Delivery particle slurries containing benefit agents

Abstract

The present invention relates to delivery particle slurries containing benefit agents, as well as to compositions comprising delivery particles containing benefit agents and methods for making and using the above particles and compositions. Such slurries are stable and when used in compositions, such as cleaning compositions or fabric care compositions, the particles in such slurries increase the efficiency of benefit agent delivery, allowing for reduced amounts of benefit agent to be employed. In addition to allowing for a reduction in the amount of benefit agent, such particles also allow for a wide range of benefit agents to be employed.

Description

[0001] This application is a divisional application of an application with the PCT international application date of March 16, 2017, PCT international application number PCT / US2017 / 022613, and Chinese national application number 201780088383.4, and the invention name is “Delivery particle slurry containing beneficial agents”. Technical Field

[0002] The present patent application is directed to slurries containing delivery particles containing beneficial agents, compositions containing such particles, and methods for making and using such particles and compositions, the delivery particles comprising a core material and a shell material encapsulating the core material. Background Art

[0003] Beneficial agents such as spices, silicones, waxes, flavors, vitamins and fabric softeners are expensive, and / or are generally inefficient when used in consumer products such as personal care compositions, cleaning compositions and fabric care compositions at high levels. Therefore, it is desirable to maximize the effectiveness of such beneficial agents. A method of achieving such purposes is to improve the delivery efficiency of such beneficial agents. Unfortunately, it is difficult to improve the delivery efficiency of beneficial agents because such agents may be lost due to the physical or chemical properties of the agents, or such agents may be incompatible with other composition components or positions to be treated. In order to improve such delivery efficiency, benefit agents have been encapsulated.

[0004] It is desirable to provide perfume benefits within all consumer contact points with delivery particles containing benefit agents, which have a shell comprising polyacrylate. For example, it is desirable that such particles provide perfume benefits to fabrics, which are treated with such particles when the fabrics are still wetted by such treatments and after such fabrics have dried. Unfortunately, over time, such particles may leak benefit agents via diffusion. Therefore, fabric odor is reduced. If, for example, such leakage is minimized by increasing the shell strength of the particles, the fabric odor of wetting and / or drying can be reduced again. This problem is particularly evident in fabric treatment products, such as liquid fabric enhancers, liquid laundry detergents, unit dose laundry detergents, and granular / powdered laundry detergents comprising such particles. Therefore, what is needed is such particles, which show reduced benefit agent leakage, yet provide desired odor characteristics to wet fabrics and dry fabrics-especially enhanced pre-friction benefits and post-friction benefits.

[0005] Herein, the applicant recognizes that the problem root of the dilemma of shell strength and beneficial agent release in the beneficial agent delivery system is a multi-component problem. This multi-component problem is rooted in the colloid type, the monomer building element for the capsule wall and the beneficial agent solvent system, because the colloid and the capsule shell polymer both form an integrated delivery system, and the polymerization process is affected by the beneficial agent solvent system. The content, type and molecular weight of the colloid such as polyvinyl alcohol used in combination with the capsule shell polymer formed during the particle preparation process can affect the effectiveness of the delivery system. When such delivery agent polymer shell is also partially constructed by monomers with many cross-linking sites / parts (such as acrylate moieties), this is especially true. Generally speaking, the molecular weight and crosslinking of the non-colloidal part of the delivery system are difficult to control. Surprisingly, the applicant recognizes that if not only the shell material is wisely selected, but also the colloid type and the encapsulated beneficial agent solvent system are wisely selected, such control can be obtained. In addition, the beneficial agent solvent system works in the obtained molecular weight and crosslinking of the polymer obtained in the non-colloidal part of the delivery system. Without being bound by theory, applicants therefore believe that the type, level and molecular weight of the selected colloid combined with the resulting shell polymer of the delivery system and the particle size of the delivery system influence the odor profile (intensity or character) that the delivery system can provide.

[0006] Although such judicious selection will provide the desired beneficial effects, delivery particles containing beneficial agents are typically supplied in the form of slurries, and the use of polyvinyl alcohol as a colloid can reduce the stability of the slurry containing particles. The applicant has found that the root of the problem is that some of the polyvinyl alcohol used to make the particles exists as free polyvinyl alcohol in the slurry. In short, the free polyvinyl alcohol is not incorporated into the shell that encapsulates the beneficial agent. Such free polyvinyl alcohol causes depletion flocculation of the delivery particles containing the beneficial agent, which makes the slurry unstable. Such depletion flocculation is exacerbated by the presence of salts. In order to obtain an acceptable level of stability, the content of free polyvinyl alcohol can be reduced by appropriately selecting the content of polyvinyl alcohol used to prepare the delivery particles containing the beneficial agent, the type of polyvinyl alcohol can be judiciously selected, a more effective method for preparing the delivery particles containing the beneficial agent can be used, and / or the slurry can be refined to remove free polyvinyl alcohol. Preferably, the salt content is also minimized. Thus, slurries containing delivery particles containing benefit agents can be prepared and used which exhibit reduced benefit agent leakage yet provide desirable odor characteristics to wet and dry fabrics - especially enhanced pre-rub and post-rub benefits. Provided herein are methods for preparing and using such slurries and compositions containing them. Summary of the invention

[0007] The present invention relates to a slurry comprising a delivery particle containing a beneficial agent, the delivery particle comprising a core material and a shell material encapsulating the core material. The present invention also relates to compositions comprising the particles and methods for making and using such particles and compositions. DETAILED DESCRIPTION

[0008] definition

[0009] As used herein, "consumer product" means a baby care product, beauty care product, fabric and home care product, household care product, feminine care product, health product, snack and / or beverage product, or a device that is intended to be used or consumed in the form in which it is sold and is not intended for subsequent commercial manufacture or modification. Such products include, but are not limited to, fine fragrances (e.g., perfumes, colognes, eau de toilette, aftershaves, pre-shaves, moisture rehydrating lotions, tonics, and other fragrance-containing compositions for direct application to the skin), diapers, bibs, wipes; products and / or methods involving the treatment of hair (human, dog and / or cat), including bleaching, coloring, dyeing, conditioning, shampooing, styling; deodorants and antiperspirants; personal cleansing; cosmetics; skin care, including the application of creams, lotions and other topical products for consumer use; and shaving products, products and / or methods involving the treatment of fabrics, hard surfaces, and any other surfaces in the fabric and home care area, including: air care, car care, dishwashing, fabric conditioning (including softening ), laundry detergents, laundry and rinse additives and / or care, hard surface cleaning and / or treatment, and other cleaning for consumer or business use; products and / or methods involving toilet paper, facial tissue, tissues and / or paper towels; tampons, feminine hygiene napkins; products and / or methods involving oral care, including toothpaste, tooth gel, tooth cleaning, denture adhesives, tooth whitening; over-the-counter health care, including cough and cold remedies, pain relievers, RX remedies, pet health and nutrition, and purified water; processed food products primarily intended for consumption between daily meals or as a companion to meals (non-limiting examples include potato chips, unfermented corn chips, popcorn, crackers, corn chips, cereal bars, vegetable chips or crisps, snack mixes, party mixes, party chips, snack crackers, cheese snacks, pork rinds, corn snacks, pellet snacks, extruded snacks, and bagel chips); and coffee.

[0010] Unless otherwise indicated, as used herein, the term "cleaning composition" includes all-purpose or "heavy-duty" detergents in granular or powder form, especially cleaning detergents; all-purpose detergents in liquid, gel or paste form, especially the so-called heavy-duty liquid types; liquid fine fabric detergents; hand dishwashing detergents or light-duty dishwashing detergents, especially those of the high-sudsing type; machine dishwashing detergents, including the various pouches, tablets, granules, liquids and rinse-aid types for home and institutional use; liquid cleaning and disinfecting agents, including antibacterial hand wash types, cleaning bars, mouthwashes, denture cleaners, dentifrices, car or carpet washes, bathroom cleaners; hair shampoos and hair rinses; shower gels and foam baths and metal cleaners; and cleaning aids, such as bleach additives and "stain bars" or pre-treatment products carrying substrates, such as dryer sheets, dry and wet wipes and pads, nonwoven substrates and sponges; and sprays and aerosols.

[0011] Unless otherwise indicated, as used herein, the term "fabric care composition" includes fabric softening compositions, fabric enhancing compositions, fabric refreshing compositions and combinations thereof. The forms of such compositions include liquids, gels, beads, powders, flakes and granules.

[0012] As used herein, the phrase "benefit agent-containing delivery particles" encompasses microcapsules, including perfume microcapsules.

[0013] As used herein, the terms "particle," "benefit agent-containing delivery particle," "encapsulated benefit agent," "capsule," and "microcapsule" are synonymous.

[0014] As used herein, reference to the term "(meth)acrylate" or "(meth)acrylic" should be understood to refer to both the acrylate type and the methacrylate type of the designated monomer, oligomer and / or prepolymer (e.g., "allyl (meth)acrylate" means both allyl methacrylate and allyl acrylate are feasible, similarly, reference to alkyl (meth)acrylate means both alkyl acrylate and alkyl methacrylate are feasible, similarly, poly (meth)acrylate means both polyacrylate and polymethacrylate are feasible). Poly(meth)acrylate materials are intended to encompass a wide range of polymeric materials including, for example, polyester poly(meth)acrylates, urethane and polyurethane poly(meth)acrylates (particularly those prepared by the reaction of a hydroxyalkyl (meth)acrylate with a polyisocyanate or urethane polyisocyanate), methyl cyanoacrylate, ethyl cyanoacrylate, diethylene glycol di(meth)acrylate, trimethylolpropane tri(meth)acrylate, ethylene glycol di(meth)acrylate, allyl (meth)acrylate, glycidyl (meth)acrylate, (meth)acrylate functional siloxanes, diethylene glycol di(meth)acrylate, triethylene glycol di(meth)acrylate, and tetraethylene glycol di(meth)acrylate. (meth)acrylates, dipropylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, dipentyl glycol di(meth)acrylate, ethylene di(meth)acrylate, neopentyl glycol di(meth)acrylate, trimethylolpropane tri(meth)acrylate, ethoxylated bisphenol A di(meth)acrylate, bisphenol A di(meth)acrylate, diglycerol di(meth)acrylate, tetraethylene glycol dichloroacrylate, 1,3-butylene glycol di(meth)acrylate, neopentyl di(meth)acrylate, trimethylolpropane tri(meth)acrylate, polyethylene glycol di(meth)acrylate and dipropylene glycol di(meth)acrylate as well as various multifunctional (meth)acrylates. Monofunctional acrylates, i.e. those containing only one acrylate group, can also be used advantageously. Typical monoacrylates include 2-ethylhexyl (meth)acrylate, 2-hydroxyethyl (meth)acrylate, cyanoethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, p-dimethylaminoethyl (meth)acrylate, lauryl (meth)acrylate, cyclohexyl (meth)acrylate, tetrahydrofurfuryl (meth)acrylate, benzyl (meth)acrylate chloride, aminoalkyl (meth)acrylate, various alkyl (meth)acrylates, and glycidyl (meth)acrylate. Of course, mixtures of (meth)acrylates or their derivatives, as well as combinations of one or more (meth)acrylate monomers, oligomers, and / or prepolymers or their derivatives with other copolymerizable monomers (including acrylonitrile and methacrylonitrile) can also be used.

[0015] For the purpose of this patent application, castor oil, soybean oil, brominated vegetable oil, propan-2-yl myristate and mixtures thereof are not considered as perfume raw materials when calculating perfume compositions / formulations. Therefore, the amount of propan-2-yl myristate present is not used to make such calculations.

[0016] As used herein, the articles including "a" and "an" when used in a claim should be understood to mean one or more of what is claimed or described.

[0017] As used herein, the terms "including," "comprising," and "containing" are intended to be non-limiting.

[0018] The test methods disclosed in the test methods section of this application are used to determine the corresponding parameter values ​​of the applicant's invention.

[0019] Unless otherwise indicated, all component or composition levels are in reference to the active portion of that component or composition and are exclusive of impurities, for example, residual solvents or by-products, which may be present in commercially available sources of such component or composition.

[0020] Unless otherwise indicated, all percentages and ratios are calculated by weight. Unless otherwise indicated, all percentages and ratios are calculated based on the total composition.

[0021] It should be understood that each maximum numerical limit given throughout this specification includes each lower numerical limit, as if such lower numerical limits were expressly written herein. Each minimum numerical limit given throughout this specification will include each higher numerical limit, as if such higher numerical limits were expressly written herein. Each numerical range given throughout this specification will include each narrower numerical range falling within such wider numerical range, as if such narrower numerical ranges were all expressly written herein.

[0022] Consumer Products

[0023] The consumer products are disclosed in this section of the present patent application. The reference to the preceding paragraphs present in this section of the present patent application applies only to the paragraphs present in this section of the present patent application. Paragraphs are indicated by capital letters in parentheses, such as (A).

[0024] (A) A composition comprising a consumer product adjuvant material and a slurry, preferably the composition comprises from about 0.001% to about 20%, more preferably from about 0.3% to about 4%, most preferably from about 0.6% to about 2% of the slurry based on the total consumer product weight, the slurry comprising a delivery particle containing a benefit agent and a continuous phase containing water, the delivery particle comprising a core and a shell encapsulating the core, the slurry comprising:

[0025] a) from about 0.1% to about 0.8% polyvinyl alcohol in the continuous phase, more preferably 0.2% to 0.7% free polyvinyl alcohol in the continuous phase, most preferably 0.5% to 0.7% polyvinyl alcohol in the continuous phase, based on the total continuous phase water weight; and / or from about 0.1% to about 1.1% polyvinyl alcohol, more preferably 0.3% to 1% polyvinyl alcohol, most preferably 0.6% to 0.9% polyvinyl alcohol, based on the total benefit agent-containing delivery particle core weight; the polyvinyl alcohol based on the total water weight of the continuous phase and the polyvinyl alcohol based on the total benefit agent-containing delivery particle core weight preferably have at least one of the following properties, more preferably at least two of the following properties, more preferably at least three of the following properties, and most preferably all of the following properties:

[0026] (i) from about 55% to about 99%, preferably from about 75% to about 95%, more preferably about 85%

[0027] to a degree of hydrolysis of about 90%, most preferably about 87% to about 89%; and

[0028] (ii) a viscosity in a 4% aqueous solution at 20° C. of from about 40 mPa.s to about 120 mPa.s, preferably from about 40 mPa.s to about 90 mPa.s, more preferably from about 45 mPa.s to about 72 mPa.s, more preferably from about 45 mPa.s to about 60 mPa.s, and most preferably from 45 mPa.s to 55 mPa.s;

[0029] (iii) a degree of polymerization of from about 1,500 to about 2,500, preferably from about 1,600 to about 2,200, more preferably from about 1,600 to about 1,900, and most preferably from about 1,600 to about 1,800;

[0030] (iv) a number average molecular weight of about 65,000 Da to about 110,000 Da, preferably about 70,000 Da to about 101,000 Da, more preferably about 70,000 Da to about 90,000 Da, and most preferably about 70,000 Da to about 80,000 Da;

[0031] b) from about 30% to about 55%, more preferably from 36% to 50%, most preferably from 42% to 46%, based on the total slurry weight, of said delivery particles containing a beneficial agent, said delivery particles containing a beneficial agent preferably having a volume weighted average particle size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, preferably

[0032] The shell of the beneficial agent-containing delivery particle comprises the polyvinyl alcohol and one or more polyacrylate polymers, the core comprises greater than 10%, preferably greater than 20% to about 80%, greater than 20% to about 70%, more preferably greater than 20% to about 60%, more preferably from about 25% to about 60%, most preferably from about 25% to about 50% of a partitioning modifier based on the total core weight, the partitioning modifier comprising a material selected from the group consisting of propan-2-yl myristate, vegetable oils, modified vegetable oils, and mixtures thereof, preferably the modified vegetable oils are esterified and / or brominated, preferably the vegetable oils comprise castor oil and / or soybean oil;

[0033] c) a monovalent, divalent or trivalent inorganic salt, preferably a divalent salt, most preferably magnesium chloride or calcium chloride, preferably the slurry comprises 0% to about 4%, preferably 0% to about 2%, more preferably 0% to about 1%, most preferably 0% to about 0.6% of said salt based on the total slurry weight;

[0034] d) a polysaccharide and / or a hydrocolloid, preferably xanthan gum, guar gum, agar, konjac gum or gellan gum, more preferably xanthan gum, preferably the slurry comprises 0% to about 1%, preferably 0.05% to about 1%, more preferably about 0.1% to about 0.8%, more preferably about 0.15% to about 0.7%, most preferably about 0.2% to about 0.4% based on the total slurry weight;

[0035] The composition is disclosed as a consumer product.

[0036] (B) A composition according to paragraph (A), wherein the partitioning modifier comprises fourteen

[0037] Propan-2-yl ester.

[0038] (C) A composition according to any one of paragraphs (A) to (B), wherein the shell comprises a polymer

[0039] Acrylates, preferably the shell comprises from about 50% to about 100%, more preferably from about 70% to about 100%, most preferably from about 80% to about 100% of said polyacrylate polymer, preferably said polyacrylate comprises a polyacrylate cross-linked polymer.

[0040] (D) A composition according to any one of paragraphs (A) to (C), wherein the shell comprises a polymer

[0041] The invention relates to a polymer derived from a material comprising one or more multifunctional acrylate moieties; preferably the multifunctional acrylate moieties are selected from trifunctional acrylates, tetrafunctional acrylates, pentafunctional acrylates, hexafunctional acrylates, heptafunctional acrylates and mixtures thereof; and optionally a polyacrylate comprising moieties selected from the group consisting of amine acrylate moieties, methacrylate moieties, carboxylic acid acrylate moieties, carboxylic acid methacrylate moieties and combinations thereof.

[0042] (E) A composition according to any one of paragraphs (A) to (D), wherein the shell comprises a polymer

[0043] The polymer is derived from a material comprising one or more multifunctional acrylate and / or methacrylate moieties, preferably a ratio of material comprising one or more multifunctional acrylate moieties to material comprising one or more methacrylate moieties of from 999:1 to about 6:4, more preferably from about 99:1 to about 8:1, and most preferably from about 99:1 to about

[0044] 8.5:1; preferably, the multifunctional acrylate portion is selected from trifunctional acrylate, tetrafunctional acrylate, pentafunctional acrylate, hexafunctional acrylate, heptafunctional acrylate and mixtures thereof; and optionally polyacrylate, the polyacrylate comprising a portion selected from the group consisting of amine acrylate portion, methacrylate portion, carboxylic acid acrylate portion, carboxylic acid methacrylate portion and combinations thereof.

[0045] (F) A composition according to any of paragraphs (A) to (E), wherein the delivery particles containing the benefit agent have a volume weighted average particle size of from about 5 microns to about 45 microns, more preferably from about 8 microns to about 25 microns, or alternatively from about 25 microns to about 60 microns, more preferably from about 25 microns to about 60 microns, and the composition comprises from about 0.1% to about 35%, preferably from about 1% to about 35%, more preferably from about 2% to about 25%, more preferably from about 3% to about 20%, more preferably from about 5% to about 15%, most preferably from about 8% to about 12% or from about 3% to about 12%, preferably from about 4% to about 10%, more preferably from about 5% to about 8% of a fabric softener active, based on the weight of the total composition, preferably the fabric softener active is selected from quaternary ammonium compounds, amines, fatty acid esters, sucrose esters, silicones, dispersible polyolefins, clays, polysaccharides, lipids Fatty acids, softening oils, polymer latexes and mixtures thereof, more preferably the fabric softener active substance is selected from bis-(2-hydroxypropyl)-dimethyl ammonium methyl sulfate fatty acid ester, 1,2-di(acyloxy)-3-trimethylpropyl ammonium chloride, N,N-bis(stearoyloxyethyl)-N,N-dimethyl ammonium chloride, N,N-bis(tallow acyloxyethyl) N,N-dimethyl ammonium chloride, N,N-bis(stearoyloxyethyl) )N-(2-hydroxyethyl)-N-methyl ammonium methyl sulfate, N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethyl ammonium methyl sulfate, N,N-bis-(tallowyl-2-hydroxypropyl)-N,N-dimethyl ammonium methyl sulfate, N,N-bis-(palmitoyl-2-hydroxypropyl)-N,N-dimethyl ammonium methyl sulfate, N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethyl ammonium chloride, 1,

[0046] 2-di(stearoyloxy)3-trimethylpropylammonium chloride, di-low-erucic acid rapeseed dimethyl ammonium chloride, di(hard) tallow dimethyl ammonium chloride, di-low-erucic acid rapeseed dimethyl ammonium methyl sulfate, 1-methyl-1-stearoylaminoethyl-2-stearoyl imidazoline methyl sulfate, 1-tallowylamidoethyl-2-tallowyl imidazoline, dipalmitoyl hydroxyethyl ammonium methyl sulfate and mixtures thereof, and mixtures thereof, most preferably the fabric softener active is selected from N,N-bis(stearoyloxyethyl) N,N-dimethyl ammonium chloride; N,N-bis(tallowyloxyethyl) N,N-dimethylammonium chloride; N,N-bis(stearoyloxyethyl)N-(2-hydroxyethyl)N-methylammonium methyl sulfate; 1,2-di(stearoyloxy)3-trimethylpropylammonium chloride; N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethylammonium methyl sulfate, N,N-bis-(tallowyl-2-hydroxypropyl)-N,N-dimethylammonium methyl sulfate, N,N-bis-(palmitoyl-2-hydroxypropyl)-N,N-dimethylammonium methyl sulfate, N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethylammonium chloride, and mixtures thereof.

[0047] (G) A composition according to any one of paragraphs (A) to (F), comprising

[0048] From about 5% to about 95%, preferably from about 10% to about 95%, more preferably from about 20% to about 95%, more preferably from about 30% to about 80%, most preferably from about 50% to about 70% water by weight of the total composition, and from about 0.1% to about 25%, preferably from about 0.5% to about 20% of a surfactant, preferably the surfactant is selected from a nonionic surfactant or an anionic surfactant and mixtures thereof.

[0049] (H) A composition according to any one of paragraphs (A) to (G), wherein the composition comprises

[0050] From about 5% to about 20%, from about 8% to about 15%, from about 9% to about 13% water based on the total composition weight, the composition is encapsulated in a film, preferably the film comprises polyvinyl alcohol.

[0051] (I) A composition according to any one of paragraphs (A) to (G), comprising a liquid

[0052] and / or gel and a membrane encapsulating the liquid and / or gel, optionally the liquid or gel comprising suspended solids.

[0053] (J) A composition according to any one of paragraphs (A) to (G), wherein the delivery particles containing the beneficial agent have a volume weighted average particle size of about 2 microns to about 40 microns, preferably about 8 microns to about 25 microns, and the composition comprises about

[0054] 5% to about 95% free water and from about 0.5% to about 25% builder.

[0055] (K) A composition according to any one of paragraphs (A) to (J), comprising

[0056] Materials selected from the group consisting of hueing dyes, structurants, additional perfume delivery systems, and mixtures thereof, based on the total composition weight; preferably,

[0057] a) The structuring agent comprises a material selected from the following: polysaccharides, preferably the polysaccharides are selected from modified cellulose, chitosan, plant cellulose, bacterial cellulose, coated bacterial cellulose, preferably the bacterial cellulose comprises xanthan gum; castor oil, hydrogenated castor oil, modified protein, inorganic salt, quaternized polymer material, imidazole; non-ionic polymer with a pKa of less than 6.0, polyurethane, non-polymeric crystalline hydroxyl functionalized material, polymer structuring agent, diamido gelling agent, homopolymer of the following formula (Ia):

[0058]

[0059] in:

[0060] R 1 is selected from hydrogen or methyl;

[0061] R 2 Selected from hydrogen or C 1 –C 4 alkyl;

[0062] R 3 Selected from C 1 –C 4 Alkylene;

[0063] R 4 , R 5 and R 6 are each independently selected from hydrogen or C 1 -C 4 alkyl;

[0064] X is selected from -O- or -NH-, preferably -O-; and

[0065] Y is selected from Cl, Br, I, hydrogen sulfate or methyl sulfate;

[0066] and mixtures thereof;

[0067] b) the hueing dye is selected from small molecule dyes, polymeric dyes, dye-clay conjugates, and organic and inorganic pigments, preferably the hueing dye comprises a chromophore selected from one or more of the following: acridine, anthraquinone, azine, azo, azulene, benzodifuran and benzodifuranone, carotenoids, coumarins, cyanines, diazahemicyanines, diphenylmethanes, formazans, hemicyanines, indigos, methanes, naphthimides, naphthoquinones, nitro and nitroso groups, oxazines, phthalocyanines, pyrazoles, stilbenes, styryls, triarylmethanes, triphenylmethanes, xanthenes, and mixtures thereof; and

[0068] c) The additional perfume delivery comprises a material selected from the group consisting of: delivery particles containing a second benefit agent, a polymer-assisted delivery system; a molecule-assisted delivery system; a fiber-assisted delivery system; a cyclodextrin delivery system; a starch encapsulation formulation; and / or an inorganic carrier delivery system.

[0069] (L) A composition according to any of paragraphs (A) to (K), wherein the delivery particle containing the beneficial agent is prepared by a free radical polymerization process comprising the steps of combining from about 50% to about 100% of a hexafunctional urethane acrylate and / or a pentafunctional urethane acrylate, from about 0% to about 25%, preferably from about 0.01% to about 25%, based on the total free radical polymerization process acrylate monomer reactants, of a methacrylate containing an amino moiety, and from about 0% to about 25%, preferably from about 0.01% to about 25%, of an acrylate containing a carboxyl moiety, with the proviso that the sum of the hexafunctional urethane acrylate and / or pentafunctional urethane acrylate, the methacrylate containing an amino moiety, and the acrylate containing a carboxyl moiety is 100%, preferably the methacrylate containing an amino moiety comprises tert-butylaminoethyl methacrylate and the acrylate containing a carboxyl moiety comprises beta-carboxyethyl acrylate.

[0070] (M) A composition according to any one of paragraphs (A) to (L), comprising deposited

[0071] The deposition aid is preferably coated on the outer surface of the shell, and preferably the deposition aid comprises a material selected from the group consisting of poly(meth)acrylate, poly(ethylene-maleic anhydride), polyamine, wax, polyvinyl pyrrolidone, polyvinyl pyrrolidone copolymer, polyvinyl pyrrolidone-ethyl acrylate, polyvinyl pyrrolidone-vinyl acrylate, polyvinyl pyrrolidone methacrylate, polyvinyl pyrrolidone / vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxane, poly(propylene maleic anhydride), maleic anhydride derivatives, maleic anhydride derivatives copolymers of materials, polyvinyl alcohol, styrene-butadiene latex, gelatin, gum arabic, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, hydroxyethyl cellulose, other modified celluloses, sodium alginate, chitosan, casein, pectin, modified starch, polyvinyl acetal, polyvinyl butyral, polyvinyl methyl ether / maleic anhydride, polyvinyl pyrrolidone and its copolymers, poly(vinyl pyrrolidone / methacrylamidopropyltrimethylammonium chloride), polyvinyl pyrrolidone / vinyl acetate, polyvinyl pyrrolidone / dimethylaminoethyl methacrylate, poly The deposition aid comprises a material selected from the group consisting of poly(meth)acrylate, poly(ethylene-maleic anhydride), polyamine, polyvinylpyrrolidone, polyvinylpyrrolidone-ethyl acrylate, polyvinylpyrrolidone-vinyl acrylate, polyvinylpyrrolidone methacrylate, polyvinylpyrrolidone / vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxane, poly(propylene maleate), polyvinyl methacrylate, polyvinyl ...methacrylate, polyvinyl pyrrolidone / vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxane, poly(propylene maleate), polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate, polyvinyl methacrylate The invention also includes but is not limited to maleic anhydride, maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, chitosan, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, hydroxyethyl cellulose, polyvinyl methyl ether / maleic anhydride, poly(vinyl pyrrolidone / methacrylamidopropyltrimethylammonium chloride), polyvinyl pyrrolidone / vinyl acetate, polyvinyl pyrrolidone / dimethylaminoethyl methacrylate, polyvinylamine, polyvinylformamide, polyallylamine, and copolymers of polyvinylamine, polyvinylformamide, polyallylamine, and mixtures thereof.

[0072] Method of making a consumer product

[0073] This patent application discloses unique compositions, compositions prepared by methods, and methods of preparing compositions, the compositions comprising delivery particles containing a beneficial agent, the delivery particles comprising a core and a shell encapsulating the core. The reference to the preceding paragraphs present in this section of the patent application applies only to the paragraphs present in this section and the preceding sections of the patent application. New paragraphs in this section are represented by capital letters and numbers in parentheses, such as (A1).

[0074] (A1) A method of preparing a consumer product, preferably a consumer product according to paragraphs (A) to (M), the method comprising combining a consumer product adjunct ingredient and a slurry comprising a delivery particle comprising a benefit agent and a continuous phase comprising water, the delivery particle comprising a core and a shell encapsulating the core, the slurry being prepared by a method comprising:

[0075] emulsifying the combination of a) and b) to form an emulsion,

[0076] wherein a) is a first composition formed by combining a first oil and a second oil, wherein the first oil comprises a core comprising a fragrance, an initiator and a partition modifier, preferably the partition modifier comprises a material selected from the group consisting of vegetable oil, modified vegetable oil, propan-2-yl myristate and mixtures thereof, preferably the modified vegetable oil is esterified and / or brominated, preferably the vegetable oil comprises castor oil and / or soybean oil; preferably the partition modifier comprises propan-2-yl myristate;

[0077] The second oil comprises

[0078] (i) oil-soluble aminoalkyl acrylate and / or methacrylate monomers;

[0079] (ii) hydroxyalkyl acrylate monomers and / or oligomers;

[0080] (iii) a material selected from the group consisting of multifunctional acrylate monomers, multifunctional methacrylate monomers, multifunctional methacrylate oligomers, multifunctional acrylate oligomers, and mixtures thereof;

[0081] (iv) spices; and

[0082] wherein b) is a second composition comprising the continuous phase, a pH adjuster, an emulsifier, preferably an anionic emulsifier, preferably the emulsifier comprises polyvinyl alcohol and optionally an initiator; and,

[0083] The emulsion is heated in one or more heating steps to form a shell encapsulating the core, thereby forming a delivery particle containing a benefit agent, the delivery particle comprising the shell encapsulating the core and dispersed in the continuous phase.

[0084] Compositions disclosed herein can be prepared by combining slurries disclosed herein with desired consumer product auxiliary materials. When the slurry and such one or more consumer product auxiliary materials are in one or more forms (including pure slurry form, pure particle form and spray-dried particle form), they can be combined. The particles can be combined with such consumer product auxiliary materials by methods including mixing and / or spraying.

[0085] The cleaning and / or treatment compositions of the present invention may be formulated in any suitable form and prepared by any method selected by the formulator, non-limiting examples of which are described in US Pat. No. 5,879,584, which is incorporated herein by reference.

[0086] Suitable equipment for use in the methods disclosed herein may include continuous stirred tank reactors, homogenizers, turbine agitators, recirculation pumps, paddle mixers, plowshare shear mixers, ribbon blenders, vertical shaft granulators, and drum mixers (both in batch process configurations and in continuous process configurations when applicable), spray dryers, and extruders. Such equipment is available from Lodige GmbH (Paderborn, Germany), Littleford Day, Inc. (Florence, Kentucky, USA), Forberg AS (Larvik, Norway), Glatt Ingenieurtechnik GmbH (Weimar, Germany), Niro (Soeborg, Denmark), Hosokawa Bepex Corp. (Minneapolis, Minnesota, USA), Arde Barinco (New Jersey, USA).

[0087] Spices Raw Materials

[0088] Perfume raw materials that may be used as core materials are disclosed below.

[0089] Table 1: Available fragrance raw materials

[0090]

[0091]

[0092]

[0093]

[0094] Consumer product additive ingredients

[0095] The compositions disclosed herein may contain additional adjunct ingredients including: bleach activators, surfactants, builders, chelants, dye transfer inhibitors, dispersants, enzymes and enzyme stabilizers, catalytic metal complexes, polymeric dispersants, clay and soil removal / anti-redeposition agents, suds suppressors, dyes, additional perfumes and perfume delivery systems, structural elasticizers, fabric softeners, carriers, hydrotropes, processing aids, structurants, anti-agglomeration agents, coatings, formaldehyde scavengers and / or pigments. Other variations of the applicant's composition do not contain one or more of the following auxiliary materials: bleach activator, surfactant, builder, chelating agent, dye transfer inhibitor, dispersant, enzyme and enzyme stabilizer, catalytic metal complex, polymer dispersant, clay and soil removal / anti-redeposition agent, suds suppressor, dye, additional perfume and perfume delivery system, structure elasticizer, fabric softener, carrier, hydrotrope, processing aid, structurant, anti-agglomeration agent, coating, formaldehyde scavenger, malodor reduction material and / or pigment. The clear nature of these additional components and their incorporation content will depend on the physical form of the composition and the nature of its used operation. However, when there are one or more auxiliary agents, such one or more auxiliary agents may exist as described in detail below. The following is a non-limiting list of suitable additional auxiliary agents.

[0096] Deposition Aid - The fabric treatment composition may contain from about 0.01% to about 10%, from about 0.05 to about 5%, or from about 0.15% to about 3% of a deposition aid. The deposition aid may be a cationic polymer or an amphoteric polymer. The deposition aid may be a cationic polymer. In general, cationic polymers and methods of making them are known in the literature. The cationic polymer may have a cationic charge density of from about 0.005 meq / g to about 23 meq / g, from about 0.01 meq / g to about 12 meq / g, or from about 0.1 meq / g to about 7 meq / g at the pH of the composition. For amine-containing polymers where the charge density depends on the pH of the composition, the charge density is measured at the intended use pH of the product. Such pH will generally be in the range of from about 2 to about 11, more generally from about 2.5 to about 9.5. The charge density is calculated by dividing the net number of charges per repeat unit by the molecular weight of the repeat unit. The positive charge may be located on the polymer backbone and / or on the polymer side chains.

[0097] The deposition aid may include an acrylic acid-based cationic polymer. The deposition aid may include a cationic polyacrylamide. The deposition aid may include a polymer comprising polyacrylamide and polymethacrylamidopropyltrimethylammonium cations. The deposition aid may include poly(acrylamide-N-dimethylaminoethyl acrylate) and its quaternized derivatives.

[0098] The deposition aid may be selected from cationic polysaccharides or amphoteric polysaccharides. The deposition aid may be selected from cationic cellulose ethers and amphoteric cellulose ethers, cationic galactomannans or amphoteric galactomannans, cationic guar gum, cationic starches or amphoteric starches, and combinations thereof.

[0099] Another group of suitable cationic polymers may include alkylamine-epichlorohydrin polymers, which are the reaction products of amines and oligoamines with epichlorohydrin. Another group of suitable synthetic cationic polymers may include polyamidoamine-epichlorohydrin (PAE) resins of polyalkylenepolyamines and polycarboxylic acids. The most commonly used PAE resins are the condensation products of diethylenetriamine reacted with adipic acid followed by reaction with epichlorohydrin.

[0100] The weight average molecular weight of the polymer may be from about 500 Daltons to about 5,000,000 Daltons, or from about 1,000 Daltons to about 2,000,000 Daltons, or from about 2,500 Daltons to about 1,500,000 Daltons, as measured by size exclusion chromatography with RI detection relative to polyethylene oxide standards. The weight average molecular weight of the cationic polymer may be from about 500 Daltons to about 37,500 Daltons.

[0101] Surfactant: The surfactant used may be of anionic, nonionic, zwitterionic, ampholyte or cationic type, or may include compatible mixtures of these types. If the fabric care product is a laundry detergent, anionic and nonionic surfactants are generally employed. On the other hand, if the fabric care product is a fabric softener, cationic surfactants are generally employed. In addition to anionic surfactants, the fabric care compositions of the present invention may also contain nonionic surfactants. The compositions of the present invention may contain up to about 30%, or from about 0.01% to about 20%, or from about 0.1% to about 10% of nonionic surfactants by weight of the composition. Nonionic surfactants may include ethoxylated nonionic surfactants. Suitable for use herein are those of formula R(OC 2 H 4 )n OH ethoxylated alcohols and ethoxylated alkylphenols wherein R is selected from aliphatic hydrocarbon radicals containing from about 8 to about 20 carbon atoms, and alkylphenyl radicals wherein the alkyl radical contains from about 8 to about 12 carbon atoms, and wherein n has an average value of from about 5 to about 15.

[0102] Suitable nonionic surfactants are of formula R1(OC 2 H 4 ) n OH, where R1 is C 10 -C 16 Alkyl group or C 8 -C 12 alkylphenyl groups, and n is 3 to about 80. Particularly useful materials are C 9-C 15 The condensation products of alcohols with from about 5 to about 20 moles of ethylene oxide per mole of alcohol.

[0103] The fabric care compositions of the present invention may contain up to about 30%, alternatively from about 0.01% to about 20%, and alternatively from about 0.1% to about 20%, by weight of the composition, of a cationic surfactant. For purposes of the present invention, cationic surfactants include those that deliver fabric care benefits. Non-limiting examples of useful cationic surfactants include: fatty amines; quaternary ammonium surfactants; and imidazoline quaternary ammonium salt materials.

[0104] Non-limiting examples of fabric softening actives are N,N-bis(stearoyloxyethyl)N,N-dimethylammonium chloride; N,N-bis(tallow oxyethyl)N,N-dimethylammonium chloride, N,N-bis(stearoyloxyethyl)N-(2-hydroxyethyl)-N-methylammonium methyl sulfate; 1,2-di(stearoyloxy)3-trimethylpropylammonium chloride; dialkylene dimethyl ammonium salts such as canola dimethyl ammonium chloride, di(hard) tallow dimethyl ammonium chloride, canola dimethyl ammonium methyl sulfate; 1-methyl-1-stearoylaminoethyl 1-tallowamidoethyl-2-tallowimidazoline methyl sulfate; 1-tallowamidoethyl-2-tallowimidazoline; N,N"-dialkyldiethylenetriamine; reaction products of N-(2-hydroxyethyl)-1,2-ethylenediamine or N-(2-hydroxyisopropyl)-1,2-ethylenediamine esterified with fatty acids and glycolic acid, wherein the fatty acids are (hydrogenated) tallow fatty acid, palm fatty acid, hydrogenated palm fatty acid, oleic acid, rapeseed fatty acid, hydrogenated rapeseed fatty acid; polyglycerol esters (PGE), oily sugar derivatives and wax emulsions and mixtures of the above substances.

[0105] It will be understood that combinations of the softener actives disclosed above are suitable for use herein.

[0106] Builder-compositions may also contain about 0.1% to 80% by weight of a builder. Liquid compositions generally contain about 1% to 10% by weight of a builder component. Granular compositions generally contain about 1% to 50% by weight of a builder component. Detergent builders are well known in the art and may include, for example, phosphates and various organic and inorganic phosphorus-free builders. Water-soluble phosphorus-free organic builders that can be used herein include various alkali metal salts, ammonium salts and substituted ammonium salts of polyacetic acid, carboxylic acid, polycarboxylic acid and polyhydroxy sulfonic acid. Examples of polyacetate builders and polycarboxylate builders are sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, polycarboxylic acid benzene and citric acid. Other polycarboxylate builders are oxydisuccinates and ether carboxylate builder compositions, which include a combination of tartrate monosuccinate and tartrate disuccinate. Builders for liquid detergents include citric acid. Suitable non-phosphorus inorganic builders include silicates, aluminosilicates, borates and carbonates, such as sodium carbonate and potassium carbonate, sodium bicarbonate and potassium bicarbonate, sodium and potassium sesquicarbonate, sodium and potassium tetraborate decahydrate, and sodium and potassium silicates having a weight ratio of SiO2 to alkali metal oxide of about 0.5 to about 4.0, or about 1.0 to about 2.4. Also available are aluminosilicates, including zeolites.

[0107] Dispersants - The composition may contain from about 0.1% to about 10% by weight of a dispersant. Suitable water-soluble organic materials are homo- or co-polymeric acids or their salts in which the polycarboxylic acid may contain at least two carboxyl groups separated from each other by not more than two carbon atoms. The dispersant may also be an alkoxylated and / or quaternized derivative of a polyamine.

[0108] Enzyme-compositions can contain one or more detergent enzymes that provide cleaning performance and / or fabric care benefits. Examples of suitable enzymes include hemicellulases, peroxidases, proteases, cellulases, xylanases, lipases, phospholipases, esterases, cutinases, pectinases, cutinases, reductases, oxidases, phenoloxidases, lipoxygenases, ligninases, pullulanases, tannases, pentosanases, melanases, beta-glucanases, arabinosidases, hyaluronidases, chondroitinase, laccases, and amylases or mixtures thereof. Typical combinations can be mixtures of conventional available enzymes such as proteases, lipases, cutinases and / or cellulases in combination with amylases. Enzymes can be used in accordance with the content proposed in their field, for example, in accordance with the content recommended by suppliers such as Novozymes and Genencor. Typical levels in the composition are from about 0.0001% to about 5%. When enzymes are present, they can be used at very low levels, such as about 0.001% or less; or they can be used in heavy-duty laundry detergent formulations at higher levels, such as about 0.1% and higher. In accordance with the preference of some consumers for "non-biological" detergents, the compositions can be enzyme-containing and / or enzyme-free.

[0109] Dye transfer inhibitors - The composition may also contain from about 0.0001%, from about 0.01%, from about 0.05% to about 10%, to about 2%, or even to about 1%, by weight of the composition, of one or more dye transfer inhibitors such as polyvinyl pyrrolidone polymers, polyamine N-oxide polymers, copolymers of N-vinyl pyrrolidone and N-vinylimidazole, polyvinyl oxazolidones and polyvinylimidazoles, or mixtures thereof.

[0110] Chelating agents - The composition may contain less than about 5%, or from about 0.01% to about 3%, of chelating agents such as citrates; nitrogen-containing, phosphorus-free aminocarboxylates such as EDDS, EDTA and DTPA; aminophosphonates such as diethylenetriaminepentamethylenephosphonic acid and ethylenediaminetetramethylenephosphonic acid; nitrogen-free phosphonates, for example HEDP; and nitrogen- or oxygen-containing, phosphorus-free, carboxylate-free chelating agents such as the general class of compounds having certain macrocyclic N-ligands such as those known for use in bleach catalyst systems.

[0111] Bleach System - The bleach system suitable for use herein contains one or more bleaching agents. Non-limiting examples of suitable bleaching agents include catalytic metal complexes; active peroxygen sources; bleach activators; bleach boosters; photobleaches; bleaching enzymes; free radical initiators; H 2 O 2; hypochlorite bleach; peroxygen source, including perborate and / or percarbonate and combinations thereof. Suitable bleach activators include fully hydrolyzable esters and fully hydrolyzable imides, such as tetraacetylethylenediamine, octanoyl caprolactam, benzoyloxybenzene sulfonate, nonanoyloxybenzene sulfonate, benzoyl valerolactam, dodecanoyloxybenzene sulfonate. Other bleaching agents include metal complexes of transition metals with ligands having specified stability constants.

[0112] Stabilizers - The composition may contain one or more stabilizers and thickeners. Any suitable amount of stabilizer may be used; exemplary amounts include from about 0.01% to about 20%, from about 0.1% to about 10%, or from about 0.1% to about 3% by weight of the composition. Non-limiting examples of stabilizers suitable for use herein include crystallized hydroxyl-containing stabilizers, trihydroxystearin, hydrogenated oils, or variations thereof, and combinations thereof. In some aspects, the crystallized hydroxyl-containing stabilizer may be a water-insoluble waxy substance including fatty acids, fatty acid esters, or fatty soaps. In other aspects, the crystallized hydroxyl-containing stabilizer may be a derivative of castor oil, such as a hydrogenated castor oil derivative, for example castor wax. Other stabilizers include thickening stabilizers such as gums and other similar polysaccharides, for example gellan gum, carrageenan, and other known types of thickeners and rheological additives. Exemplary stabilizers of this type include gum-type polymers (e.g., xanthan gum), polyvinyl alcohol and its derivatives, cellulose and its derivatives (including cellulose ethers and cellulose esters), and tamarind gum (e.g., including xyloglucan polymers), guar gum, locust bean gum (in some aspects, including galactomannan polymers), and other industrial gums and polymers.

[0113] Siloxane - Suitable siloxanes contain Si-O moieties and may be selected from (a) non-functionalized siloxane polymers, (b) functionalized siloxane polymers, and combinations thereof. The molecular weight of an organosiloxane is typically shown by reference to the viscosity of the material. The organosiloxane may include a viscosity of from about 10 centistokes to about 2,000,000 centistokes at 25°C. Suitable organosiloxanes may have a viscosity of from about 10 centistokes to about 800,000 centistokes at 25°C.

[0114] Suitable organosiloxanes may be linear, branched or cross-linked.

[0115] The organosiloxane may include a cyclic siloxane. The cyclic siloxane may include a cyclic siloxane of the formula [(CH 3 ) 2 SiO] n The invention relates to a cyclomethicone, wherein n is an integer which may range from about 3 to about 7, or from about 5 to about 6.

[0116] Organosiloxanes can include functionalized siloxane polymers. Functionalized siloxane polymers can include one or more functional moieties selected from amino, amido, alkoxy, hydroxyl, polyether, carboxyl, hydrogen ion, sulfhydryl, sulfate, phosphate, and / or quaternary ammonium moieties. These moieties can be directly connected to the siloxane backbone (i.e., "side groups") via divalent alkylene groups, or can be a part of the backbone. Suitable functionalized siloxane polymers include materials selected from aminosiloxanes, amidosiloxanes, siloxane polyethers, siloxane-urethane polymers, quaternary ABn siloxanes, aminoABn siloxanes, and combinations thereof.

[0117] Functionalized silicone polymers may include silicone polyethers, which are also known as "dimethicone copolyols". Generally speaking, silicone polyethers contain a polydimethylsiloxane backbone with one or more polyoxyalkylene chains. The polyoxyalkylene moieties may be incorporated into the polymer as side chains or as end blocks. Functionalized silicone polymers may include aminosilicones.

[0118] Organosiloxanes may include amine ABn siloxanes and quaternary ABn siloxanes. Such organosiloxanes are generally prepared by reacting a diamine with an epoxide.

[0119] Functionalized silicone polymers may include silicone-urethanes. These are available under the trade name Commercially available from Wacker Silicones.

[0120] Perfume: The optional perfume component may include a component selected from the following

[0121] (1) a fragrance-containing delivery particle or a moisture-activated fragrance-containing delivery particle comprising a fragrance carrier and an encapsulated fragrance composition, wherein the fragrance carrier may be selected from cyclodextrin, starch microcapsules, porous carrier microcapsules, and mixtures thereof; and wherein the encapsulated fragrance composition may comprise a low volatility fragrance ingredient, a high volatility fragrance ingredient, and mixtures thereof;

[0122] (2) former fragrance;

[0123] (3) a low odor detection threshold fragrance ingredient, wherein the low odor detection threshold fragrance ingredient may be less than about 25% by weight of the total neat fragrance composition; and

[0124] (4) mixtures thereof; and

[0125] Porous Carrier Microcapsules - A portion of the perfume composition may also be absorbed onto and / or into a porous carrier such as a zeolite or clay to form perfume porous carrier microcapsules to reduce the amount of free perfume in the multi-use fabric conditioning composition.

[0126] Pro-Fragrance - The fragrance composition may further comprise a pro-fragrance. The pro-fragrance may comprise a non-volatile material that is released or converted into a fragrance material, for example, by simple hydrolysis, or may be a pro-fragrance triggered by a pH change (e.g., triggered by a drop in pH), or may be an enzyme-released pro-fragrance, or a light-triggered pro-fragrance. Depending on the pro-fragrance selected, the pro-fragrance may exhibit different release rates.

[0127] Fabric hueing agent - The composition may include a fabric hueing agent (sometimes referred to as a hueing agent, bluing agent or whitening agent). Hueing agents typically provide a blue or purple hue to the fabric. Hueing agents can be used alone or in combination to produce a specific hueing shade and / or to shade different fabric types. This can be provided, for example, by mixing a red and a cyan dye to produce a blue or purple hue. The tinting agent may be selected from any known chemical class of dyes including, but not limited to, acridines, anthraquinones (including polycyclic quinones), azines, azos (e.g., monoazo, disazo, trisazo, tetrakisazo, polyazos), including premetallated azos, benzodifurans and benzodifuranones, carotenoids, coumarins, cyanines, diazahemicyanines, diphenylmethanes, formazans, hemicyanines, indigos, methanes, naphthamides, naphthoquinones, nitro and nitroso, oxazines, phthalocyanines, pyrazoles, stilbenes, styryls, triarylmethanes, triphenylmethanes, xanthenes, and mixtures thereof.

[0128] Suitable fabric hueing agents include dyes, dye-clay conjugates, and organic and inorganic pigments. Suitable dyes include small molecule dyes and polymeric dyes. Suitable small molecule dyes include those selected from the following small molecule dyes: dyes belonging to the Color Index (CI) classification of acidic, direct, basic, reactive, or hydrolyzed reactive, solvent or disperse dyes, such as dyes classified as blue, purple, red, green or black, and provide desired hues individually or in combination. Suitable small molecule dyes include small molecule dyes selected from the following numbered ones of the Colour Index (British Institute of Dyers, Bradford, UK): direct violet dyes such as 9, 35, 48, 51, 66 and 99, direct blue dyes such as 1, 71, 80 and 279, acid red dyes such as 17, 73, 52, 88 and 150, acid violet dyes such as 15, 17, 24, 43, 49 and 50, acid blue dyes such as 15, 17, 25, 29, 40, 45, 75, 80, 83, 90 and 113, acid black dyes such as 1, basic violet dyes such as 1, 3, 4, 10 and 35, basic blue dyes such as 3, 16, 22, 47, 66, 75 and 159, disperse dyes or solvent dyes (US 8,268,016 B2), or dyes as disclosed in US 7,208,459 B2, and mixtures thereof. Suitable small molecule dyes include small molecule dyes selected from the following: CI number acid violet 17, acid blue 80, acid violet 50, direct blue 71, direct violet 51, direct blue 1, acid red 88, acid red 150, acid blue 29, acid blue 113 or mixtures thereof.

[0129] Suitable polymeric dyes include those selected from the group consisting of polymers containing a covalently bound (sometimes referred to as conjugated) chromogen (dye-polymer conjugate) (e.g., a polymer having a chromogen copolymerized into the polymer backbone) and mixtures thereof. Polymeric dyes include those described in US 7,686,892 B2.

[0130] Suitable polymeric dyes include those selected from the group consisting of polymeric dyes sold under the trade names (Milliken, Spartanburg, South Carolina, USA), a dye-polymer conjugate formed from at least one reactive dye, and a polymer selected from a polymer comprising a moiety selected from the group consisting of a hydroxyl moiety, a primary amine moiety, a secondary amine moiety, a thiol moiety, and mixtures thereof. Suitable polymeric dyes include polymeric dyes selected from the group consisting of: Violet CT, carboxymethyl cellulose (CMC) covalently bound to a reactive blue, reactive violet or reactive red dye, such as CMC conjugated to CI Reactive Blue 19 (sold by Megazyme, Wicklow, Ireland under the product name AZO-CM-CELLULOSE, product code S-ACMC), alkoxylated triphenyl-methane polymer colorants, alkoxylated thiophene polymer colorants, and mixtures thereof.

[0131] Suitable dye clay conjugates include dye clay conjugates selected from the following: at least one cationic / basic dye and a smectite clay, and mixtures thereof. Suitable dye clay conjugates include dye clay conjugates selected from the following: a cationic / basic dye selected from: CI Basic Yellow 1 to 108, CI Basic Orange 1 to 69, CI Basic Red 1 to 118, CI Basic Violet 1 to 51, CI Basic Blue 1 to 164, CI Basic Green 1 to 14, CI Basic Brown 1 to 23, CI Basic Black 1 to 11 and clay selected from montmorillonite clay, hectorite clay, saponite clay and mixtures thereof. Suitable dye clay conjugates include dye clay conjugates selected from the group consisting of montmorillonite basic blue B7 CI42595 conjugate, montmorillonite basic blue B9 CI52015 conjugate, montmorillonite basic violet V3 CI42555 conjugate, montmorillonite basic green G1 CI42040 conjugate, montmorillonite basic red R1 CI45160 conjugate, montmorillonite CI basic black 2 conjugate, hectorite basic blue B7 CI42595 conjugate, hectorite basic blue B9 CI52015 conjugate, hectorite basic violet V3 CI42555 conjugate, hectorite basic green G1 CI42040 conjugate, hectorite basic red R1 CI45160 conjugate, hectorite CI basic black 2 conjugate, soap basic blue B7 CI42595 conjugate, soap basic blue B9 CI52015 conjugate, hectorite basic violet V3 CI42555 conjugate, CI52015 conjugate, Soap Basic Violet V3 CI42555 conjugate, Soap Basic Green G1 CI42040 conjugate, Soap Basic Red R1 CI45160 conjugate, Soap CI Basic Black 2 conjugate and mixtures thereof.

[0132] Toners can be incorporated into detergent compositions as part of a reaction mixture that is the result of an organic synthesis of dye molecules by one or more optional purification steps. Such reaction mixtures generally contain the dye molecules themselves, and in addition may also contain unreacted starting materials and / or by-products of the organic synthesis route.

[0133] Suitable polymer bluing agents may be alkoxylated. As with all such alkoxylated compounds, organic synthesis may prepare mixtures of molecules having different degrees of alkoxylation. Such mixtures may be used directly to provide a toner, or may undergo a purification step to increase the proportion of the target molecule.

[0134] Suitable pigments include those selected from the group consisting of flavanthrone, indanthrone, chlorinated indanthrone containing 1 to 4 chlorine atoms, pyranthrone, dichloropyranthrone, monobromodichloropyranthrone, dibromodichloropyranthrone, tetrabromopyranthrone, perylene-3,4,9,10-tetracarboxylic acid diimide, wherein the imide group may be unsubstituted or substituted with C 1 -C 3 -alkyl or phenyl or heterocyclic group substitution, and wherein the phenyl and heterocyclic groups may additionally carry substituents that do not provide solubility in water, anthrapyrimidinecarboxylic acid amides, anthrone violet, isoanthrone violet, dioxazine pigments, copper phthalocyanines that may contain up to 2 chlorine atoms per molecule, polychlorinated copper phthalocyanines or polybrominated chlorinated copper phthalocyanines containing up to 14 bromine atoms per molecule, and mixtures thereof. Suitable pigments include pigments selected from the group consisting of Ultramarine Blue (CI Pigment Blue 29), Ultramarine Violet (CI Pigment Violet 15), Monostellar Blue and mixtures thereof.

[0135] The above fabric hueing agents may be used in combination (any mixture of fabric hueing agents may be used).

[0136] Structuring agents - Useful structurant materials that can be added to adequately suspend the delivery particles containing the beneficial agent include polysaccharides such as gellan gum, waxy corn or dent corn starch, starch octenyl succinate, derivatized starches such as hydroxyethylated or hydroxypropylated starches, carrageenan, guar gum, pectin, xanthan gum, and mixtures thereof; modified celluloses such as hydrolyzed cellulose acetate, hydroxypropyl cellulose, methyl cellulose, and mixtures thereof; modified proteins such as gelatin; hydrogenated and unhydrogenated polyolefins, and mixtures thereof; inorganic salts such as magnesium chloride, calcium chloride, calcium formate, magnesium formate, aluminum chloride, potassium permanganate, laponite clay, bentonite, and mixtures thereof; polysaccharides in combination with inorganic salts; quaternized polymeric materials such as polyetheramines, alkyltrimethylammonium chloride, diester ditallow ammonium chloride; imidazoles; nonionic polymers having a pKa of less than 6.0, such as polyethyleneimine, polyethyleneimine ethoxylates; polyurethanes. Such materials are available from CP Kelco Corp. (San Diego, California, USA); Degussa AG or Dusseldorf, Germany; BASF AG (Ludwigshafen, Germany); Rhodia Corp. (Cranbury, New Jersey, USA); Baker Hughes Corp. (Houston, Texas, USA); Hercules Corp. (Wilmington, Delaware, USA); Agrium Inc. (Calgary, Alberta, Canada), ISP (New Jersey, USA).

[0137] Anti-agglomeration agents - Available anti-agglomeration agent materials include divalent salts, such as magnesium salts, for example, magnesium chloride, magnesium acetate, magnesium phosphate, magnesium formate, magnesium boride, magnesium titanate, magnesium sulfate heptahydrate; calcium salts, for example, calcium chloride, calcium formate, calcium acetate, calcium bromide; trivalent salts, such as aluminum salts, for example, aluminum sulfate, aluminum phosphate, aluminum chlorohydrate, and polymers having the ability to suspend anionic particles, such as suspending polymers, for example, polyethyleneimine, alkoxylated polyethyleneimine, polyquaternium-6 and polyquaternium-7.

[0138] Coating - Delivery particles containing beneficial agents can be manufactured and subsequently coated with additional materials. Non-limiting examples of coating materials include, but are not limited to, materials selected from the group consisting of poly(meth)acrylates, poly(ethylene-maleic anhydride), polyamines, waxes, polyvinylpyrrolidone, polyvinylpyrrolidone copolymers, polyvinylpyrrolidone-ethyl acrylate, polyvinylpyrrolidone-vinyl acrylate, polyvinylpyrrolidone methacrylate, polyvinylpyrrolidone / vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxanes, poly(propylene maleic anhydride), maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, styrene-butadiene latex, gelatin, gum arabic, carboxymethyl cellulose cellulose, carboxymethyl hydroxyethyl cellulose, hydroxyethyl cellulose, other modified cellulose, sodium alginate, chitosan, casein, pectin, modified starch, polyvinyl acetal, polyvinyl butyral, polyvinyl methyl ether / maleic anhydride, polyvinyl pyrrolidone and copolymers thereof, poly(vinyl pyrrolidone / methacrylamidopropyltrimethylammonium chloride), polyvinyl pyrrolidone / vinyl acetate, polyvinyl pyrrolidone / dimethylaminoethyl methacrylate, polyvinyl amine, polyvinyl formamide, polyallylamine, copolymers of polyvinyl amine, polyvinyl formamide and polyallylamine, and mixtures thereof. Such materials are available from CP Kelco Corp. (San Diego, California, USA); Degussa AG or Dusseldorf, Germany; BASF AG (Ludwigshafen, Germany); Rhodia Corp. (Cranbury, New Jersey, USA); Baker Hughes Corp. (Houston, Texas, USA); Hercules Corp. (Wilmington, Delaware, USA); Agrium Inc. (Calgary, Alberta, Canada), ISP (New Jersey, USA).

[0139] Odor Reduction Materials

[0140] The compositions of the present invention may contain malodour reducing materials. Such materials are capable of reducing or even eliminating the perception of one or more malodours.

[0141] The compositions of the present invention may comprise from about 0.00025% to about 0.5%, preferably from about 0.0025% to about 0.1%, more preferably from about 0.005% to about 0.075%, most preferably from about 0.01% to about 0.05% of one or more malodor reduction materials by weight of the composition. The composition may comprise from about 1 to about 20 malodor reduction materials, more preferably from 1 to about 15 malodor reduction materials, most preferably from 1 to about 10 malodor reduction materials.

[0142] The compositions of the present invention may include a fragrance that provides a hedonic benefit. The weight ratio of the malodor reduction composition to the fragrance may be from about 1:20,000 to about 3,000:1, preferably from about 1:10,000 to about 1,000:1, more preferably from about 5,000:1 to about 500:1, and most preferably from about 1:15 to about 1:1. As the ratio of the malodor reduction composition to the fragrance decreases, the one or more malodor reduction materials provide less and less odor impact while continuing to combat malodor.

[0143] The composition may comprise one or more malodor reducing materials having a log P greater than 3, preferably greater than 3 but less than 11. The one or more malodor reducing materials may be selected from the group consisting of materials 7; 14; 39; 48; 183; 185; 195; 206; 212; 215; 227; 228; 229; 230; 231; 248; 260; 261; 276; 289; 335; 343; 360; 391; 428; 441; 484; 487; 488; 501; 520; 566; 567; 5 69; 570; 572; 573; 574; 592; 603; 616; 621; 624; 627; 632; 644; 663; 677; 679; 680; 684; 694; 696; 700; 704; 708; 712; 714; 722; 723; 726; 750; 769; 775; 776; 788; 804; 872; 912; 919; 925; 927; 933; 978; 1007; 1022; 1024; 1029; 1035; 1038; 1060; 1073; 1077; 1089; 1107; 1129; 1131; 1137; 1140; 1142; 1143; 1144; 1145; 1148; 1149; 1152; 1153; 1154 and mixtures thereof, preferably Preferably, the material is selected from the group consisting of materials 185; 215; 260; 261; 276; 289; 335; 391; 428; 441; 501; 520; 572; 573; 592; 627; 677; 700; 769; 788; 912; 919; 925; 1073; 1129; 1148; 1149; 1152; 1153; 1154 and mixtures thereof. All of the foregoing materials have a log P equal to or greater than 3 but less than 11, and therefore they are deposited by particularly thorough washing. The more preferred and most preferred foregoing materials are particularly preferred because they effectively counteract all key malodors.

[0144] A non-limiting group of suitable malodor reduction materials is provided in Table 2 below. The compositions described herein may include a malodor reduction material selected from any one of the materials listed in Table 2, or a combination thereof. For ease of reference herein, each material in Table 2 is assigned a numerical identifier, which can be found in the column of each table, which is designated as serial number .

[0145] Table 2: List of Materials

[0146]

[0147]

[0148]

[0149]

[0150] The materials in Table 2 can be supplied by one or more of the following: Firmenich Inc. (Plainsboro NJ USA); International Flavor and Fragrance Inc. (New York, NY USA); Takasago Corp. (Teterboro, NJ USA); Symrise Inc. (Teterboro, NJ USA); Sigma-Aldrich / SAFC Inc. (Carlsbad, CA USA); and Bedoukian Research Inc. (Danbury, CT USA).

[0151] Directions for use and areas to be treated

[0152] The compositions disclosed herein comprising delivery particles containing a beneficial agent can be used to clean or treat a situs, particularly a surface or fabric. Typically, at least a portion of the situs is contacted with an embodiment of Applicants' composition (in neat form or diluted in a liquid, such as a wash liquor), and then the situs can be optionally washed and / or rinsed.

[0153] A method of treating and / or cleaning a site is disclosed, the method comprising

[0154] a) optionally washing, rinsing and / or drying the area;

[0155] b) contacting the site with a consumer product according to any one of paragraphs (A) to (M) of this specification and / or prepared by the method of paragraph (A1) of this specification; and

[0156] c) optionally washing, rinsing and / or drying the site, wherein the drying step comprises active drying and / or passive drying.

[0157] For purposes of the present invention, washing includes, but is not limited to, scrubbing and mechanical agitation. Fabrics may include any fabric that can be washed or handled under normal consumer use conditions. The liquid that may contain the disclosed composition may have a pH of about 3 to about 11.5. Such compositions are typically used at a concentration of about 500 ppm to about 15,000 ppm in solution. When the washing solvent is water, the water temperature is typically in the range of about 5°C to about 90°C, and when the site includes fabric, the ratio of water to fabric is typically about 1:1 to about 30:1.

[0158] Disclosed is a situs treated with any embodiment of any composition disclosed herein.

[0159] Disclosed is a situs treated with a consumer product according to any one of paragraphs (A) to (M) of this specification and / or prepared by the method of paragraph (A1) of this specification.

[0160] Test Method

[0161] It should be understood that the test methods disclosed in the Test Methods section of this application should be used to determine the corresponding parameter values ​​of Applicants' invention as described and claimed herein.

[0162] (1) Extraction of delivery particles containing beneficial agents from finished products

[0163] Unless otherwise specified herein, the preferred method for separating the delivery particles containing the beneficial agent from the finished product is based on the fact that the density of most such particles is different from the density of water. The finished product is mixed with water to dilute and / or release the particles. The diluted product suspension is centrifuged to accelerate the separation of the particles. Such particles tend to float or settle in the dilute solution / dispersion of the finished product. Using a pipette or a spatula, remove the top and bottom layers of the suspension and undergo additional dilution and centrifugation cycles to separate and enrich the particles. Use an optical microscope equipped with a cross-polarized filter or differential interference contrast (DIC) to observe the particles at a total magnification of 100 times and 400 times. Microscopic observation provides an initial indication of the presence, size, quality and aggregation of the delivery particles.

[0164] To extract the delivery particles from the liquid fabric enhancer, the finished product undergoes the following steps:

[0165] 1. Place three approximately 20 ml aliquots of liquid fabric enhancer into three separate 50 ml centrifuge tubes and dilute each aliquot 1:1 with deionized water (e.g. 20 ml fabric enhancer + 20 ml deionized water), mix each aliquot thoroughly, and centrifuge each aliquot at approximately 10,000 x g for 30 minutes.

[0166] 2. After centrifugation in step 1, discard the bottom water layer (about 10 ml) in each 50 ml centrifuge tube, and then add 10 ml of deionized water to each 50 ml centrifuge tube.

[0167] 3. For each aliquot, the process of centrifuging, removing the bottom aqueous layer, and then adding 10 ml of deionized water to each 50 ml centrifuge tube was repeated two more times.

[0168] 4. Remove the top layer with a spatula or pipette.

[0169] 5. Transfer the top layer to a 1.8 ml centrifuge tube and centrifuge at approximately 20,000 x g for 5 minutes.

[0170] 6. Remove the top layer with a scraper and transfer to a new 1.8 ml centrifuge tube and add deionized water until the tube is completely full, then centrifuge at approximately 20,000 x g for 5 minutes.

[0171] 7. Remove the bottom layer with a fine pipette and add deionized water until the tube is completely full and centrifuge at approximately 20,000 x g for 5 minutes.

[0172] 8. Repeat step 7 5 more times (6 times in total).

[0173] If both the top layer and the bottom layer of the enriched particles appear in the above step 1, then immediately go to step 3 (i.e., ignore step 2) and continue with the steps 4 to 8. Once those steps have been completed, use a scraper or / and a pipette to remove the bottom layer from the 50 ml centrifuge tube of step 1. The bottom layer is transferred to a 1.8 ml centrifuge tube and centrifuged at approximately 20,000 × g for 5 minutes. The bottom layer in the new tube is removed and deionized water is added until the tube is completely full, and then centrifuged at approximately 20,000 × g for 5 minutes. The top layer (water) is removed and deionized water is added again until the tube is full. This is repeated 5 more times (6 times in total). The enriched particles and the separated top and bottom layers are reassembled together.

[0174] If the fabric enhancer has a white color, or the particle-rich layer is difficult to discern, add 4 drops of dye (such as Liquitint Blue JH 5% premix from Milliken & Company (Spartanburg, South Carolina, USA) to the centrifuge tube in step 1 and separate as described.

[0175] For extraction of delivery particles from solid finished products that are easily dispersed in water, 1 L of deionized water is mixed with 20 g of the finished product (e.g., detergent foams, films, gels, and granules; or water-soluble polymers; soap flakes and bars; and other readily water-soluble matrices such as salts, sugars, clays, and starches). When extracting particles from finished products that are not easily dispersed in water, such as waxes, dryer sheets, dryer strips, and greasy materials, it may be necessary to add detergent, stir and / or gently heat the product, and dilute to release the particles from the matrix. The use of organic solvents or drying of the particles should be avoided during the extraction step, as these actions can damage the delivery particles during this stage.

[0176] To extract the delivery particles from a liquid finished product that is not a fabric softener or fabric enhancer (e.g., liquid laundry detergent, liquid dishwashing detergent, liquid hand soap, lotion, shampoo, conditioner, and hair dye), 20 ml of the finished product is mixed with 20 ml of deionized water. If necessary, NaCl (e.g., 100 g to 200 g NaCl) can be added to the diluted suspension to increase the density of the solution and facilitate the particles to float to the top layer. If the product has a white color that makes it difficult to distinguish the particle layer formed during centrifugation, a water-soluble dye can be added to the diluent to provide visual contrast.

[0177] The water and product mixture is subjected to successive centrifugation cycles involving removal of the top and bottom layers, resuspension of those layers in new diluent, and further centrifugation, separation, and resuspension. Each centrifugation cycle occurs in a tube of 1.5 ml to 50 ml volume, using a centrifugal force of up to 20,000 × g, for a period of 5 minutes to 30 minutes. At least six centrifugation cycles are typically required to extract and clean enough particles for testing. For example, an initial centrifugation cycle may be performed in a 50 ml tube, spinning at 10,000 × g for 30 minutes, followed by five additional centrifugation cycles in which the material from the top and bottom layers is individually resuspended in new diluent in a 1.8 ml tube, and each cycle is spun at 20,000 × g for 5 minutes.

[0178] If delivery particles are observed microscopically in both the top and bottom layers, the particles from these two layers are recombined after the final centrifugation step to form a single sample containing all the delivery particles extracted from the product. The extracted particles should be analyzed as quickly as possible, but they can be stored as a suspension in deionized water for up to 14 days prior to analysis.

[0179] Those skilled in the art will recognize that various other schemes may be devised for extracting and isolating the delivery particles from the finished product, and will recognize that such methods need to be validated by comparing the resulting measurements taken before and after the particles are added to and extracted from the finished product.

[0180] (2) Particle size (diameter)

[0181] A drop of particle suspension or finished product is placed on a microscope glass slide and dried for several minutes at ambient conditions to remove water and obtain a sparse monolayer of individual particles on the dried slide. The concentration of particles in the suspension is adjusted as needed to obtain a suitable particle density on the slide. The slide is placed on the sample stage of an optical microscope equipped with 100x or 400x total magnification and examined at this magnification. The image is captured and calibrated to accurately measure the particle size. Three replicate slides are prepared and analyzed.

[0182] To measure particle size, at least 50 delivery particles containing beneficial agents are selected on each slide for measurement in a manner that is not biased by their size, thereby forming a representative sample presenting a particle size distribution. This can be achieved by examining a field of view selected randomly or according to a predefined grid pattern, and by measuring the diameters of all delivery particles presented in each field of view examined. Delivery particles that appear to be obviously non-spherical, deflated, leaking, or damaged are not suitable for measurement, are not included in the selection process, and their diameters are not recorded. The diameter of each suitable delivery particle examined is measured using a microscope, and the value is recorded. The recorded particle size measurements are used to calculate the percentage of particles having a particle size within one or more particle size ranges protected by the claims, and are also used to calculate the average particle size.

[0183] (3) Particle shell thickness

[0184] Using a freeze fracture low temperature scanning electron microscope (FF cryoSEM), at a magnification between 50,000 times and 150,000 times, the particle shell thickness of 50 delivery particles containing beneficial agents is measured in nanometers. By flash freezing a small volume suspension of particles or finished products, the sample is prepared. Flash freezing can be achieved by immersion in liquid ethane, or by using a device such as a 706802EM Pact type high pressure freezer (Leica Microsystems, Wetzlar, Germany). The frozen sample is broken at -120 ° C, then cooled to less than -160 ° C, and slightly sputtered with gold / palladium. Low temperature preparation devices such as those from Gatan Inc. (Pleasanton, CA, USA) can be used to achieve these steps. Then at -170 ° C or lower temperatures, the frozen, broken and coated samples are transferred to a suitable cryoSEM microscope such as Hitachi S-5200SEM / STEM (Hitachi High Technologies, Tokyo, Japan). Imaging was performed in a Hitachi S-5200 with 3.0 KV accelerating voltage and 5 μA to 20 μA tip emission current.

[0185] Images of the broken shells were collected in the form of cross-sectional views of 50 beneficial delivery particles selected in a random manner without bias due to their size to form a representative sample of the particle size distribution of the present invention. The shell thickness of each of the 50 particles was measured using calibrated microscope software by drawing a measurement line perpendicular to the outer surface of the particle wall. The 50 independent shell thickness measurements were recorded and used to calculate the average thickness, and the percentage of particles having a shell thickness within the claimed range.

[0186] (4) Leakage of beneficial agents

[0187] The beneficial agent leakage of the delivery particles was determined according to the following method:

[0188] a.) Obtain two 1 g samples of the stock slurry of benefit delivery particles.

[0189] b.) 1 g of the raw slurry of benefit delivery particles was added to 99 g of the product matrix in which the particles will be employed, and the mixture was labeled Sample 1. A second 1 g sample of the raw particle slurry in its pure form without contact with the product matrix was used immediately in step d below, and it was labeled Sample 2.

[0190] c.) The product matrix containing the particles (Sample 1) was aged in a sealed glass jar at 35°C for 2 weeks.

[0191] d.) Recover particles from both samples by filtration. Particles from Sample 1 (in product matrix) were recovered after the aging step. Particles from Sample 2 (pure raw material slurry) were recovered at the same time as the aging step for Sample 1 was initiated.

[0192] e.) treating the recovered particles with a solvent to extract the benefit agent material from the particles.

[0193] f.) The solvent containing the beneficial agent extracted from each sample is analyzed via chromatography. The resulting beneficial agent peak areas under the curve are integrated and the areas are summed to determine the total amount of beneficial agent extracted from each sample.

[0194] g.) Determine the benefit agent leakage percentage by calculating the difference between the total amount of benefit agent extracted from Sample 2 and the total amount of benefit agent extracted from Sample 1, expressed as a percentage of the total amount of benefit agent extracted from Sample 2, as represented by the following formula:

[0195]

[0196] (5) Viscosity

[0197] The viscosity of the liquid finished product was measured using an AR 550 Rheometer / Viscometer from TA instruments, using parallel steel plates with a 40 mm diameter and a 500 μm gap size. -1 High shear viscosity and 0.05 -1 The low shear viscosity can be increased from 0.1s to -1 Up to 25s -1 The logarithmic shear rate scan was performed.

[0198] (6) Flavors and flavor raw materials (PRMs)

[0199] To determine the identity of the fragrance, fragrance ingredient or fragrance raw material (PRM) encapsulated in the delivery agent particles and to quantify the weight, a gas chromatography with a mass spectrometer / flame ionization detector (GC-MS / FID) is used. Suitable equipment includes: Agilent Technologies G1530A GC / FID; Hewlett Packard mass selective device 5973; and 5% phenyl-methyl polysiloxane column J&W DB-5 (30m long×0.25mm inner diameter×0.25μm film thickness). Approximately 3g of the finished product or suspension of the delivery particles is weighed and the weight is recorded, then the sample is diluted with 30mL of deionized water and filtered through a 5.0μm pore size nitrocellulose filter membrane. The material trapped on the filter is dissolved in 5mL of ISTD solution (25.0mg / L tetradecane in anhydrous alcohol) and heated at 60°C for 30 minutes. The cooled solution is filtered through a 0.45μm pore size PTFE syringe filter and analyzed via GC-MS / FID. Three known fragrance oils were used as comparative benchmark standards. Data analysis involved summing the total area counts minus the ISTD area counts and calculating the average response factor (RF) of the three standard fragrances. The response factor and total area counts of the product of the encapsulated fragrance were then used together with the sample weight to determine the total weight percentage of each PRM in the encapsulated fragrance. PRMs were indicated by mass spectrum peaks.

[0200] (7) Volume weighted average particle size

[0201] Particle size is measured using a static light scattering device such as an Accusizer 780A manufactured by Particle Sizing Systems (Santa Barbara CA). The instrument is calibrated from 0μ to 300μ using a Duke particle size standard. If the volume weighted average particle size of an emulsion is to be determined, about 1 g of the emulsion is diluted in about 5 g of deionized water and about 1 g of the solution is further diluted in about 25 g of water, or if the volume weighted average particle size of the finished particles is to be determined, 1 g of a delivery particle slurry containing a benefit agent is diluted in about 5 g of deionized water and about 1 g of the solution is further diluted in about 25 g of water to prepare samples for particle size evaluation.

[0202] About 1g of the most diluted sample is added to the Accusizer and the test is started, using the automatic dilution feature. The Accusizer should be read at over 9200 counts / second. If the count is less than 9200, additional sample should be added. The accusizer will dilute the test sample until 9200 counts / second and begin evaluation. 2 minutes after the test, the Accusizer will display the results, including the volume-weighted median particle size.

[0203] The breadth index can be calculated by determining the particle size exceeding 95% of the cumulative particle volume (95% size), the particle size exceeding 5% of the cumulative particle volume (5% size), and the median volume-weighted particle size (50% particle size - 50% of the particle volume both above and below this particle size). Breadth index (5) = ((95% size) - (5% size) / 50% size).

[0204] (8) The polyvinyl alcohol in the continuous phase and the delivery agent containing the beneficial agent are calculated based on the total continuous phase water weight. The polyvinyl alcohol in the delivery particle containing the beneficial agent is based on the weight of the delivery particle core.

[0205] Determination of free polyvinyl alcohol content using capillary gel permeation chromatography-quadrupole transit time mass spectrometry

[0206] The method is based on measuring the ion intensity of specific fragment ions generated in an electrospray quadrupole time-of-flight mass spectrometer operated at elevated collision energy (CE). Specifically, polyvinyl alcohol polymer molecules can be fragmented at CE 70V to generate unique marker ions, such as m / z 131. The ion intensity is related to the polyvinyl alcohol concentration in the PMC slurry sample solution.

[0207] Experimental conditions :

[0208] Calibration solution preparation A 5% polyvinyl alcohol stock solution was first diluted with deionized water (Millipore) to obtain a 0.05% solution and then further 2-fold serial dilutions were performed to cover the concentration range from 0.00078% to 0.05%.

[0209] Sample solution preparation Each of the delivery particle slurry solutions containing the benefit agent was first diluted 5 or 10 times with water and then filtered by passing them through a 0.45 um PVDF membrane filter (PALL Gelman Lab).

[0210] Capillary Gel Permeation Chromatography-Mass Spectrometry ("GPC") Both calibration standard solutions and sample solutions were analyzed by injecting 5ul into a GPC system connected to an electrospray quadrupole time-of-flight mass spectrometer (QTOF, Waters, Beverly, MA) with four 1mm id x 150mm TSKGel G5000 or G6000 columns (Tosoh Bioscience, Japan) in series, 25ul / min isoproportional flow and 30min run time. The GPC buffer used was 5mM ammonium acetate containing 10% acetonitrile. For mass spectrometry, the first quadrupole was operated in broadband RF mode only, so all ions passed through the quadrupole, split at CE 70V in the second quadrupole, and analyzed by a TOF mass analyzer. The mass range scanned was 50Da to 3000Da.

[0211] Data acquisition, processing and analysis The QTOF mass spectrometer uses MassLynx (Waters) for data acquisition and data processing. The peak intensity of the main polyvinyl alcohol fragment ion m / z 131 was measured and averaged from two repeated CapGPC-QTOF runs. The polyvinyl alcohol concentration percentage in each sample was calculated based on the polyvinyl alcohol standard calibration curve. Good linear coverage was obtained under the current measurement conditions.

[0212] Calculate the bound polyvinyl alcohol content by using the following formula:

[0213] % bound polyvinyl alcohol = % total polyvinyl alcohol added to the slurry - % free polyvinyl alcohol

[0214] (9) Determination of degree of hydrolysis of polyvinyl alcohol

[0215] The degree of hydrolysis, defined as percent hydrolysis, refers to the mole % hydrolysis of the polyvinyl alcohol determined as follows: This measurement is a measure of the number of acetate groups replaced by hydroxyl groups during alcoholysis.

[0216] The degree of hydrolysis of polyvinyl alcohol is determined using reflux in a strong base to hydrolyze the remaining acetate groups and then post titration with hydrochloric acid according to the general principles outlined in established methods such as the USP monograph for polyvinyl alcohol (USP39-NF34, pp. 5448-5449). Those skilled in the art will know to appropriately select sample size, container volume, and volumes and concentrations of reagents for the range of degree of hydrolysis being measured.

[0217] (10) Determination of viscosity of polyvinyl alcohol

[0218] Viscosity is measured using a Brookfield LV series viscometer or equivalent and is measured to be 4.00% + / - 0.05% solids.

[0219] a. Prepare 4.00% + / - 0.05% polyvinyl alcohol solid solution .

[0220] Weigh the 500 mL beaker and stirrer. Record the weight. Add 16.00 + / - 0.01 grams of the polyvinyl alcohol sample to the beaker. Add approximately 350 mL to 375 mL of deionized water to the beaker and stir the solution. Place the beaker in a hot water bath with a covered plate. Stir at medium speed for 45 minutes to 1 hour, or until the polyvinyl alcohol is completely dissolved. Turn off the stirrer. Cool the beaker to approximately 20°C.

[0221] Calculate the final weight of the beaker as follows:

[0222] Final weight = (weight of empty beaker and stirrer) + (% solids as decimal x 400)

[0223] Example: Weight of empty beaker and stirrer = 125.0 g

[0224] Solids % of polyvinyl alcohol (sample) = 97.50% or 0.9750 (as a decimal)

[0225] Final weight = 125.0 + (0.9750 x 400) = 515.0 g

[0226] The top load balance was zeroed and the beaker of polyvinyl alcohol solution was placed on it with the propeller. Deionized water was added to bring the weight to the calculated final weight of 515.0 grams.

[0227] The solids content of the sample must be 4.00 + 0.05% to measure viscosity.

[0228] b. Measuring viscosity

[0229] Dispense a sample of 4% polyvinyl alcohol solution into the chamber of the viscometer, insert the spindle and attach it to the viscometer. Sample adapter (SSA) with chamber SC4-13RPY, Ultralow adapter. Spindle is SC4-18 and 00. Allow the sample to achieve equilibrium at a temperature of 20°C. Start the viscometer and record the steady state viscosity value.

[0230] Viscosities are reported to the nearest 0.01 cP for <13 cP and to the nearest 0.1 cP for 13 cP to 100 cP; viscosities over 100 cP are reported to the nearest 1 cP.

[0231] If the calculated solution solids content is 4.00 ± 0.05%, no correction is required for the measured viscosity. Otherwise, use the following formula to correct the measured viscosity for solution solids deviation.

[0232]

[0233] Corrected viscosity = 2.718282 (logarithm of corrected viscosity)

[0234] (11) Number average molecular weight of polyvinyl alcohol

[0235] The weight % of polyvinyl alcohol in aqueous solution was prepared and the sample was injected into the GPC instrument:

[0236] Connecting a Malvern Viscotek GPCmax VE 2001 sample module to a Malvern Viscotek model 305 TDA (Triple Detector Array)

[0237] Instrument settings during analysis:

[0238] Solvent: Water

[0239] Column setting: SOLDEX SB804+802.5

[0240] Flow rate: 0.750mL / min

[0241] Injection volume: 100 μl

[0242] Detector temperature: 30°C

[0243] Results are reported in Daltons (Da).

[0244] (12) Degree of polymerization of polyvinyl alcohol

[0245] The degree of polymerization is determined from the molecular weight data of the number average molecular weight test. Using the output from the GPC instrument, the molecular weight n The degree of polymerization was calculated from the GPC value

[0246]

[0247] Example

[0248] Although specific embodiments of the present invention have been illustrated and described, it will be apparent to those skilled in the art that many other changes and modifications may be made without departing from the spirit and scope of the present invention. Therefore, it is intended that all such changes and modifications within the scope of the present invention be covered in the appended claims.

[0249] Example 1 :

[0250] The first oil phase is composed of 37.5 g of fragrance oil, and the fragrance oil contains:

[0251] a) from about 3% to about 20% of a fragrance raw material selected from the group consisting of fragrance raw materials 85 to 88, 100, 108 of Table 1 and mixtures thereof;

[0252] b) from about 2% to about 35% of a fragrance raw material selected from the group consisting of fragrance raw materials 62 to 84, 114, 115 of Table 1 and mixtures thereof;

[0253] c) from about 2% to about 35% of a fragrance raw material selected from the group consisting of fragrance raw materials 1 to 61, 101, 102, 104, 109, 113 of Table 1 and mixtures thereof;

[0254] d) from about 0% to about 10% of a fragrance raw material selected from the group consisting of fragrance raw materials 99, 106, 111, 112 of Table 1 and mixtures thereof;

[0255] e) from about 0% to about 10% of a fragrance raw material selected from the group consisting of fragrance raw materials 89 to 94, 107, 110 of Table 1, and mixtures thereof; and

[0256] f) from about 0% to about 0.5% of a fragrance raw material selected from the group consisting of fragrance raw materials 95 to 98, 103, 105 of Table 1 and mixtures thereof.

[0257] 0.2 g of tert-butylaminoethyl methacrylate and 0.2 g of beta-hydroxyethyl acrylate were mixed for about 1 hour, and then 18 g of CN975 (Sartomer, Exter, PA) was added. The solution was allowed to mix until needed later in the process.

[0258] A second oil phase consisting of 65 g of fragrance oil, 84 g of isopropyl myristate, 1 g of 2,2'-azobis(2-methylbutyronitrile) and 0.8 g of 4,4'-azobis[4-cyanovaleric acid] was added to a jacketed steel reactor. The reactor was maintained at 35°C and the oil solution was mixed at 500 rpm with a 2" flat blade mixer. A nitrogen blanket was applied to the reactor at a flow rate of 300 cc / min. The solution was heated to 70°C in 45 minutes and maintained at 70°C for 45 minutes, then cooled to 50°C in 75 minutes. At 50°C, the first oil phase was added and the combined oils were mixed at 50°C for an additional 10 minutes.

[0259] An aqueous phase containing 85 g Celvol 540 polyvinyl alcohol (Sekisui Specialty Chemicals, Dallas, TX) at 5% solids, 268 g water, 1.2 g 4,4'-azobis[4-cyanovaleric acid], and 1.1 g 21.5% NaOH was prepared and mixed until the 4,4'-azobis[4-cyanovaleric acid] was dissolved. The pH of the aqueous phase for the batch was 4.90.

[0260] Once the oil phase temperature dropped to 50°C, mixing was stopped and the water phase was added to the mixed oil. High shear agitation was applied to prepare an emulsion with the desired size characteristics (1900 rpm for 60 minutes).

[0261] The temperature was raised to 75° C. over 30 minutes, maintained at 75° C. for 4 hours, raised to 95° C. over 30 minutes, and maintained at 95° C. for 6 hours. The batch was allowed to cool to room temperature.

[0262] The benefit agent containing delivery particles had a volume weighted median particle size of 20 microns.

[0263] From a total of 1.2% polyvinyl alcohol added to the batch, the content of free polyvinyl alcohol measured in the aqueous phase was 0.44%.

[0264] Example 2

[0265] Example 2 was prepared similarly to Example 1, except that the amount of water in the aqueous phase was increased to 340 grams. The aqueous phase pH was 4.84. After the batch was complete, the batch was reheated to 85°C and mixed to evaporate 72 grams of water from the batch. The volume weighted median particle size of the delivery particles containing the beneficial agent was 19.8 microns.

[0266] From a total of 1.2% polyvinyl alcohol added to the batch, the content of free polyvinyl alcohol measured in the aqueous phase was 0.44%.

[0267] Example 3

[0268] Example 3 was prepared similarly to Example 1, except that the amount of water in the aqueous phase was reduced to 188 grams. The aqueous phase pH was 4.84. After the batch was completed, 80 grams of water was added back to the batch. The volume weighted median particle size of the delivery particles containing the beneficial agent was 19.8 microns.

[0269] From a total of 1.2% polyvinyl alcohol added to the batch, the content of free polyvinyl alcohol measured in the aqueous phase was 0.47%.

[0270] Example 4

[0271] Example 4 was prepared similarly to Example 1, except the amount of Celvol 540 polyvinyl alcohol was increased to 127 grams. The pH of the aqueous phase was 4.84. The volume weighted median particle size of the delivery particles containing the benefit agent was 19.8 microns.

[0272] From a total of 1.6% polyvinyl alcohol added to the batch, the content of free polyvinyl alcohol measured in the aqueous phase was 0.87%.

[0273] Example 5

[0274] Example 5 was prepared similarly to Example 1, except the amount of Celvol 540 polyvinyl alcohol was reduced to 56 grams. The pH of the aqueous phase was 4.84. The volume weighted median particle size of the delivery particles containing the benefit agent was 19.8 microns.

[0275] From a total of 0.86% polyvinyl alcohol added to the batch, the free polyvinyl alcohol content measured in the aqueous phase was 0.26%.

[0276] Example 6 :

[0277] A first oil phase consisting of 200 g of fragrance oil, 1.2 g of tert-butylaminoethyl methacrylate, and 1.2 g of beta-hydroxyethyl acrylate was mixed for about 1 hour before 99 g of CN975 (Sartomer, Exter, PA) was added. The solution was allowed to mix until needed later in the process.

[0278] A second oil phase consisting of 360 g of fragrance oil, 460 g of isopropyl myristate, 5.5 g of 2,2'-azobis(2-methylbutyronitrile) and 4.4 g of 4,4'-azobis[4-cyanovaleric acid] was added to a jacketed steel reactor. The reactor was maintained at 35°C and the oil solution was mixed at 500 rpm with a 2" flat blade mixer. A nitrogen blanket was applied to the reactor at a flow rate of 300 cc / min. The solution was heated to 70°C in 45 minutes and maintained at 70°C for 45 minutes, then cooled to 50°C in 75 minutes. At 50°C, the first oil phase was added and the combined oils were mixed at 50°C for an additional 10 minutes.

[0279] An aqueous phase containing 233 g Celvol 540 polyvinyl alcohol (Sekisui Specialty Chemicals, Dallas, TX) at 5% solids, 1224 g water, 6.6 g 4,4'-azobis[4-cyanovaleric acid], and 6 g 21.5% NaOH was prepared and mixed until the 4,4'-azobis[4-cyanovaleric acid] was dissolved. The pH of the aqueous phase for the batch was 4.90.

[0280] Once the oil phase temperature dropped to 50°C, mixing was stopped and the water phase was added to the mixed oil. High shear agitation was applied to prepare an emulsion with desired size characteristics (3100 rpm for 60 minutes).

[0281] The temperature was raised to 75°C in 30 minutes, held at 75°C for 4 hours, raised to 95°C in 30 minutes, and held at 95°C for 6 hours. The batch was allowed to cool to room temperature. The delivery particles containing the benefit agent had a volume weighted median particle size of 18 microns, and 0.8% total polyvinyl alcohol was added to the batch.

[0282] Example 7

[0283] Example 7 was prepared similarly to Example 6, except that the amount of Celvol 540 polyvinyl alcohol (Sekisui Specialty Chemicals, Dallas, TX) was increased to 350 g and the amount of water was reduced to 1100 g. The pH of the aqueous phase was 4.8. The volume weighted median particle size of the delivery particles containing the beneficial agent was 18 microns, and 1.2% total polyvinyl alcohol was added to the batch.

[0284] Example 8

[0285] Example 8 was prepared similarly to Example 6, except that the amount of Celvol 540 polyvinyl alcohol (Sekisui Specialty Chemicals, Dallas, TX) was increased to 525 g and the amount of water was reduced to 933 g. The pH of the aqueous phase was 4.8. The volume weighted median particle size of the delivery particles containing the beneficial agent was 19 microns, and 1.8% total polyvinyl alcohol was added to the batch.

[0286] The delivery particle slurries containing the beneficial agent described in Examples 6 to 8 were refined with water and centrifuged to remove some of the unbound ("free") polyvinyl alcohol. The slurries were diluted with water to 28% to 30% solids and heated to 70°C. Each batch was fed through a continuous centrifuge at a bowl speed of 50 Hz (about 9000 rpm) and a target split ratio of 60% light (accept stream) and 40% heavy (reject stream). The light stream was collected and the heavy stream was discarded. The dilution, heating and centrifugation process was repeated a second time using half of the light stream collected from each batch.

[0287] The slurries from Examples 6 to 8 were analyzed for free and bound polyvinyl alcohol content for unrefined, once refined and twice refined samples. The results are summarized in the following table

[0288]

[0289]

[0290] Example 9

[0291] Unrefined slurry samples with 0.8%, 1.2% and 1.8% total polyvinyl alcohol were prepared in a similar manner to Examples 6 to 8. Magnesium chloride and xanthan gum (Novaxxan—ADM) were mixed into the slurry at room temperature to structure the solids and stored in 4 oz glass containers at 30° C. and 40° C. Phase separation was measured after one month.

[0292]

[0293] Example 10

[0294] Unrefined slurry samples with 1.2% total polyvinyl alcohol and unrefined and refined samples with 1.8% total polyvinyl alcohol were prepared in a similar manner to Examples 6 and 8 and stored in 4 oz glass containers at 30° C. and 40° C. Phase separation was measured after one month.

[0295] Total polyvinyl alcohol% Xanthan gum% MgCl2% Separation % at 30C Separation % at 40C 0.8 0.2 0 0.0 0.0 1.8 0.2 0 15.2 22.5 1.8* 0.12 0 0.0 1.7

[0296] *1x refined sample

[0297] Non-limiting examples of product formulations comprising delivery particles comprising beneficial agents disclosed in this specification are summarized in the following table.

[0298] Embodiment 11

[0299] Free-Flowing Solid Granular Laundry Detergent Composition Examples

[0300]

[0301]

[0302] Example 12: Heavy Duty Liquid Laundry Detergent Composition

[0303]

[0304]

[0305] *Not exceeding 12% water by weight of the total cleaning and / or treatment composition

[0306] (1) Optional.

[0307] (2) The benefit agent-containing delivery particles of the present invention, comprising a core containing fragrance and / or silicone, include Examples 1 to 8 and mixtures thereof.

[0308] Example 13: Unit Dose Composition

[0309]

[0310]

[0311] (2) A beneficial agent-containing delivery particle according to the present invention, comprising a core containing a fragrance, comprising Examples 1 to 8

[0312] and mixtures thereof.

[0313] Embodiment 14

[0314] Examples of free flowing particulate products comprising benefit agent containing delivery particles according to the invention. The following table also illustrates combinations further comprising free perfume and benefit agent containing delivery particles, or combinations of these with combinations of the above mentioned malodour reducing materials and / or compositions.

[0315]

[0316]

[0317] Embodiment 15

[0318] Examples of liquid fabric softening products comprising benefit agent containing delivery particles according to the invention. The following table also illustrates combinations further comprising free perfume and benefit agent containing delivery particles, or combinations of these with combinations of the above mentioned malodour reducing materials and / or compositions.

[0319]

[0320] Materials and Descriptions for Composition Examples

[0321] LAS is supplied by Stepan (Northfield, Illinois, USA) or Huntsman Corp. with C 9 -C 15 Average aliphatic carbon chain length linear alkylbenzene sulfonate (HLAS in acid form).

[0322] C 12-14 Dimethylhydroxyethylammonium chloride, supplied by Clariant GmbH (Germany)

[0323] AE3S is a C supplied by Stepan (Northfield, Illinois, USA). 12-15 Alkyl ethoxy (3) sulfate

[0324] AE7 is C 12-15 Alcohol ethoxylate, having an average degree of ethoxylation of 7, supplied by Huntsman (Salt Lake City, Utah, USA)

[0325] AES is C supplied by Shell Chemicals 10-18 Alkyl ethoxy sulfate.

[0326] AE9 is C 12-13 Alcohol ethoxylate, having an average degree of ethoxylation of 9, supplied by Huntsman (Salt Lake City, Utah, USA)

[0327] HSAS or HC1617HSAS is a mid-branched primary alkyl sulfate with an average carbon chain length of about 16 to 17

[0328] Sodium tripolyphosphate was supplied by Rhodia (Paris, France)

[0329] Zeolite A was supplied by Industrial Zeolite (UK) Ltd (Grays, Essex, UK)

[0330] 1.6R silicate supplied by Koma (Nestemica, Czech Republic)

[0331] Sodium carbonate was supplied by Solvay (Houston, Texas, USA)

[0332] Polyacrylate with a molecular weight of 4500 was supplied by BASF (Ludwigshafen, Germany).

[0333] Carboxymethyl cellulose was supplied by CP Kelco (Arnhem, Netherlands). V

[0334] Suitable chelating agents are, for example, diethylenetetraaminepentaacetic acid (DTPA) supplied by Dow Chemical (Midland, Michigan, USA), or hydroxyethanediphosphonate (HEDP) supplied by Solutia (St Louis, Missouri, USA Bagsvaerd, Denmark).

[0335] Celluclean TM , and All are products of Novozymes (Bagsvaerd, Denmark).

[0336] Proteases can be supplied by Genencor International (Palo Alto, California, USA) (e.g., Purafect ) or supplied by Novozymes (Bagsvaerd, Denmark) (e.g. ).

[0337] Sodium percarbonate, supplied by Solvay (Houston, Texas, USA)

[0338] Sodium perborate was supplied by Degussa (Hanau, Germany)

[0339] NOBS is sodium nonanoyloxybenzene sulfonate supplied by Future Fuels (Batesville, USA)

[0340] TAED is tetraacetylethylenediamine, which is sold under the trade name Supplied by Clariant GmbH (Sulzbach, Germany)

[0341] S-ACMC is carboxymethyl cellulose conjugated to CI Reactive Blue 19, sold under the product name AZO-CM-CELLULOSE (product code S-ACMC) by Megazyme (Wicklow, Ireland).

[0342] The detergent was supplied by Rhodia (Paris, France). PF

[0343] The acrylic acid / maleic acid copolymer had a molecular weight of 70,000 and a ratio of acrylate to maleate of 70:30 and was supplied by BASF (Ludwigshafen, Germany)

[0344] Ethylenediamine-N,N'-disuccinic acid sodium salt, (S,S) isomer (EDDS) was supplied by Octel (Ellesmere Port, UK)

[0345] Hydroxyethane diphosphonate (HEDP) was supplied by Dow Corning (Midland, Michigan, USA) Suds suppressor agglomerates were supplied by Dow Corning (Midland, Michigan, USA)

[0346] HSAS is a mesobranched alkyl sulfate, as disclosed in US 6,020,303 and US 6,060,443.

[0347] C 12-14 Dimethylamine oxide was supplied by Procter & Gamble Chemicals (Cincinnati, USA)

[0348] The random graft copolymer is a polyethylene oxide copolymer grafted with polyvinyl acetate, which has a polyethylene oxide main chain and a plurality of polyvinyl acetate side chains. The molecular weight of the polyethylene oxide main chain is about 6000, and the weight ratio of polyethylene oxide to polyvinyl acetate is about 40:60, and there is no more than 1 grafting point per 50 ethylene oxide units.

[0349] Ethoxylated polyethyleneimine is polyethyleneimine (MW=600) having 20 ethoxylate groups per -NH.

[0350] The cationic cellulose polymer was LK400, LR400 and / or JR30M from Amerchol Corporation (Edgewater NJ).

[0351] Note: All enzyme contents are expressed as % enzyme starting material.

[0352] The dimensions and values ​​disclosed herein are not to be understood as being strictly limited to the exact numerical values ​​cited. Instead, unless otherwise indicated, each such dimension is intended to represent the stated value and a functionally equivalent range around that value. For example, a dimension disclosed as "40 mm" is intended to mean "about 40 mm".

[0353] The relevant parts of all documents cited in the specific embodiments of the present invention are incorporated herein by reference; the reference to any document should not be interpreted as an admission that it is the prior art related to the present invention. When 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 the term in this document shall be obeyed.

[0354] Although specific embodiments of the present invention have been illustrated and described, it will be apparent to those skilled in the art that many other changes and modifications may be made without departing from the spirit and scope of the present invention. Therefore, it is intended that all such changes and modifications within the scope of the present invention be covered in the appended claims.

Claims

1. A composition comprising a consumer product adjunct material and a slurry, wherein the composition comprises 0.3% to 4% of the slurry based on the total consumer product weight, the slurry comprising a delivery particle comprising a benefit agent and a continuous phase comprising water, the delivery particle comprising a core and a shell encapsulating the core, the slurry comprising: a) 0.1% to 0.5% of free polyvinyl alcohol in the continuous phase, based on the total continuous phase water weight, and 0.6% to 0.9% of polyvinyl alcohol in the delivery particle containing the benefit agent, based on the total benefit agent-containing delivery particle core weight; the free polyvinyl alcohol based on the total water weight of the continuous phase and the polyvinyl alcohol based on the total benefit agent-containing delivery particle core weight having at least one of the following characteristics: (i) a degree of hydrolysis of 55% to 99%, preferably 75% to 95%, more preferably 85% to 90%, most preferably 87% to 89%; and (ii) a viscosity in a 4% aqueous solution at 20° C. of 40 to 120 mPa.s, preferably 40 to 90 mPa.s, more preferably 45 to 72 mPa.s, more preferably 45 to 60 mPa.s, most preferably 45 to 55 mPa.s; (iii) a degree of polymerization of 1,500 to 2,500, preferably 1,600 to 2,200, more preferably 1,600 to 1,900, most preferably 1,600 to 1,800; (iv) a number average molecular weight of 65,000 Da to 110,000 Da, preferably 70,000 Da to 101,000 Da, more preferably 70,000 Da to 90,000 Da, most preferably 70,000 Da to 80,000 Da; b) 30% to 55% of said benefit agent-containing delivery particles based on the total slurry weight, said benefit agent-containing delivery particles preferably having a volume weighted average particle size of 0.5 microns to 100 microns, said benefit agent-containing delivery particles having a shell comprising said polyvinyl alcohol and one or more polyacrylate polymers, said core comprising greater than 10% of a partitioning modifier based on the total core weight, said partitioning modifier comprising a material selected from the group consisting of propan-2-yl myristate, vegetable oils, modified vegetable oils, and mixtures thereof; c) a monovalent, divalent or trivalent inorganic salt, wherein the slurry comprises 0% to 0.6% of the salt based on the total slurry weight; d) polysaccharides and / or hydrocolloids, wherein the slurry comprises 0% to 0.4% of the polysaccharides and / or hydrocolloids based on the total slurry weight; The composition is a consumer product, The slurry has been refined to remove free polyvinyl alcohol.

2. The composition of claim 1, wherein the partitioning modifier comprises propan-2-yl myristate.

3. A composition according to any one of the preceding claims, wherein the shell comprises a polyacrylate, preferably the shell comprises 50% to 100%, more preferably 70% to 100%, most preferably 80% to 100% of the polyacrylate polymer, preferably the polyacrylate comprises a polyacrylate cross-linked polymer.

4. A composition according to any of the preceding claims, wherein the shell comprises a polymer derived from a material comprising one or more multifunctional acrylate moieties; preferably the multifunctional acrylate moieties are selected from trifunctional acrylates, tetrafunctional acrylates, pentafunctional acrylates, hexafunctional acrylates, heptafunctional acrylates and mixtures thereof; and optionally a polyacrylate comprising moieties selected from the group consisting of amine acrylate moieties, methacrylate moieties, carboxylic acid acrylate moieties, carboxylic acid methacrylate moieties and combinations thereof.

5. A composition according to any of the preceding claims, wherein the shell comprises a polymer derived from a material comprising one or more multifunctional acrylate and / or methacrylate moieties, preferably in a ratio of 999:1 to 6:4, more preferably 99:1 to 8:1, most preferably 99:1 to 8.5:1 of material comprising one or more multifunctional acrylate moieties to material comprising one or more methacrylate moieties; preferably the multifunctional acrylate moieties are selected from trifunctional acrylates, tetrafunctional acrylates, pentafunctional acrylates, hexafunctional acrylates, heptafunctional acrylates and mixtures thereof; and optionally a polyacrylate comprising a moiety selected from the group consisting of an amine acrylate moiety, a methacrylate moiety, a carboxylic acid acrylate moiety, a carboxylic acid methacrylate moiety and combinations thereof.

6. A composition according to any preceding claim, wherein the benefit agent-containing delivery particles have a volume weighted average particle size of from 5 microns to 45 microns, more preferably from 8 microns to 25 microns, or alternatively from 25 microns to 60 microns, more preferably from 25 microns to 60 microns, the composition comprising from 0.1% to 35%, preferably from 1% to 35%, more preferably from 2% to 25%, more preferably from 3% to 20%, more preferably from 5% to 15%, most preferably from 8% to 12% fabric softener active or 3% to 12%, preferably 4% to 10%, more preferably 5% to 8% of a fabric softener active, preferably the fabric softener active is selected from quaternary ammonium compounds, amines, fatty acid esters, sucrose esters, silicones, dispersible polyolefins, clays, polysaccharides, fatty acids, softening oils, polymer latexes and mixtures thereof, more preferably the fabric softener active is selected from bis-(2-hydroxypropyl)-dimethyl ammonium methyl sulfate fatty acid ester, 1,2-di(acyloxy)-3-trimethylpropyl ammonium chloride, N,N-bis(stearoyloxyethyl)-N,N- Dimethylammonium chloride, N,N-bis(tallowyloxyethyl) N,N-dimethylammonium chloride, N,N-bis(stearoyloxyethyl) N-(2-hydroxyethyl)-N-methyl ammonium methyl sulfate, N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethyl ammonium methyl sulfate, N,N-bis-(tallowyl-2-hydroxypropyl)-N,N-dimethyl ammonium methyl sulfate, N,N-bis-(palmitoyl-2-hydroxypropyl)-N,N-dimethyl ammonium methyl sulfate, N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethyl ammonium chloride ammonium chloride, 1,2-di(stearoyloxy)3-trimethylpropyl ammonium chloride, canola dimethyl ammonium chloride, di(hard) tallow dimethyl ammonium chloride, canola dimethyl ammonium methyl sulfate, 1-methyl-1-stearoylaminoethyl-2-stearoyl imidazoline methyl sulfate, 1-tallowylamidoethyl-2-tallowyl imidazoline, dipalmitoyl hydroxyethyl ammonium methyl sulfate and mixtures thereof, and mixtures thereof, most preferably the fabric softener active is selected from N,N-bis(stearoyloxyethyl) N,N-dimethyl ammonium chloride; N,N-bis(tallowoyloxyethyl)N,N-dimethylammonium chloride; N,N-bis(stearoyloxyethyl)N-(2-hydroxyethyl)N-methylammonium methyl sulfate; 1,2-di(stearoyloxy)3-trimethylpropylammonium chloride; N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethylammonium methyl sulfate, N,N-bis-(tallowoyl-2-hydroxypropyl)-N,N-dimethylammonium methyl sulfate, N,N-bis-(palmitoyl-2-hydroxypropyl)-N,N-dimethylammonium methyl sulfate, N,N-bis-(stearoyl-2-hydroxypropyl)-N,N-dimethylammonium chloride, and mixtures thereof.

7. A composition according to any one of the preceding claims, comprising from 5% to 95%, preferably from 10% to 95%, more preferably from 20% to 95%, more preferably from 30% to 80%, most preferably from 50% to 70% water, and from 0.1% to 25%, preferably from 0.5% to 20% of a surfactant, preferably selected from a nonionic surfactant or an anionic surfactant and mixtures thereof, based on the total composition weight.

8. A composition according to any one of claims 1 to 7, wherein the composition comprises 5% to 20%, 8% to 15%, 9% to 13% water based on the total composition weight, the composition being encapsulated in a film, preferably the film comprises polyvinyl alcohol.

9. A composition according to any one of claims 1 to 7, comprising a liquid and / or gel and a film encapsulating the liquid and / or gel, optionally the liquid or gel comprising suspended solids.

10. A composition according to any one of claims 1 to 7 wherein the benefit agent-containing delivery particles have a volume weighted average particle size of from 2 microns to 40 microns, preferably from 8 microns to 25 microns, the composition comprising from 5% to 95% free water and from 0.5% to 25% builder based on total composition weight.

11. A composition according to any one of the preceding claims, comprising, based on the total composition weight, a material selected from the group consisting of: hueing dyes, structurants, additional perfume delivery systems, and mixtures thereof; preferably, a) The structuring agent comprises a material selected from the following: polysaccharides, preferably the polysaccharides are selected from modified cellulose, chitosan, plant cellulose, bacterial cellulose, coated bacterial cellulose, preferably the bacterial cellulose comprises xanthan gum; castor oil, hydrogenated castor oil, modified protein, inorganic salt, quaternized polymer material, imidazole; non-ionic polymer with a pKa of less than 6.0, polyurethane, non-polymeric crystalline hydroxyl functionalized material, polymer structuring agent, diamido gelling agent, homopolymer of the following formula (Ia): in: R1 is selected from hydrogen or methyl; R2 is selected from hydrogen or C1-C4 alkyl; R3 is selected from C1-C4 alkylene; R4, R5 and R6 are each independently selected from hydrogen or C1-C4 alkyl; X is selected from -O- or -NH-, preferably -O-; and Y is selected from Cl, Br, I, hydrogen sulfate or methyl sulfate; and mixtures thereof; b) the hueing dye is selected from small molecule dyes, polymeric dyes, dye-clay conjugates, and organic and inorganic pigments, preferably the hueing dye comprises a chromophore selected from one or more of the following: acridine, anthraquinone, azine, azo, azulene, benzodifuran and benzodifuranone, carotenoids, coumarins, cyanines, diazahemicyanines, diphenylmethanes, formazans, hemicyanines, indigos, methanes, naphthimides, naphthoquinones, nitro and nitroso groups, oxazines, phthalocyanines, pyrazoles, stilbenes, styryls, triarylmethanes, triphenylmethanes, xanthenes, and mixtures thereof; and c) The additional perfume delivery comprises a material selected from the group consisting of: delivery particles containing a second benefit agent, a polymer-assisted delivery system; a molecule-assisted delivery system; a fiber-assisted delivery system; a cyclodextrin delivery system; a starch encapsulation formulation; and / or an inorganic carrier delivery system.

12. A composition according to any of the preceding claims, wherein the beneficial agent-containing delivery particle is prepared by a free radical polymerization process comprising the steps of combining 50% to 100% of a hexafunctional urethane acrylate and / or a pentafunctional urethane acrylate, 0% to 25%, preferably 0.01% to 25%, of a methacrylate containing an amino moiety, and 0% to 25%, preferably 0.01% to 25%, of an acrylate containing a carboxyl moiety, based on the total free radical polymerization process acrylate monomer reactants, with the proviso that the sum of the hexafunctional urethane acrylate and / or pentafunctional urethane acrylate, the methacrylate containing an amino moiety, and the acrylate containing a carboxyl moiety is 100%, preferably the methacrylate containing an amino moiety comprises tert-butylaminoethyl methacrylate and the acrylate containing a carboxyl moiety comprises beta-carboxyethyl acrylate.

13. A composition according to any one of the preceding claims, comprising a deposition aid, preferably the deposition aid coats the outer surface of the shell, preferably the deposition aid comprises a material selected from the group consisting of poly(meth)acrylates, poly(ethylene-maleic anhydride), polyamines, waxes, polyvinylpyrrolidone, polyvinylpyrrolidone copolymers, polyvinylpyrrolidone-ethyl acrylate, polyvinylpyrrolidone-vinyl acrylate, polyvinylpyrrolidone methacrylate, polyvinylpyrrolidone / vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxanes, polyvinyl (propylene maleic anhydride), maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, styrene-butadiene latex, gelatin, gum arabic, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, hydroxyethyl cellulose, other modified celluloses, sodium alginate, chitosan, casein, pectin, modified starch, polyvinyl acetal, polyvinyl butyral, polyvinyl methyl ether / maleic anhydride, polyvinyl pyrrolidone and its copolymers, poly(vinyl pyrrolidone / methacrylamidopropyltrimethylammonium chloride), polyvinyl pyrrolidone / vinyl acetate, polyvinyl pyrrolidone / dimethylaminoethyl methacrylate, polyvinyl amine, polyvinyl formamide, polyallylamine, and copolymers of polyvinyl amine, polyvinyl formamide, polyallylamine, and mixtures thereof, more preferably the deposition aid comprises a material selected from the group consisting of poly(meth)acrylate, poly(ethylene-maleic anhydride), polyamine, polyvinyl pyrrolidone, polyvinyl pyrrolidone-ethyl acrylate, polyvinyl pyrrolidone-vinyl acrylate, polyvinyl pyrrolidone methacrylate, polyvinyl pyrrolidone / vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxane The invention also includes but is not limited to alkanes, poly(propylene maleic anhydride), maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, chitosan, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, hydroxyethyl cellulose, polyvinyl methyl ether / maleic anhydride, poly(vinyl pyrrolidone / methacrylamidopropyltrimethylammonium chloride), polyvinyl pyrrolidone / vinyl acetate, polyvinyl pyrrolidone / dimethylaminoethyl methacrylate, polyvinylamine, polyvinylformamide, polyallylamine, and copolymers of polyvinylamine, polyvinylformamide, polyallylamine, and mixtures thereof.

14. A method of making a composition according to any one of the preceding claims, the method comprising combining a consumer product adjunct ingredient and a slurry comprising a delivery particle comprising a benefit agent and a continuous phase comprising water, the delivery particle comprising a core and a shell encapsulating the core, the slurry being prepared by a method comprising: emulsifying the combination of a) and b) to form an emulsion, wherein a) is a first composition formed by combining a first oil and a second oil, wherein the first oil comprises a core comprising a fragrance, an initiator and a partition modifier, preferably the partition modifier comprises a material selected from the group consisting of vegetable oil, modified vegetable oil, propan-2-yl myristate and mixtures thereof, preferably the modified vegetable oil is esterified and / or brominated, preferably the vegetable oil comprises castor oil and / or soybean oil; preferably the partition modifier comprises propan-2-yl myristate; The second oil comprises (i) oil-soluble aminoalkyl acrylate and / or methacrylate monomers; (ii) hydroxyalkyl acrylate monomers and / or oligomers; (iii) a material selected from the group consisting of multifunctional acrylate monomers, multifunctional methacrylate monomers, multifunctional methacrylate oligomers, multifunctional acrylate oligomers, and mixtures thereof; (iv) spices; and wherein b) is a second composition, the second composition comprising the continuous phase, a pH adjuster, an emulsifier, preferably an anionic emulsifier, preferably the emulsifier comprises polyvinyl alcohol and optionally an initiator; and, heating the emulsion in one or more heating steps to form a shell encapsulating the core, thereby forming a delivery particle containing a benefit agent, the delivery particle comprising the shell encapsulating the core and dispersed in the continuous phase, The method further comprises refining the slurry to remove free polyvinyl alcohol.

15. A method for treating and / or cleaning a site, the method comprising a) optionally washing, rinsing and / or drying the area; b) contacting the site with a consumable product according to any one of claims 1 to 13 and / or prepared by the method of claim 14; and c) optionally washing, rinsing and / or drying the site, wherein the drying step comprises active drying and / or passive drying.

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