabric care benefit active(s) are dispersed in a matrix of water soluble polymer.

[0034] The particles can comprise from about 20% to about 99% PEG by weight of the individual particle. Optionally, the individual particles can 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 40% to about 90% PEG by weight, optionally from about 50% to about 80% PEG by weight, optionally a combination thereof, and any total percentage or range of total percentages within any of the aforementioned ranges.

[0035] The water-soluble polymer has the formula: H—(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (wherein x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200); a polyalkylene polymer of the formula (C2H4O) q -C(O)O-(CH2) r polyethylene glycol fatty acid esters of the formula -CH3 (wherein q is from about 20 to about 200 and r is from about 10 to about 30); s -CH2) t )—CH3, where s is from about 30 to about 250 and t is from about 10 to about 30; and mixtures thereof. x -(CH(CH3)CH2O) y -(C2H4O) z The polyalkylene polymer of -OH (wherein x is from about 50 to about 300, y is from about 20 to about 100, and z is from about 10 to about 200) can be a block copolymer or a random copolymer.

[0036] The water-soluble polymers include the following: polyethylene glycol; x-(CH(CH3)CH2O) y -(C2H4O) 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; polyalkylene polymers of the formula (C2H4O) q -C(O)O-(CH2) r polyethylene glycol fatty acid esters of the formula —CH3, where q is from about 20 to about 200 and r is from about 10 to about 30; and polyethylene glycol fatty acid esters of the formula HO—(C2H4O) s -(CH2) t )-CH3, where s is from about 30 to about 250 and t is from about 10 to about 30.

[0037] The water-soluble polymer may be from about 20% to about 95% by weight of the plurality of particles or individual particles, and may be a polymer of the formula H—(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z The polymer may include a polyalkylene polymer of the formula -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 individual particles, of the formula (C2H4O) q -C(O)O-(CH2) r It may include a polyethylene glycol fatty acid ester of -CH3 (wherein q is about 20 to about 200, and r is about 10 to about 30).

[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 of the formula HO—(C2H4O) s -CH2) t )-CH3, where 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% of the total weight of the particles; or (b) a modified starch having a dextrose equivalent of 20, 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 2:1 to 16:1, or 2:1 to 10:1, or 2:1 to 3:1; or (b) a modified starch having a dextrose equivalent of 4 to less than 15, 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 more than about 20% by weight of the water-soluble carrier. The particles may comprise more 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 40% to about 90%, or even from about 50% to about 80% by weight of the water-soluble carrier. The water-soluble carrier may be a compound having the formula: H—(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (wherein x is 50 to 300, y is 20 to 100, and z is 10 to 200); polyalkylene polymers of the 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 of the formula HO-(C2H4O) s -(CH2) t )-CH3 (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 Da to 15000 Da; 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 Da to 15000 Da, and mixtures thereof.

[0042] Fabric Care Beneficial Active Agents The particles may comprise from about 0.1% to about 45% 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] The fabric care benefit active may be selected from the group consisting of amines, surfactant systems, nonionic 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, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, suds suppressors, dyes, hueing agents, free perfume, structural elastomers, fabric softeners, quaternary amines, hardened and softened tallow, hydrotropes, organic solvents, antimicrobials and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structurants, opacifiers, pearlescent agents, pigments, corrosion and / or colorfastness agents, and mixtures thereof. The fabric care benefit active may be selected from the group consisting of antimicrobial agents, antioxidants, perfumes, fabric conditioning agents, dyes, dye stepping agents, and combinations thereof. The fabric care benefit active may be a non-encapsulated perfume or an encapsulated perfume.

[0044] fragrance Fabric care beneficial agent can be perfume.Fragrance is oil or fragrance that contains one or more fragrant compounds, for example, ester, ether, aldehyde, ketone, alcohol and hydrocarbon type synthetic products.The mixture of various fragrant substances that combine to produce attractive fragrance notes can be used.Such perfume oil can also include the natural mixture of fragrant compounds, such as those that can be obtained 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] Fragrances can be provided as non-encapsulated fragrances.Fragrances can be provided in fragrance delivery systems.Zeolite and cyclodextrin are examples of fragrance delivery systems.Fragrances can be encapsulated in starch.For example, an emulsion of starch and fragrance oil can be spray-dried to form starch particles with perfume droplets dispersed within the starch matrix.Fragrance delivery systems can be particulate or fine particulate materials that can be difficult to handle in manufacturing environments 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 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 comonomers; 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 polyurea, polyurethane, and / or polyurea-urethane. The polyurea may include polyoxymethylene urea and / or melamine formaldehyde. Encapsulations having an encapsulation shell comprising a polysaccharide may be useful. The encapsulation shell may be selected from the group consisting of chitosan, gum arabic, alginate, beta-glucan, starch, starch derivatives, plant proteins, gelatin, alyssum homologous carpum 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%, by weight of the shell, of inorganic material, which is selected from the group consisting of metal oxides, semi-metal oxides, metals, minerals, and mixtures thereof, optionally selected from the group consisting of SiO2, TiO2, Al2O3, ZrO2, ZnO2, CaCO3, Ca2SiO4, Fe2O3, Fe3O4, clay, gold, silver, iron, nickel, copper, and mixtures thereof, optionally from the group consisting of SiO2, TiO2, Al2O3, CaCO3, and mixtures thereof, and optionally can be SiO2. The encapsulation shell can include a first shell component including a condensation layer and a nanoparticle layer, where the condensation layer includes a condensation product of precursors, the nanoparticle layer includes inorganic nanoparticles, and the condensation layer is disposed between the core and the nanoparticle layer, and a second shell component surrounding the first shell component, where the second shell component surrounds the nanoparticle layer. The encapsulation body can be any of the encapsulations described in U.S. Patent Application 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, and lemon. In some embodiments, the essential oils may be selected from the group consisting of laurel, lime, magnolia, mandarin, marjoram, melissa, mugwort, myrrh, myrtle, neroli, niaouli, nutmeg, orange sweet, oregano, palmarosa, patchouli, pepper black, peppermint, petitgrain, 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 that includes: an amino-functional silicone, the amino-functional silicone comprising one or more primary amine moieties and characterized by a total amine content of from 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. 20156010.9, filed February 7, 2020.

[0053] The amino-functional silicone may be: (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 from about 0.05 to about 2.2, optionally 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 (c) a ratio of primary amine content to total amine content of from about 1:2 to about 1:1, optionally about 1.2:2, more optionally about 1.5:2, or even more optionally about 1.8:2.

[0054] The amino functional silicone has 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 from 0 to 150, optionally from 0 to 50, more optionally from 0 to 20; m is an integer from 10 to 1500, optionally from 10 to 1000, more optionally from 20 to 500; l is an integer from 0 to 150, optionally from 1 to 150, more optionally from 0 to 50, most optionally from 0 to 20; where j+m+l is equal to an integer greater than or equal to 50, Each of the R1, R2, R3, R4, R5, and R6 moieties independently is H, OH, C1-C 32 Alkyl, C1-C 32 Substituted alkyl, C6-C 32 Aryl, C5-C 32 Substituted Aryl, C6-C 32 Alkylaryl, C6-C 32 Substituted alkylaryl, C1-C 32 Alkoxy and C1-C 32 substituted alkoxy, and XZ, wherein at least one of the moieties R1-R6 is XZ; Optionally, each R 1~6 is independently selected from the group consisting of OH, C1-C2 alkyl, C1-C2 substituted alkyl, C1-C2 alkoxy, C1-C2 substituted alkoxy, and XZ; each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing from 2 to 12 carbon atoms, optionally each X is independently a substituted or unsubstituted divalent alkylene or alkylidene radical containing from 2 to 6 carbon atoms, and most optionally 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 containing one or more primary amine moieties; Optionally, each Z may be characterized by a group independently selected from -NH2, -N(H)-X-NH2, or mixtures thereof.

[0055] The emulsion composition has the following properties (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 comprises from about 30% to about 90%, or from about 35% to about 75%, or from about 35% to about 50% water by weight; and / or (c) characterized by a viscosity of about 10 to about 500 Pa s, optionally about 20 to about 400 Pa s, more optionally about 25 to about 300 Pa s, and even more optionally about 100 to about 300 Pa s, measured at 0.1 rad / s and 25°C; and / or (d) the plurality of droplets comprises a plurality of droplets characterized by an average diameter of about 1 micron to about 5 microns.

[0056] One or more fragrance ingredients may be: a. Oncidal, methylnonylacetaldehyde, adoxal, melanal, calypsone, or mixtures thereof; b. Cuminaldehyde, benzaldehyde, anisaldehyde, heliotropin, isocyclocitral, triplal / ligustral, 3,6-ivycarbaldehyde, ligustral, centenal, or mixtures thereof; c. Satinaldehyde (Jasmolene), Otropal, Cyclamen Homoaldehyde, Cyclamen Aldehyde (Cyclamar), Lilial, Canthoxal, Floralozone, Cinnamic Aldehyde, 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 can include a nonionic surfactant, optionally, the nonionic surfactant includes an alkoxylated fatty alcohol, and even more optionally, the one or more emulsifiers are characterized by an HLB value of from about 5 to about 20, optionally 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, and optionally, the first emulsifier is a linear nonionic surfactant and / or optionally, the second emulsifier is a branched nonionic surfactant.

[0059] Fabric softening The fabric care benefit active 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 Application 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-methylhydroxyethylammonium methylsulfate.

[0060] The fabric softening active may be a fatty amine. The particles may contain from about 8% to about 45% by weight of a fatty amine. The fatty 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 45% 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 benefit active agent can be a branched polyester. The particles can include about 5% to about 45% by weight of the 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 benefit active can be a cationic polymer. The particles can comprise from about 0.1% to about 10% by weight of the cationic polymer. The cationic polymer can 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 can be a polymeric quaternary ammonium salt of hydroxyethyl cellulose reacted with an epoxide substituted with trimethylammonium groups.

[0064] enzyme The fabric care benefit active can be an enzyme. The particles can include about 0.0001% to about 5% by weight of the 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 benefit active can be a graft copolymer. The particles can include about 0.1% to about 45% 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 active can be an antioxidant. The particles can include about 0.1% to about 2% by weight of the antioxidant. The antioxidant can be dispersed in the water-soluble carrier matrix. The antioxidant can be one described in U.S. Patent Application No. 63 / 034,766. The antioxidant can be butylated hydroxytoluene.

[0067] Apparatus and process for forming particles Apparatus 1 for forming particles is shown in FIG. 1. 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 polymer.

[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 Da to about 13000 Da, 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 the fed amount of raw materials for a sufficient residence time to allow the 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 line 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 within the batch mixer 10.

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

[0071] Optionally, a fully formulated precursor material comprising a water soluble carrier and a fabric care benefit active can be formed by using in-line mixing so that the process is a continuous process. The fabric care benefit active can be continuously fed to the water soluble carrier to form precursor material 20, which is further processed downstream. The precursor material 20 or a partially formulated precursor material can be fed into feed line 40, and the fabric care benefit active can be fed into feed line 40 and mixed with the partially formulated precursor material to form precursor material 20.

[0072] The precursor material 20 may be supplied to a supply pipe 40. The supply pipe 40 is a transport means for transporting the precursor material 20. The supply pipe 40 includes a transport means between elements of the apparatus 1 and the transport means for transporting 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 means entering the mill 200 and a portion of the transport means exiting the mill 200. Each of these portions is a part of the supply pipe 40. Thus, the supply pipe 40 can be considered the entire transport means between the batch mixer 10 and the distributor 30, with various elements along the supply pipe 40 including 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 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.

[0073] The intermediate mixer 55 may be provided downstream of the mill 200 and in line with the feed pipe 40. The intermediate mixer 55 may be a static mixer 50. The intermediate mixer 55 may be in fluid communication with the feed pipe 40 between the 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, if used, the batch mixer 10 may be upstream of the intermediate mixer 55 or the static mixer 55. The intermediate mixer 55 may be in line with the feed pipe 40. The intermediate mixer 55 may be a rotor-stator mixer. The intermediate mixer 55 may be a colloid mill. The intermediate mixer 55 may be a driven in-line fluid disperser. The intermediate mixer 55 may be an Ultra Turrax disperser, a Dispax-reactor disperser, a Colloid Mill MK, or a Cone Mill MKO, available from IKA (Wilmington, North Carolina, United States of America). Intermediate mixer 55 can be a perforated disc mill, a toothed colloid mill, or a DIL in-line homogenizer available from FrymaKoruma (Rheinfelden, Switzerland). Static mixer 50 can be a helical static mixer. Static mixer 50 can be a Kenics KMS 6 (1.905 cm internal diameter) available from Chemineer (Dayton, Ohio, USA).

[0074] Without being 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.

[0075] 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.

[0076] The distributor 30 may be provided with a plurality of holes 60. The precursor material 20 may pass through the holes 60. After passing through the holes 60, the precursor material 20 may be deposited on a moving conveyor 80 provided 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.

[0077] 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 warm or cold water on the underside of the conveyor 80.

[0078] Once the particles 90 have a sufficiently high cohesion, the particles 90 may be transferred from the conveyor 80 to processing equipment downstream of the conveyor 80 for further processing and / or packaging.

[0079] 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 having a plurality of holes 60 thereon, as shown in FIG. 2. Thus, the apparatus 1 may include a stator 100 in fluid communication with a feed tube 40. After the precursor material 20 passes through the mill 200, the feed tube 40 may supply the precursor material 20 to the stator 100.

[0080] 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 the cylinder 110 about which the cylinder 110 rotates. The cylinder 110 has an outer surface 120. A plurality of holes 60 may be present in the outer surface 120 of the cylinder 110.

[0081] Because the cylinder 110 is driven to rotate about its longitudinal axis L, 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 similarly 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 plurality 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 precursor material 20.

[0082] Typically, precursor material 20 can be fed to the stator 100 via one or more gas supply lines 155 through the mill 200 and 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, 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 within the stator 100 and the rotational speed of the cylinder 110, or by optionally controlling the viscosity of the precursor material 20 by controlling the temperature of the precursor material 20.

[0083] A small amount of precursor material 20 is deposited onto a conveyor 80 across the working width of the cylinder 110. The conveyor 80 may be translatable relative to the longitudinal axis L 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.

[0084] As shown in FIG. 1 , the flow rate of precursor material 20 through feed pipe 40 can be provided by gravity flow from batch mixer 10 and distributor 30. To improve controllability of production, apparatus 1 can be provided with feed pump 140, as shown in FIG. 2 . The feed pump 140 can be in-line with feed pipe 40 (“in-line” means in the line through which precursor material 20 flows). The feed pump 140 can be between batch mixer 10 and distributor 30. The feed pump 140 can be upstream of distributor 30. When stator 100 is used, feed pump 140 can be in-line with feed pipe 40 (“in-line” means in the line through which precursor material 20 flows). When stator 100 is used, feed pump 140 can be between batch mixer 10 and distributor 100. The feed pump 140 can be upstream of stator 100. When describing the location of the feed pump 140, "between" is used to describe that the feed pump 140 is in line downstream of the batch mixer 10 and upstream of the distributor 30 or stator 100, if used.

[0085] One or more gas supply lines 155 and mill 200 may be located in line between feed pump 140 and distributor 30 or stator 100 (if used in apparatus 1).

[0086] The flow rate of the precursor material 20 can be about 3 L / min. The precursor material 20 can be a melt comprising any of the compositions described herein for the precursor material 20 or particles 90.

[0087] 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 material can actually be supplied through a single gas supply line 155. As described herein, a gas 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 via a reaction process or by combining air with another gas supplied from a container. The gas may be pressurized via a compressor.

[0088] One or more gas supply lines 155 may include a flow regulator 158. The flow regulator 158 can regulate the flow rate of gas into the supply line 40. The amount of gas added per unit volume of precursor material 20 can be controlled by setting the flow regulator 158 to a desired flow rate. The more gas is supplied to precursor material 20 in supply line 40, the more gas will be contained in particles 90. One or more gas supply lines 155 can be provided to mix gas into precursor material 20.

[0089] Flow regulator 158 may be a Key Instruments Flo-Rite Series GS 65 mm (part number 60410-R5). Supply line 40 may be 1.5 inch stainless steel sanitary tubing. Gas supply line 155 may be 0.25 inch inner diameter polyethylene tubing. Gas may be supplied in gas supply line 155 at a pressure greater than about 4 bar, for example, 5.9 bar.

[0090] If two or more gas supply lines 155 are separately connected to 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 gas supply line 155. If a mixture of gases is introduced into supply pipe 40 via a single gas supply line 155, a single flow regulator 158 may be practical.

[0091] At the connection between the gas supply line 155 and the supply tube, an injection quill device may be provided for introducing the gas.

[0092] 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.

[0093] Mill 200 can be a rotor-stator type mill. The mill can be a Quadro Z1 in-line mixer with a single medium rotor-stator stage operating at approximately 400 RPM.

[0094] The mill 200 and one or more gas supply lines 155 may be combined into a single unit.

[0095] An Oakes Foamer (2MT1A continuous former manufactured by ETOakes Corporation, 686 Old Willets Path, Hauppauge, NY 11788) may be used to provide gas supply line 155, flow regulator 158, and mill 200 in a single unit.

[0096] The apparatus 1 as viewed in the machine direction MD is shown in Figure 3. As shown in Figure 3, the apparatus 1 may have a working width W, while the cylinder 110 may rotate about a longitudinal axis L.

[0097] 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 about the stator 100 and rotatable about 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 about 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 pipe 40 may be in fluid communication with the batch mixer 10.

[0098] A process for forming particles 90 may include the steps of: supplying precursor material 20 to a supply pipe 40; mixing a gas with precursor material 20, wherein the gas comprises 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 precursor material 20 from the supply pipe 40 to the distributor 30; passing precursor material 20 through the holes 60; providing a moving conveyor 80 below the holes 60; depositing precursor material 20 on the moving conveyor 80; and cooling precursor material 20 to form a plurality of particles 90.

[0099] The gases can be mixed into the precursor material 20 as a mixture of gases. For example, the mixture of gases can be directed to the precursor material 20 via a single gas supply line 155. The mixture of gases can include about 50% to about 75% by volume carbon dioxide and about 25% to about 50% by volume of other components. The mixture can be supplied from a container 157 containing the mixture of gases. For example, the container 157 can be a gas cylinder filled with the desired gases, which can be a mixture of different gases.

[0100] Optionally, carbon dioxide can be supplied from a primary container 157a, and other components of the gas can be supplied from one or more secondary containers 157b (FIG. 4). The primary container 157a and secondary containers 157b can be fed into 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 can be provided in or upstream of the gas supply line 155 to mix the gases from the primary container 157a and secondary containers 157b.

[0101] The primary container 157a may contain carbon dioxide. Other components of the gas may be provided from the secondary container 157b. Other components of the gas may be provided as air from the secondary container 157b. Canisters of air are readily available commercially. Similarly, canisters of carbon dioxide are readily available commercially. An operator of the apparatus 1 can 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 to form a single stream of gas before being mixed with the precursor material 20.

[0102] 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.

[0103] During operation, it may be practical to provide precursor material 20 in the supply tube at an operating pressure of about 2 bar to about 8 bar. The gas may be supplied to the supply tube at a pressure higher than the operating pressure of supply tube 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.

[0104] 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 supplied 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 low solubility in precursor material 20 relative to carbon dioxide remain primarily as gas bubbles in precursor material 20.

[0105] As precursor material 20 passes through hole 60, the pressure drops toward or to atmospheric pressure. Precursor material 20 may also begin to cool. Precursor material 20 may continue to cool as precursor material 20 moves from hole 60 to movable conveyor 80. After precursor material 20 is deposited onto movable conveyor 80, cooling continues. Heat is removed from precursor material 20 by the conveyor, and the belt-facing side of precursor material 20 in contact with movable conveyor 80 begins to solidify. Similarly, the surface of precursor material 20 continues to cool after precursor material 20 is deposited onto movable conveyor 80. Thus, once deposited onto movable conveyor 80, cooling of precursor material 20 is a three-dimensional time-dependent process.

[0106] As the molten precursor material 20 cools, a solidification front develops from the belt-facing side of the precursor material 20, and the solidification front advances away from the movable 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 movable conveyor 80 as the precursor material 20 cools.

[0107] When the gas entrained in precursor material 20 is air, which is approximately 78% by volume nitrogen, approximately 21% by volume oxygen, approximately 0.93% by volume argon, and approximately 0.03% by volume carbon dioxide, most of the gas has limited solubility in precursor material 20, and the air remains as bubbles in precursor material 20 throughout the particle-making process. This limits the amount of air that can be entrained in precursor material 20 and still produce particles with the desired stability and appearance. After precursor material 20 is deposited on moving belt 40, the buoyancy of the bubbles within precursor material 20 and the solidification front advancing from the belt-facing side of precursor material 20 tend to drive some of the bubbles away from moving conveyor 80. As the bubbles are driven upward, they may coalesce to form larger bubbles. Some of the bubbles may escape through the air-facing side of precursor material 20. The escaped bubbles no longer contribute to the porosity of particles 90. If a skin layer is formed on the air-facing side of precursor material 20, air bubbles may erupt through the skin layer, resulting in particles 90 with physically unstable outer surfaces. A physically unstable outer surface is undesirable because it may make the particles more susceptible to flaking, making the particles less usable.

[0108] A problem with using air as the entrained gas is that as precursor material 20 is deposited onto moving belt 40, air bubbles may be present within precursor material 20, causing the phenomenon described in the preceding paragraph and 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 precursor material 20 to retain air bubbles as it cools on 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 particles 90.

[0109] 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 exist 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 by which carbon dioxide comes out of solution from the precursor material 20 is time-dependent. 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 the carbon dioxide comes out of solution, the precursor material 20 also cools. As previously explained, 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 solidifying or solidified precursor material 20 forms a barrier against gas bubbles escaping from the precursor material 20. As carbon dioxide gradually comes out of solution from precursor material 20, bubbles of carbon dioxide may form, and / or the carbon dioxide may come out of solution and enter pre-existing bubbles of the relatively insoluble gas component. The delayed formation of carbon dioxide bubbles, or the expansion of pre-existing bubbles of the relatively insoluble gas component as carbon dioxide nucleates on such bubbles, allows larger volumes of bubbles to form in precursor material 20. These later-formed bubbles are less likely to escape precursor material 20. When precursor material 20 is fully solidified, the formed particles 90 may have a large volume of voids.

[0110] The solidification fronts developed on the belt-facing side of precursor material 20 and the air-facing side of precursor material 20, and the subsequently formed bubbles, can also provide the advantage that the bubble size distribution within particle 90 is more uniform throughout the particle's 90 vertical profile along the particle axis, where vertical is taken perpendicular to the flat bottom. Having relatively uniform bubble sizes throughout the particle can be advantageous in that there may be no large bubble concentrations near or on the top surface of particle 90, or pitting or craters on the top surface of particle 90 (evidence of bubbles erupting through the surface of particle 90). Bubbles at or near the surface of particle 90, as well as pitting and craters on the top surface of particle 90, can structurally weaken the top surface of the particle and reduce the particle's physical stability. An irregular surface of particle 90 may also be perceived by users as an indication of poor manufacturing quality control, reducing user confidence in the quality and performance of particle 90.

[0111] particle The particles 90 can be formed as described herein. The composition can include a plurality of individual particles 90. The individual particles 90 can be formed as described herein and can include about 20% to about 99% by weight of a water-soluble carrier. The individual particles 90 can further include about 0.1% to about 45% by weight of a fabric care benefit active, optionally about 0.1% to about 20% by weight of a fabric care benefit active. Each particle can have a mass of about 5 mg to about 200 mg, optionally about 10 mg to about 100 mg, and optionally about 20 mg to about 50 mg. The particles can have a hemispherical or compressed hemispherical shape.

[0112] Each individual particle 90 can have a flat bottom 91, a rounded top 92, and a maximum height 93 perpendicular to the flat bottom 91 (FIG. 5). The maximum height 93 is a scalar quantity. Each particle 90 can include a porous bottom third (94), a porous middle third (95) above the bottom third (94), and a porous top third (96) above the middle third (95) and bottom third (94). The middle third (95) is between the bottom third (94) and the top third (96). Each third of particle 90 is a horizontal cross section of particle 90, where horizontal is understood to be the flat bottom 91. Each horizontal section or each third can have a section height that is one-third of the maximum height 93. The bottom third (94) can have a bottom third section height BTH perpendicular to the flat bottom 91 that is one-third of the maximum height 93. Similarly, the middle third (95) can have a middle third section height MTH perpendicular to the flat bottom 91 that is one-third of the maximum height 93. And the top third (96) can have a top-third section height TTH perpendicular to the flat bottom 91 that is one-third of the maximum height 93. The bottom third section height BTH, the middle third section height MTH, and the top-third section height TTH each have the same scalar.

[0113] The bottom third (94) can extend from the flat bottom 91 to a bottom third section height BTH perpendicular to the flat bottom 91 that is one-third of the maximum height 93. The middle third (95) is above the bottom third (94) and extends from the bottom third (94) to a middle third section height MTH above the bottom third (94) that is one-third of the maximum height 93. The top third (96) is above the middle third (95) and extends from the middle third (95) to a top third section height TTH above the middle third (95) that is one-third of the maximum height 93. The scalar lengths of the bottom third section height BTH, the middle third section height MTH, and the top third section height TTH are equal to one another. An exploded perspective view of particle 90 is shown in FIG.

[0114] The bottom third (94) can have the average pore radius of the bottom third. Similarly, the middle third (95) can have the average pore radius of the middle third. The top third (96) can have the average pore radius of the top third. The average pore radius of each third can be measured as described herein.

[0115] The average pore radius of the bottom third and the average pore radius of the top third can differ by less than about 15 μm. Such uniformity in the average pore radius between the top and bottom of particle 90 can result in particle 90 having the same or similar structural stability on the flat bottom 91 and rounded top 92. Furthermore, the gloss of the flat bottom 91 and rounded top 92 can be the same or sufficiently similar to each other so that surface imperfections are not apparent to a user of particle 90. When the average pore radius of the bottom third and the average pore radius of the top third are so similar to each other, a large total volume of pores can be provided within each particle 90.

[0116] The average pore radius in the bottom third can be about 5 μm to about 100 μm, optionally about 10 μm to about 50 μm, and optionally about 30 μm. Similarly, the average pore radius in the top third can be about 5 μm to about 100 μm, optionally about 10 μm to about 50 μm, and optionally about 30 μm. The average pore radius in the middle third can also be about 5 μm to about 100 μm, optionally about 10 μm to about 50 μm, and optionally about 30 μm. Pores of such sizes in particle 90 at these locations can provide the ability to contain a large total volume of voids within particle 90, and particle 90 can be structurally stable.

[0117] Each of the particles 90 can have a particle axis P. The particle axis P is perpendicular to the flat bottom 91 and passes through the bottom third (94), the middle third (95), and the top third (96). The middle third (95) can have an average sectional pore radius that varies as a function of position along the particle axis P. The average sectional pore radius of the middle third can have a range of less than about 30 μm, optionally less than about 20 μm.

[0118] An individual particle 90 can have a middle third (95) with an average pore radius that is greater than the average pore radius of the bottom third and the average pore radius of the top third. Such particles 90 can tend to have larger pores confined within the core of each particle 90, away from the outer surface of the particle 90. A solidification front that can form as the particle 90 cools during manufacture can limit the movement of bubbles within the solidifying particle 90, preventing bubbles from erupting through the outer surface of the particle 90. Having fewer large bubbles near the outer surface of the particle 90 improves the physical stability of the particle but can also limit the number of scars on the surface of the particle 90 caused by bubbles erupting through the outer surface of the particle 90.

[0119] 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, and optionally from about 20 mg to about 50 mg. The particles may have a hemispherical or compressed hemispherical shape.

[0120] Each of the particles 90 has a density of about 1 g / cm 3 less than, optionally about 0.95 g / cm 3 less than, optionally about 0.92 g / cm 3 less than, optionally about 0.9 g / cm 3 It can have a density of less than about 1 g / cm 3 Particles 90 having a density less than 0.015 may tend to float or remain suspended in the wash solution during a wash cycle long enough for the particles 90 to completely dissolve.

[0121] The particles 90 may have a hemispherical or compressed hemispherical shape. Individual particles 90 may have a diameter of about 2 mm to about 5 mm, or about 3 mm. 2 ~about 20mm 2 The individual particles 90 may have a maximum height of about 2 to about 5 mm.

[0122] A micro-CT image of a particle 90 formed using a process in which the included gas is air is shown in FIG. 7. Also shown in FIG. 7 is a graph of the average pore radius (radius profile in millimeters) as a function of position (in millimeters) within particle 90. In FIG. 7, the flat base 91 is at the top of the image, and the rounded top 92 is at the bottom of the image. The top third (labeled 96) is toward the bottom of the image and graph shown in FIG. 7. The bottom third (labeled 94) is toward the top of the image and graph shown in FIG. 7. As shown in FIG. 7, the average pore radius (radius profile in millimeters) in the top third (labeled 96) of particle 90 is substantially larger than the average pore radius in the middle third (labeled 95) and bottom third (labeled 94). In the particle shown in FIG. 7, large pores predominate near the rounded top 92 of particle 90.

[0123] A micro-CT image of a particle 90 formed using a process in which the gas content is a mixture of air and carbon dioxide (approximately 24% air with carbon dioxide and approximately 76% carbon dioxide) is shown in FIG. 8. Also shown in FIG. 8 is a graph of the average pore radius (radius profile in millimeters) as a function of position (in millimeters) within particle 90. In FIG. 8, the flat base 91 is at the top of the image, and the rounded top 92 is at the bottom of the image. The top third (labeled 96) is toward the bottom of the image and graph shown in FIG. 8. The bottom third (labeled 94) is toward the top of the image and graph shown in FIG. 8. As shown in FIG. 8, the average pore radius (radius profile in millimeters) in the top third (labeled 96) and bottom third (labeled 94) of particle 90 differ by less than 15 μm. Furthermore, the average pore radius (radius profile in millimeters) in the middle third (95) is similar to the average pore radius in the bottom third (94) and top third (96). In general, the average pore radius of particle 90 shown in Figure 8 is smaller than the average pore radius of particle 90 shown in Figure 7.

[0124] Particles 90 can be produced as follows: A 50 kg batch of precursor material 20 can be prepared in a mixer. Molten PEG 8000 can be added to a jacketed mixer maintained at 70°C and agitated at 125 rpm using a pitch blade agitator. Butylated hydroxytoluene can be added to the mixer in an amount of about 0.01% by weight of precursor material 20. An aqueous slurry of perfume microcapsules or other fabric care benefit active(s), optionally an aqueous slurry of other fabric care benefit active(s), can be added to the mixer at a concentration of about 0.1% to about 45% by weight of precursor material 20, optionally about 4% by weight. Optionally, non-encapsulated perfume can be added to the mixer at a concentration of about 8% by weight of precursor material 20. A dye can be added to the mixer at a concentration of about 0.01% by weight of precursor material 20. PEG can comprise the remaining weight percent of precursor material 20. The precursor material 20 may be mixed for 30 minutes.

[0125] The precursor material 20 may be formed into particles 90 in a SANDVIK ROTOFORM 3000 with a 750 mm wide, 10 m long belt. The cylinder 110 may have 2 mm diameter holes 60 spaced 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.

[0126] 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 about 2 to about 7 bar, or about 5.5 bar or about 5 bar, as in the feed pipe 40 downstream of the mill 200.

[0127] The gas may be entrained in 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 tube 40 to ensure gas flow and entrainment into the precursor material 20. The precursor material 20 flow rate may be about 4.5 liters / minute, and the gas flow rate may be about 3.4 liters / minute. The gas may be a mixture of carbon dioxide and other insoluble gases.

[0128] The precursor material 20 with the entrained gas can be passed through a Quadro Z1 mill equipped with medium rotor / stator elements. 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.

[0129] Packaging The particles 90 can be contained in a package 300 (FIG. 9). The package 300 can contain about 100 g to about 2000 g of particles 90. The package 300 can include a body 310 and a closure 320. The particles 90 can be contained within the body 310 of the package 300. The closure 320 can be a removable closure. The body 310 can be a tube, a tub, a carton, a bottle, a sachet, or the like. The body 310 and the closure 320 can be selected from the group consisting of paperboard, corrugated board, plastic, plastic film, paper, foil, and glass. The closure 320 can be a flip-top closure, a screw-on closure, a slide-on closure, a plug closure, an adhesive closure, an interlock closure, or the like.

[0130] How to Use Particles The particles 90 can be used in a process for treating laundry, which includes dispensing about 10 g to about 50 g of the packaged composition into a laundry washing machine or laundry tub. The particles 90 can be any of the particles disclosed herein. The process for treating laundry can include dispensing the particles 90 from the package 300 into a dispensing cup. The particles 90 contained in the dispensing cup can be dispensed into the laundry washing machine or laundry tub. Water can be added to the laundry washing machine or laundry tub. During a wash cycle or hand washing, the particles 90 can dissolve in water or wash liquor, and the fabric care benefit actives contained in the particles can contact the laundry being treated.

[0131] Micro-CT (micro-computed tomography) measurement method Micro-CT is used to measure various properties of individual particles, including the size and spatial distribution of void volume. Structural measurements are based on the analysis of 3D X-ray sample images obtained with a high-energy micro-CT instrument capable of acquiring data sets with high isotropic spatial resolution. A suitable instrument is the Scanco μCT50 or equivalent, available from Scanco Medical AG (Switzerland). This micro-CT instrument is a cone-beam microtomograph equipped with a shielded cabinet. A maintenance-free X-ray tube is used as the source, with an adjustable focal spot diameter. A polychromatic X-ray beam passes through the sample, and a portion of the X-rays is attenuated by the chemical and physical properties of the particle. The degree of attenuation correlates to the mass, structural distribution, and overall elemental composition of the material through which the X-rays must pass. The transmitted / attenuated X-rays then impinge on a digital detector array, generating a 2D projection image of the particle. A 3D volumetric image of the sample is generated by rotating the particle (180°-360°) and collecting several individual 2D projection images, which are then reconstructed into a single 3D image. The instrument is interfaced with a computer with dedicated software to control the image collection and reconstruction of the raw data into a 3D image. The 3D images are then analyzed using image analysis software (suitable image analysis software is MATLAB, available from The Mathworks, Inc., Natick, MA, and Avizo Lite, available from Visualization Sciences Group / FEI Company, Burlington, MA, or equivalent).

[0132] Particle preparation: Individual particles are randomly derived from a larger particle population, excluding broken or chipped particles. The particles are held in place by low-density foam in a low-density plastic holder placed within the scanning chamber. The particles remain in this original configuration throughout the scanning process.

[0133] Image acquisition: The micro-CT instrument is set up and calibrated according to the manufacturer's specifications. The particle is placed in a 9 mm diameter holder between two rings of low-density material to prevent movement during scanning rotation. The particle is positioned upright and perpendicular to the scanner detector. A single 3D dataset of contiguous 2.0 μm (micron) isotropic voxels is collected. Images are acquired using a 45 kVp and 177 μA source without additional low-energy filtering. These current and voltage settings are optimized to allow sufficient x-rays to penetrate the sample to maximize contrast in the projection data, but once optimized, they are maintained constant for all substantially similar particles. A total of 2,000 projection images are acquired with an integration time of 550 ms and three averages per batch. Two vertical batches are performed to completely scan the particle height. The projection images are reconstructed into a 3D dataset of approximately 4,700 tomographic images with an isotropic spatial resolution of 2 μm (micron) and saved in 16-bit raw format to preserve the full detector output signal for analysis.

[0134] The 3D dataset is loaded into image analysis software and cropped to remove the surrounding holder and excess void / background space, thus creating a smaller 3D volumetric image of the object of interest for data processing and analysis. This cropped 3D image is then scaled from 16-bit to 8-bit and thresholded using Otsu's method, which calculates a threshold level that minimizes the weighted intraclass variance, to isolate and remove background signal due to air, while preserving signal from solid material in the particle image.

[0135] A connected component + region growing algorithm (region growing: using a seed point, the largest connected volume is selected that contains the seed voxel itself and all voxels with gray values ​​within a defined range, where connected voxels are those that share at least one face) is run to identify the largest objects and remove noise.

[0136] The total void space (void voxels) and total solid space (solid voxels) occupied within the sample structure in the 3D image are used to calculate the percent void and solid space fractions. A "total volume" mask is used to encapsulate the complete sample structure. This mask is achieved by performing a closure method, which involves performing a dilation operation followed by a shrinkage operation on the solid portion of the sample. Porosity is the void space divided by the total volume.

[0137] To characterize the pore size distribution in the height direction, a local thickness map algorithm, or LTM, is implemented within the pore voxels. The LTM method begins with Euclidean Distance Mapping (EDM), assigning each pore voxel a gray-level value equal to its distance from its nearest boundary. Based on the EDM data, the 3D pore space representing the pores is tessellated with spheres sized to match the EDM values. Voxels enclosed by the spheres are assigned the radius value of the largest sphere. In other words, each pore voxel is assigned the radius value of the largest sphere that both fits within the pore space boundary and contains the assigned voxel. The 3D labeled spherical distribution output from the LTM data scan is processed as a stack of two-dimensional images in the height direction (or along the grain axis) and can be used to estimate the change in spherical diameter in the height direction, slice by slice. The depth of the mapped region is divided into three horizontal sections: the bottom third, the middle third, and the top third. The weighted average mean radius of all spheres representing void voxels is calculated and reported as the mean pore radius to the nearest 0.01 micron for each of the bottom, middle, and top thirds. Within the middle third, the mean section pore radius of the middle third as a function of position along the particle axis is the change in spherical diameter across the height, per section. The mean section pore radius of the middle third as a function of position along the particle axis is calculated and recorded, and the range of mean pore radii within the middle third is recorded.

[0138] combination: An example is shown below. A. A composition comprising a plurality of particles (90), the particles comprising: about 20% by weight to about 99% by weight of a water-soluble carrier; about 0.1% to about 45% by weight of a fabric care benefit active; The individual particles have a flat bottom (91), a rounded top (92), and a maximum height (93) perpendicular to the flat bottom; the individual particles have a porous bottom third (94) extending from the flat bottom to a bottom third section height (BTH) above the flat bottom, the bottom third having a bottom third average pore radius; The individual particles have a porous middle third (95) above the bottom third, extending from the porous middle third to a maximum height, middle third section height (MTH), above the bottom third; the individual particles have a porous top third (96) above a middle third, extending from the middle third to a top third section height (TTH) above the middle third that is one-third of the maximum height, the top third having a top third average pore radius; the average pore radius of the bottom third differs from the average pore radius of the top third by less than about 15 μm; The composition, wherein the particles each have a mass of from about 5 mg to about 200 mg, optionally from about 10 mg to about 100 mg, and optionally from about 20 mg to about 50 mg. B. The composition of paragraph A, wherein the individual particles have a hemispherical or compressed hemispherical shape. C. The composition of paragraph A or B, wherein the average pore radius in the bottom third and the average pore radius in the top third are from about 5 μm to 100 μm. D. The composition of any of paragraphs A-C, wherein the middle third has an average pore radius in the middle third of about 5 μm to 100 μm. E. The composition of any of paragraphs A-D, wherein the middle third has an average pore radius that is greater than each of the average pore radius of the bottom third and the average pore radius of the top third. F. The composition of any of paragraphs A-E, wherein each individual particle has a particle axis (P) perpendicular to the flat bottom and passing through the middle third, and an average sectional pore radius in the middle third that varies as a function of position along the particle axis, wherein the average sectional pore radius in the middle third has a range of less than about 30 μm. G. Each individual particle weighs approximately 1 g / cm 3 The composition of any of paragraphs A-F, having a density of less than H. The composition of any of paragraphs A-G, wherein the fabric care benefit active is selected from the group consisting of amines, surfactant systems, nonionic 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 complexed benefit agents, stain removal / anti-redeposition agents, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, suds suppressors, dyes, hueing agents, non-encapsulated perfumes, structural elasticizers, fabric softeners, quaternary amines, hard and soft tallow, hydrotropes, organic solvents, antimicrobials and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structuring agents, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof. I. The composition of any of paragraphs AH, wherein the fabric care benefit active is a non-encapsulated perfume or an encapsulated perfume. J. The composition of any of paragraphs AI, wherein the water-soluble carrier is selected from the group consisting of polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxoalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, polyglycerol ester, sodium sulfate, carbohydrate, starch, and mixtures thereof. K. The composition of any of paragraphs AJ, wherein the water-soluble carrier comprises polyethylene glycol having a weight average molecular weight of about 2,000 Da to about 15,000 Da. L. The composition of any of paragraphs AI, wherein the water-soluble carrier is selected from the group consisting of polyethylene glycol, polypropylene glycol, and combinations thereof, having a weight average molecular weight of 2,000 Da to 15,000 Da. M. The water-soluble carrier is a compound represented by 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 block copolymer having a combination thereof. wherein EO is a —CHCHO— group and PO is a —CH(CH)CHO— 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, the sum of o, p, and q is greater than 35, The composition of any of paragraphs AI, wherein the block copolymer has a weight average molecular weight in the range of 3,000 Da to 15,000 Da. N. The composition of any of paragraphs AI, wherein the water-soluble carrier is selected from the group consisting of a C8-C22 alkyl polyalkoxylate containing greater than 40 alkoxylate units, an ethoxylated nonionic surfactant having a degree of ethoxylation greater than 0, an EO / PO / EO block copolymer, a PO / EO / PO block copolymer, an EO / PO block copolymer, a PO / EO block copolymer, and combinations thereof, wherein EO is a —CHCHO— group and PO is a —CH(CH)CHO— group. O. Water-soluble carriers are R1 O-(EO)x-(PO)yR 2 , R 1 O--(PO)x-(EO)yR 2 , R 1 O-(EO)o-(PO)p-(EO)qR 2 , R 1 O--(PO)o-(EO)p-(PO)qR 2 (In the formula, aR 1 and R 2 are independently H or a C1-C22 alkyl group, bx, y, o, p, and q are independently 1 to 100, the sum of x and y is greater than 35, and the sum of o, p, and q is greater than 35; The composition of paragraph N, wherein the block copolymer has a weight average molecular weight in the range of 3000 Da to 15,000 Da), or a combination thereof. P. The carrier is Formula H-(C2H4O) x -(CH(CH3)CH2O) y -(C2H4O) z -OH (wherein x is 50 to 300, y is 20 to 100, and z is 10 to 200); Formula (C2H4O) q -C(O)O-(CH2) r polyethylene glycol fatty acid ester of —CH3 (wherein q is 20 to 200 and r is 10 to 30); Formula HO-(C2H4O) s -(CH2) t )-CH3 (wherein s is 30 to 250, and t is 10 to 30); C8-C22 alkyl polyalkoxylates containing more than 40 alkoxylate units; ethoxylated nonionic surfactants having a degree of ethoxylation greater than 30; Polyvinyl alcohol; Polyethylene glycol having a weight average molecular weight of 2000 Da to 15000 Da; The composition of any of paragraphs AI, wherein the composition is selected from the group consisting of: and mixtures thereof. Q. The composition of any one of the preceding claims, wherein the plurality of individual particles is contained in a package (300), and the plurality of individual particles has a mass of about 100 g to about 2000 g. R. A process for treating laundry using a plurality of discrete particles according to any one of the preceding claims, comprising: placing about 10 g to about 50 g of a plurality of discrete particles into a laundry washing machine or laundry tub; dissolving a plurality of individual particles in water; contacting the laundry with a fabric care benefit active.

[0139] The dimensions and values ​​disclosed herein should not be understood as being strictly limited to the exact numerical values ​​recited. Instead, unless otherwise specified, 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."

[0140] 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 or references. 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 assigned to that term in this document shall govern.

[0141] 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. This specification discloses the following inventions. [1] A composition comprising a plurality of discrete particles (90), the discrete particles comprising: 20% by weight to 99% by weight of a water-soluble carrier; 0.1% to 45% by weight of a fabric care benefit active; and Including, The individual particles have a flat bottom (91), a rounded top (92), and a maximum height (93) perpendicular to the flat bottom; the individual particles have a porous bottom third (94) extending from the flat bottom to a bottom third section height (BTH) above the flat bottom that is one-third of the maximum height, the bottom third having a bottom third average pore radius; the individual particles have a porous middle third (95) above the bottom third, extending from the bottom third to a middle third section height (MTH) above the bottom third that is one-third of the maximum height; the individual particles have a porous upper third (96) above the middle third, extending from the middle third to a top-third section height (TTH) above the middle third that is one-third of the maximum height, the top third having a top-third average pore radius; the average pore radius of the bottom third differs from the average pore radius of the top third by less than 15 μm; The composition, wherein each of said particles has a mass of from 5 mg to 200 mg, optionally from 10 mg to 100 mg, optionally from 20 mg to 50 mg. [2] The composition according to [1], wherein the individual particles have a hemispherical or compressed hemispherical shape. [3] The composition according to [1] or [2], wherein the average pore radius of the bottom third and the average pore radius of the upper third are 5 μm to 100 μm. [4] The composition according to any one of [1] to [3], wherein the middle third has an average pore radius of 5 μm to 100 μm. [5] The composition according to any one of [1] to [4], wherein the middle third has an average pore radius that is greater than both the average pore radius of the bottom third and the average pore radius of the upper third. [6] The composition of any of [1] to [5], wherein each of the individual particles has a particle axis (P) that is perpendicular to the flat bottom and passes through the middle third, and an average sectional pore radius in the middle third that varies as a function of position along the particle axis, the average sectional pore radius in the middle third having a range of less than 30 μm. [7] Each of the individual particles has a density of 1 g / cm 3 The composition according to any one of [1] to [6], having a density of less than 10 ... [8] 10. The composition of claim 1, wherein the fabric care benefit active is selected from the group consisting of amines, surfactant systems, nonionic 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 complexed benefit agents, stain removal / anti-redeposition agents, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, suds suppressors, dyes, hueing agents, non-encapsulated perfumes, structural elastomers, fabric softeners, quaternary amines, hard and soft tallow, hydrotropes, organic solvents, antimicrobials and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structuring agents, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof. [9] The composition according to any one of [1] to [8], wherein the fabric care benefit active is a non-encapsulated fragrance or an encapsulated fragrance.

[10] The composition according to any one of [1] to [9], wherein the water-soluble carrier is selected from the group consisting of polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxoalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, polyglycerol ester, sodium sulfate, carbohydrate, starch, and mixtures thereof.

[11] The composition according to any one of [1] to [9], wherein the water-soluble carrier is selected from the group consisting of polyethylene glycol, polypropylene glycol, and combinations thereof, each having a weight-average molecular weight of 2000 Da to 15000 Da.

[12] The water-soluble carrier is represented by 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 block copolymer having a combination thereof. (Wherein, EO is -CH 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, the sum of o, p, and q is greater than 35, The composition according to any one of [1] to [9], wherein the block copolymer has a weight average molecular weight in the range of 3,000 Da to 15,000 Da.

[13] The water-soluble carrier is selected from the group consisting of C8-C22 alkyl polyalkoxylates containing more than 40 alkoxylate units, ethoxylated nonionic surfactants having a degree of ethoxylation greater than 0, EO / PO / EO block copolymers, PO / EO / PO block copolymers, EO / PO block copolymers, PO / EO block copolymers, and combinations thereof, wherein EO is selected from the group consisting of -CH 2 CH 2 O- group, and PO is -CH(CH 3 )CH 2 The composition according to any one of [1] to [9], wherein the O- group is an O- group.

[14] The water-soluble carrier is R 1 O-(EO)x-(PO)yR 2 、R 1 O--(PO)x-(EO)yR 2 、R 1 O-(EO)o-(PO)p-(EO)qR 2 、R 1 O--(PO)o-(EO)p-(PO)qR 2 (In the formula, aR 1 and R 2 are independently H or a C1-C22 alkyl group, bx, y, o, p, and q are independently 1 to 100, the sum of x and y is greater than 35, and the sum of o, p, and q is greater than 35; The composition according to

[13] , wherein the block copolymer has a weight average molecular weight in the range of 3000 Da to 15,000 Da, or a combination thereof.

[15] The composition according to any one of [1] to

[14] , wherein the plurality of individual particles are contained in a package (300), and the plurality of individual particles have a mass of 100 g to 2000 g.

Claims

1. A composition comprising a plurality of individual particles (90), said individual particles comprising: 20% to 99% by weight of a water-soluble carrier; 0.1% to 45% by weight of a fabric care benefit active; Including, The individual particles have a flat base (91), a rounded top (92), and a maximum height (93) perpendicular to the flat base; the individual particles have a porous bottom third (94) extending from the flat bottom to a bottom third section height (BTH) above the flat bottom that is one-third of the maximum height, the bottom third having a bottom third average pore radius; the individual particles have a porous middle third (95) above the bottom third, extending from the bottom third to a middle third section height (MTH) above the bottom third that is one-third of the maximum height, and the middle third has an average pore radius in the middle third of 5 μm to 100 μm; the individual particles have a porous upper third (96) above the middle third, extending from the middle third to a top-third section height (TTH) above the middle third that is one-third of the maximum height, the top third having a top-third average pore radius; the average pore radius of the bottom third differs from the average pore radius of the top third by less than 15 μm; The composition, wherein each of said particles has a mass of between 5 mg and 200 mg.

2. The composition of claim 1 , wherein the individual particles have a hemispherical shape.

3. 2. The composition of claim 1, wherein the average pore radius of the bottom third and the average pore radius of the top third are from 5 μm to 100 μm.

4. 10. The composition of claim 1, wherein the middle third has an average pore radius in the middle third of from 10 μm to 50 μm.

5. 2. The composition of claim 1, wherein each of the individual particles has a particle axis (P) perpendicular to the flat bottom and passing through the middle third, and an average sectional pore radius in the middle third that varies as a function of position along the particle axis, the average sectional pore radius in the middle third having a range of less than 30 μm.

6. Each of the individual particles has a density of 1 g / cm ３ 10. The composition of claim 1 having a density of less than 1000 .mu.m.

7. 10. The composition of claim 1, wherein the fabric care benefit active is selected from the group consisting of amines, surfactant systems, nonionic 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 complexed benefit agents, stain removal / anti-redeposition agents, encapsulated perfumes, polymeric dispersants, polymeric grease cleaners, brighteners, suds suppressors, dyes, hueing agents, non-encapsulated perfumes, structural elasticizers, fabric softeners, quaternary amines, hard and soft tallow, hydrotropes, organic solvents, antimicrobials and / or preservatives, neutralizers and / or pH adjusters, processing aids, fillers, antioxidants, rheology modifiers or structuring agents, opacifiers, pearlescent agents, pigments, corrosion and / or rust inhibitors, and mixtures thereof.

8. 10. The composition of claim 1, wherein the fabric care benefit active is a non-encapsulated perfume or an encapsulated perfume.

9. 9. The composition of any one of claims 1 to 8, wherein the water-soluble carrier is selected from the group consisting of polyethylene glycol, sodium acetate, sodium bicarbonate, sodium chloride, sodium silicate, polypropylene glycol polyoxoalkylene, polyethylene glycol fatty acid ester, polyethylene glycol ether, polyglycerol ester, sodium sulfate, carbohydrate, starch, and mixtures thereof.

10. The composition of any one of claims 1 to 8, wherein the water-soluble carrier is selected from the group consisting of polyethylene glycol, polypropylene glycol, and combinations thereof, having a weight average molecular weight of 2,000 Da to 15,000 Da.

11. The water-soluble carrier may be a compound represented by formula (I), (II), (III), or (IV): 2 １ Y-(EOxm-(O)ym2 ２ (9)、 ( １ _______________________________ ２ (......)、 2 １ 9-(59)o-(O)pm(59)qm2 ２ (999)、 R １ ------------------ ２ (IV), or a block copolymer having a combination thereof. (Wherein, EO is —CH ２ CH ２ O- group, and 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 composition of any one of claims 1 to 8, wherein the block copolymer has a weight average molecular weight in the range of 3000 Da to 15,000 Da.

12. The water-soluble carrier is selected from the group consisting of C8-C22 alkyl polyalkoxylates containing more than 40 alkoxylate units, ethoxylated nonionic surfactants having a degree of ethoxylation greater than 30, EO / PO / EO block copolymers, PO / EO / PO block copolymers, EO / PO block copolymers, PO / EO block copolymers, and combinations thereof, wherein EO is selected from the group consisting of -CH ２ CH ２ O- group, and PO is -CH(CH ３ ) CH ２ The composition according to any one of claims 1 to 8, wherein the O- group is an O- group.

13. The water-soluble carrier is R １ O-(EO)x-(PO)y-R ２ 、R １ O-(PO)x-(EO)y-R ２ 、R １ O-(EO)o-(PO)p-(EO)q-R ２ 、R １ O-(PO)o-(EO)p-(PO)q-R ２ (wherein, a.R １ and R ２ are independently H or a C1-C22 alkyl group; b. x, y, o, p, and q are independently 1 to 100, the sum of x and y is greater than 35, and the sum of o, p, and q is greater than 35; or a combination thereof; The composition of claim 12, wherein the water-soluble carrier has a weight average molecular weight in the range of 3000 Da to 15,000 Da.

14. 10. The composition of claim 1, wherein the plurality of discrete particles is contained in a package (300), and the plurality of discrete particles has a mass of between 100 g and 2000 g.

Images