阅读说明：本技术 包含含有有益剂的递送颗粒的组合物 (Compositions comprising benefit agent-containing delivery particles ) 是由 J·斯梅兹 C·E·A·朱斯 P·韦斯特拉特 冯林胜 F·S·查卡尔 R·S·博布诺克 于 2019-12-05 设计创作，主要内容包括：公开了包括有益剂递送颗粒的组合物,所述颗粒具有核和包封所述核的壳,所述壳包括某些基于丙烯酸酯的聚合物。公开了制作和使用这类组合物的方法。(Disclosed are compositions comprising benefit agent delivery particles having a core and a shell encapsulating the core, the shell comprising certain acrylate-based polymers. Methods of making and using such compositions are disclosed.)

1. A composition comprising a benefit agent delivery particle having a volume weighted median particle size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, said benefit agent delivery particle comprising a core and a shell, said shell encapsulating said core,

a) the shell comprises a poly (meth) acrylate polymer comprising the reaction product of at least one monomer or oligomer thereof,

i. the monomer comprises a structure according to formula I:

wherein R is¹Is selected from C₁To C₈An alkyl group, a carboxyl group,

wherein R is²Is hydrogen or a methyl group,

wherein n is an integer of 1 to 3,

wherein a is a ring structure selected from:

or

b. The core comprises a benefit agent;

the core also comprises from about 0% to about 80%, preferably from 0% to 50%, more preferably from about 0% to about 30%, most preferably from about 0% to about 20%, based on total core weight, of a partitioning modifier.

2. The composition of claim 1, wherein the poly (meth) acrylate polymer of the shell comprises the reaction product of at least three monomers, or oligomers thereof, the monomers comprising a first monomer, a second monomer, and a third monomer,

a. the first monomer comprises the structure according to formula I,

b. the second monomer comprises a basic (meth) acrylate monomer,

c. the third monomer comprises an acidic (meth) acrylate monomer.

3. A composition comprising a benefit agent delivery particle having a volume weighted median particle size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, said benefit agent delivery particle comprising a core and a shell, said shell encapsulating said core,

a) the shell comprises a poly (meth) acrylate polymer comprising the reaction product of at least a first monomer, a second monomer, and a third monomer, or oligomers thereof,

i. the first monomer comprises a structure according to formula I,

wherein R is¹Is selected from C₁To C₈An alkyl group, a carboxyl group,

wherein R is²Is hydrogen or a methyl group,

wherein n is an integer of 1 to 3,

wherein a is a ring structure selected from:

or

With the proviso that when a of formula I is structure II, the shell is free of polymers formed from monofunctional ethylenically unsaturated monomers;

the second monomer comprises a basic (meth) acrylate monomer,

the third monomer comprises an acidic (meth) acrylate monomer; and is

b) The core comprises a benefit agent.

4. The composition of claim 3, wherein the core further comprises from about 0% to about 80%, preferably from 0% to 50%, more preferably from about 0% to about 30%, most preferably from about 0% to about 20%, based on total core weight, of a partitioning modifier.

5. The composition of any one of the preceding claims, wherein the median volume weighted particle size is from 25 microns to 60 microns.

6. The composition according to any preceding claim, wherein the benefit agent delivery particle has a one week leakage percentage of the core of less than 25 wt% measured at 35 ℃.

7. The composition of any of the preceding claims, wherein the basic (meth) acrylate monomer or oligomer thereof comprises less than 1 weight percent of the particles, and the acidic (meth) acrylate monomer or oligomer thereof comprises less than 1 weight percent of the particles.

8. A composition according to any one of the preceding claims, wherein in formula I, n-3, R¹Is selected from C₂To C₅Alkyl, and A is

9. The composition according to any one of the preceding claims, wherein the monomer according to formula I is selected from:

or oligomers of any such monomer.

10. The composition of any of the preceding claims, wherein the partitioning modifier comprises a compound selected from the group consisting of vegetable oils, modified vegetable oils, C₄-C₂₄Mono-, di-and triesters of fatty acids, propane-2-yltetradecanoate, isopropyl myristate, dodecylbenzophenone, lauryl alcohol laurate, methyl behenate, methyl laurate, methyl palmitate, methyl stearate and mixtures thereof, preferably isopropyl myristate.

11. The composition according to any of the preceding claims, wherein the benefit agent delivery particle comprises from about 0.5% to about 40%, more preferably from 0.8% to 5%, based on total benefit agent delivery particle weight, of an emulsifier, preferably the emulsifier is selected from the group consisting of polyvinyl alcohol, carboxylated or partially hydrolyzed polyvinyl alcohol, methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, methylhydroxypropyl cellulose, salts or esters of stearic acid, lecithin, organic sulfonic acids, 2-acrylamido-2-alkylsulfonic acids, styrenesulfonic acid, polyvinylpyrrolidone, copolymers of N-vinylpyrrolidone, polyacrylic acid, polymethacrylic acid, copolymers of acrylic acid and methacrylic acid, and water soluble surfactant polymers that reduce the surface tension of water, more preferably the emulsifier comprises polyvinyl alcohol, preferably, the polyvinyl alcohol has at least one of the following properties:

(i) a degree of hydrolysis of from about 55% to about 99%, preferably from about 75% to about 95%, more preferably from about 85% to about 90%, most preferably from about 87% to about 89%; and/or

(ii) A viscosity of from about 40cps to about 80cps, preferably from about 45cps to about 72cps, more preferably from about 45cps to about 60cps, most preferably from 45cps to 55cps in a 4% aqueous solution at 20 ℃; and/or

(iii) A degree of polymerization of from about 1500 to about 2500, preferably from about 1600 to about 2200, more preferably from about 1600 to about 1900, most preferably from about 1600 to about 1800; and/or

(iv) A weight average molecular weight of from about 130,000 to about 204,000 daltons, preferably from about 146,000 to about 186,000, more preferably from about 146,000 to about 160,000, most preferably from about 146,000 to about 155,000; and/or

(v) A number average molecular weight of from about 65,000 to about 110,000 daltons, preferably from about 70,000 to about 101,000, more preferably from about 70,000 to about 90,000, most preferably from about 70,000 to about 80,000.

12. The composition of any of the preceding claims, wherein any of the first, second, and third monomers is an oligomer or prepolymer of the monomer.

13. The composition of any preceding claim, wherein the basic (meth) acrylate monomer or oligomer comprises an aminoalkyl acrylate or aminoalkyl methacrylate, wherein the alkyl moiety is one to twelve carbons.

14. The composition of any preceding claim, wherein the basic (meth) acrylate monomer is selected from the group consisting of: ethylaminoethyl acrylate, ethylaminoethyl methacrylate, aminoethyl acrylate, aminoethyl methacrylate, t-butylaminoethyl acrylate, t-butylaminoethyl methacrylate, diethylamino acrylate, diethylamino methacrylate, diethylaminoethyl acrylate, diethylaminoethyl methacrylate, dimethylaminoethyl acrylate and dimethylaminoethyl methacrylate.

15. The composition of any preceding claim, wherein the acidic (meth) acrylate monomer or oligomer comprises a carboxyl-substituted acrylate or methacrylate monomer.

16. A composition according to any preceding claim, wherein the acidic (meth) acrylate monomer comprises a carboxyalkyl acrylate, a carboxyalkyl methacrylate, a carboxyaryl acrylate, a carboxyaryl methacrylate, or a (meth) acryloxyphenyl alkyl carboxylic acid, wherein the alkyl moiety is one to twelve carbons.

17. The composition of any preceding claim, wherein the acidic (meth) acrylate monomer is selected from the group consisting of: 2-carboxyethyl acrylate, 2-carboxyethyl methacrylate, 2-carboxypropyl acrylate, 2-carboxypropyl methacrylate, carboxyoctyl acrylate, carboxyoctyl methacrylate, 2-acryloxybenzoic acid, 3-acryloxybenzoic acid, 4-acryloxybenzoic acid, 2-methacryloxybenzoic acid, 3-methacryloxybenzoic acid, and 4-methacryloxybenzoic acid, 4-acryloxyphenylacetic acid, and 4-methacryloxyphenylacetic acid.

18. A composition according to any preceding claim, wherein the benefit agent delivery particle comprises a coating on the shell, preferably the coating comprises a coating material selected from the group consisting of: poly (meth) acrylates, polyethylene-maleic anhydride, polyamines, waxes, polyvinylpyrrolidone copolymers, polyvinylpyrrolidone-ethyl acrylate, polyvinylpyrrolidone-vinyl acrylate, polyvinylpyrrolidone-methacrylic acid ester, polyvinylpyrrolidone/vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxanes, polypropylene maleic anhydride, maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, styrene-butadiene latex, gelatin, gum arabic, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, other modified celluloses, sodium alginate, chitosan, casein, pectin, modified starch, polyvinyl acetal, polyvinyl butyral, polyvinyl methyl ether/maleic anhydride, polyvinylpyrrolidone and its copolymers, poly (vinylpyrrolidone/methacrylamidopropyltrimethylammonium chloride), polyvinylpyrrolidone/vinyl acetate, polyvinylpyrrolidone/dimethylaminoethyl methacrylate, polyvinylamine, polyvinylformamide, polyallylamine, copolymers of polyvinylamine, polyvinylformamide, polyallylamine, and mixtures thereof.

19. The composition of any of the preceding claims, additionally comprising an adjunct material, wherein said adjunct material 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%, by weight of the total composition, of a conditioning active, preferably said conditioning active is selected from the group consisting of: quaternary ammonium compounds, amines, fatty esters, sucrose esters, silicones, dispersible polyolefins, clays, polysaccharides, fatty acids, softening oils, polymer latexes, and mixtures thereof, wherein the composition is different from a consumer product.

20. The composition of any one of the preceding claims, wherein the adjunct material comprises from about 1% to about 70%, or from about 2% to about 60%, or from about 5% to about 50%, by weight of the composition, of a surfactant system.

21. The composition according to any of the preceding claims, wherein the benefit agent is selected from the group consisting of: perfume raw materials, lubricants, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, skin cooling agents, vitamins, sunscreens, antioxidants, glycerin, catalysts, bleach particles, silica particles, odor reducing agents, odor control materials, chelating agents, antistatic agents, softeners, insect and moth repellents, agricultural actives, colorants, antioxidants, chelating agents, thickeners, drape and form control agents, smoothing agents, wrinkle control agents, detergents, disinfectants, bacteria control agents, mildew control agents, antiviral agents, desiccants, antifouling agents, detergents, fabric fresheners and preservatives, chlorine bleach odor control agents, color fixatives, dye transfer inhibitors, color maintenance agents, optical brighteners, color reduction/restoration agents, anti-fading agents, whiteness enhancers, anti-abrasion agents, abrasion resistance agents, fabric integrity agents, anti-wear agents, anti-pilling agents, anti-foaming agents, UV protection agents, solar fade inhibitors, anti-allergic agents, enzymes, water repellents, fabric comfort agents, anti-shrinkage agents, anti-stretch agents, elastic recovery agents, skin care agents, synthetic or natural actives, antibacterial actives, antiperspirant actives, cationic polymers, dyes, and mixtures thereof; preferably a perfume raw material, and wherein the composition is different from a consumer product.

22. The composition of claim 17, 18 or 19, wherein the auxiliary material is selected from the group consisting of: surfactants, conditioning actives, deposition aids, rheology modifiers or structurants, bleach systems, stabilizers, synergists, chelants, dye transfer inhibitors, dispersants, enzymes, enzyme stabilizers, catalytic metal complexes, polymeric dispersants, desliming and soil/anti-redeposition agents, brighteners, suds suppressors, silicones, toners, aesthetic dyes, additional perfumes and perfume delivery systems, structure elasticizing agents, carriers, hydrotropes, processing aids, structurants, anti-agglomeration agents, coatings, formaldehyde scavengers, pigments, and mixtures thereof; preferably at least a structuring agent, a deposition aid or a mixture thereof.

23. The composition of any of the preceding claims, further comprising a structurant, a deposition aid, or a mixture thereof.

24. The composition according to any preceding claim, wherein at least 75% of the benefit agent delivery particles have a median volume weighted particle size of from about 6 microns to about 50 microns, preferably from about 10 microns to about 50 microns.

25. The composition of any one of the preceding claims, wherein at least 75% of the encapsulates have a diameter of greater than 15 microns, preferably greater than 20 microns, more preferably greater than 25 microns.

26. The composition according to any one of the preceding claims, wherein at least 75% of the benefit agent delivery particles have a particle wall thickness of from about 10nm to about 350nm, from about 20nm to about 200nm, or from 25nm to about 180 nm.

27. The composition according to any of the preceding claims, having a particle size distribution in 20s^-1And a viscosity of 1 to 1500 cps (1-1500 mPas), 100 to 1000 cps (100-.

28. The composition according to any preceding claim, comprising from about 0.001 wt% to about 25 wt% of the benefit agent delivery particle, based on the total mass.

29. The composition of any one of the preceding claims, wherein the composition is in the form of a liquid composition, a granular composition, or a slurry.

Technical Field

The present application relates to benefit agent-containing delivery particles, compositions comprising such particles, and methods of making and using such particles and compositions.

Background

Benefit agents such as perfumes, silicones, waxes, perfumes, vitamins and fabric softeners are expensive and/or generally less effective when employed at high levels in consumer products such as personal care compositions, cleaning compositions and fabric care compositions. Therefore, there is a need to maximize the effectiveness of such benefit agents. One way to achieve this goal is to improve the delivery efficiency of such benefit agents. Unfortunately, it is difficult to improve the efficiency of delivery of benefit agents because such agents may be lost due to the physical or chemical characteristics of the agent, or such agents may be incompatible with other compositional components or the site being treated. To improve this delivery efficiency, benefit agents have been encapsulated.

Encapsulated benefit agents, such as perfume microcapsules having a shell comprising polyacrylate, are expected to provide fragrance benefits throughout all consumer contacts. The particles are core-shell and core-shell particles may comprise microcapsules, capsules and encapsulates (encapsulates), and for the purposes of this application microcapsules, capsules and encapsulates are synonymous. For example, it is desirable to treat fabrics with such capsules, which provide a fragrance benefit to the treated fabrics while the fabrics are still wet by such treatment and after such fabrics have dried. Unfortunately, the encapsulated benefit agent may leak out of the benefit agent over time via diffusion in the finished product. Thus, the fabric odor is reduced. If such leakage is minimized (e.g., by increasing the strength of the enclosure shell), the odor of the treated fabric may also be diminished because there is not enough fragrance released from the capsules. This problem is particularly evident in fabric treatment products comprising such encapsulates, such as liquid fabric enhancers, liquid laundry detergents, unit dose laundry detergents and particulate/powdered laundry detergents. Accordingly, what is needed is an encapsulate that exhibits reduced leakage of benefit agents, yet provides desirable odor characteristics to wet and dry fabrics, particularly enhanced pre-rub (prerub) benefits and post-rub (post rub) benefits.

One solution to providing an encapsulate with the desired shell strength/benefit agent release characteristics is to select monomers and oligomers with appropriate molecular weights and functional groups. However, even when suitable monomers and oligomers are selected, partitioning modifiers are often employed in the prior art. Partitioning modifiers are taught to suitably dissolve such monomers and oligomers so that the desired shell wall can be obtained. Unfortunately, the partitioning modifier occupies space in the final encapsulant that could otherwise be filled with the benefit active. In short, the partitioning modifier reduces the payload of the encapsulate. Surprisingly, applicants have recognized that the partitioning modifier also avoids plasticizing the enclosure walls of the encapsulant with a benefit agent such as perfume. Thus, applicants use this knowledge to select monomers and oligomers that do not require much or no solubility modification and are resistant to plasticization of the benefit agent actives when formed into shell walls.

Accordingly, applicants herein disclose an encapsulate having an unexpectedly high payload yet exhibiting reduced benefit agent leakage and providing desirable odor characteristics, particularly enhanced pre-rub and post-rub benefits, to wet and dry fabrics, and a method of making the same. Applicants disclose an encapsulate composition comprising a reduced amount of a partitioning modifier, or wherein the partitioning modifier is completely eliminated.

Disclosure of Invention

The present invention relates to benefit agent containing delivery particles comprising a core material and a wall material encapsulating the core material. The invention also relates to compositions comprising the particles, and methods of making and using such particles and compositions.

Detailed Description

The present invention relates to encapsulates comprising a specific polymer in the wall of the encapsulate. The encapsulate can include a partition modifier in the encapsulate core. Without wishing to be bound by theory, it is believed that making such selections in the design of the encapsulant results in an encapsulant that provides improved performance characteristics.

In prior art systems, leakage tends to increase with increasing particle size. One unexpected aspect of the presently described particles is that the unique combination of monomers, oligomers and/or prepolymers results in core-shell microcapsules as benefit agent particles wherein as the median particle size of the benefit agent particles increases, the one week leakage is reduced compared to systems without the present combination.

In the art, leakage generally increases as the size of benefit agent particles, such as core-shell encapsulates and microcapsules, increases. Core-shell benefit agent delivery particles of larger size are disclosed which unexpectedly achieve lower leakage relative to particles of comparable size in the art.

The present invention relates to particles that make it possible to achieve an unexpectedly high payload. The ratio of core to shell, measured on the weight of the benefit agent particles, may be higher than 2:1, or even 3:1, preferably 4:1, or even at least 10:1, or even at least 20: 1. The core as a percentage of benefit agent particles may be at least 50%, or even 60 to 98%, or in some aspects at least 75%, or even at least 80%, on a weight percentage basis. It is expected that the present invention relates to high payloads, such as 60 to 98% of the particles.

For example, the resulting particles of the present invention with partitioning modifier are relatively large particles, yet have lower leakage and higher strength than particles in the art.

The encapsulates of the invention and related methods are described in more detail below.

Definition of

As used herein, "consumer product" means baby care, beauty care, fabric and home care, feminine care, health care, snack and/or beverage products or appliances that are intended to be used or consumed in the form in which they are sold, rather than for subsequent commercial manufacture or modification. Such products include, but are not limited to: fine fragrances (e.g., perfumes, colognes, after-shave lotions, before-shave lotions, facial lotions, supplements, and other fragrance/fragrance containing compositions applied directly to the skin), diapers, bibs, wet wipes; products or methods for and/or relating to treating hair (human, dog and/or cat) including bleaching, coloring, dyeing, conditioning, shampooing, styling; deodorants and antiperspirants; personal cleansing; a cosmetic; skin care, including application of creams, lotions, and other topically applied products for consumer use; and shaving products; products and/or methods for and/or with respect to treating fabrics, hard surfaces, and any other surfaces in the fabric and home care arts, comprising: air care, automotive care, dishwashing, fabric conditioning (including softening), laundry washing, wash and rinse additive and/or care, hard surface cleaning and/or treatment, and other cleaning for consumer or institutional use; products and/or methods relating to toilet, facial, handkerchief and/or paper towels; tampons, sanitary napkins; products and/or methods relating to oral care, including toothpaste, tooth gel, tooth rinsing, denture adhesive, tooth whitening; over-the-counter health care including cough and cold medications, analgesics; prescription drugs, pet health and nutrition, and water purification; processed foods intended primarily for consumption between meals or as a appetizer (non-limiting examples include potato chips, tortilla chips, popcorn, crackers, corn chips, cereal bars, vegetable chips or crisps, snack combinations, party plates, cereal chips, snack biscuits, cheese snacks, pigskin, corn snacks, pellet snacks, extruded snacks, and bread chips); and coffee.

As used herein, "different from a consumer product" means a raw material that is used neat or in the manufacture of a consumer and/or industrial product. Such raw materials include dry capsules, microcapsules, slurry of microcapsules, microcapsule aggregates, microcapsule powders, microcapsule dispersions, microcapsule coatings and binding materials with microcapsules. End-uses may include, but are not limited to, coatings for substrates, slurries for delivering benefit agents, such as slurries for industrial uses such as delivering perfumes/fragrances, lubricants, or other active agents.

As used herein, unless otherwise indicated, the term "cleaning composition" includes general-purpose or "heavy-duty" detergents, especially cleaning detergents, in granular or powder form; general detergents in the form of liquids, gels or pastes, especially the so-called heavy-duty liquid type; a liquid fine fabric soil release agent; manual dishwashing agents or light-duty dishwashing agents, especially those of the high-foam type; machine dishwashing agents, including various tablet, granular, liquid, and rinse aid types used in both household and institutional applications; liquid cleaning and disinfecting agents, including antibacterial hand-wash types, cleaning sticks, mouthwashes, denture cleaners, dentifrice, car or carpet shampoos, bathroom cleaners; shampoo and hair conditioner; body washes and foam baths and metal cleaners; and cleaning aids such as bleach additives and "stain-stick" or pretreatment types, substrate-laden products such as dryer-added sheets, dry and wet wipes and pads, nonwoven substrates, and sponges; as well as sprays and mists.

As used herein, unless otherwise indicated, the term "fabric care composition" includes fabric softening compositions, fabric enhancing compositions, fabric freshening compositions, and combinations thereof.

The term "benefit agent containing delivery particle" as used herein encompasses microcapsules comprising perfume microcapsules.

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

As used herein, reference to the term "(meth) acrylate" or "(meth) acrylic" is understood to refer to both acrylate and methacrylate versions of the specified monomer, oligomer, and/or prepolymer. For example, "(meth) acrylate" indicates that both allyl methacrylate and allyl acrylate are possible, and similarly reference to "(alkyl (meth) acrylate" indicates that both alkyl acrylate and alkyl methacrylate are possible, and similarly poly (meth) acrylate indicates that both polyacrylate and polymethacrylate are possible. Poly (meth) acrylate materials are intended to encompass a broad spectrum of polymeric materials including, for example: polyester poly (meth) acrylates, urethane and polyurethane poly (meth) acrylates (especially prepared by reaction of hydroxyalkyl (meth) acrylates with polyisocyanates or urethane polyisocyanates), methyl cyanoacrylates, ethyl cyanoacrylates, diethylene glycol di (meth) acrylates, trimethylolpropane tri (meth) acrylates, ethylene glycol di (meth) acrylates, allyl (meth) acrylates, glycidyl (meth) acrylates, (meth) acrylate functional silicones, di-, tri-and tetraethylene glycol di (meth) acrylates, dipropylene glycol di (meth) acrylates, polyethylene glycol di (meth) acrylates, di (pentylene glycol) di (meth) acrylates, ethylene di (meth) acrylates, neopentyl glycol di (meth) acrylates, trimethylolpropane tri (meth) acrylate, ethoxylated bisphenol a di (meth) acrylate, diglycerol di (meth) acrylate, tetraethyleneglycol dichloroacrylate, 1, 3-butanediol di (meth) acrylate, neopentyl di (meth) acrylate, trimethylolpropane tri (meth) acrylate, polyethylene glycol di (meth) acrylate and dipropylene glycol di (meth) acrylate, and various polyfunctional (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, chlorobenzyl (meth) acrylate, aminoalkyl (meth) acrylate, various alkyl (meth) acrylates and glycidyl (meth) acrylate. Mixtures of (meth) acrylates or their derivatives may also be used, 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.

As used herein, "encapsulate," "particle," and "capsule" are used interchangeably unless otherwise indicated.

For the purposes of the present invention, propane-2-yltetradecanoate is not considered a perfume raw material when calculating a perfume composition/formulation. Thus, the amount of propane-2-yltetradecanoate present is not used to make such calculations.

As used herein, articles including "a" and "an" when used in a claim are understood to mean one or more of what is claimed or described.

The terms "comprising," "including," and "containing," as used herein, are intended to be non-limiting.

The test methods disclosed in the test methods section of this application should be used to determine the corresponding values for the parameters of applicants' invention.

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, e.g., residual solvents or by-products, which may be present in commercially available sources of such components or compositions.

All percentages and ratios are by weight unless otherwise indicated. All percentages and ratios are calculated based on the total composition, unless otherwise indicated.

It is to be understood that each maximum numerical limitation given throughout this specification includes every lower numerical limitation, as if such lower numerical limitations were expressly written herein. Every minimum numerical limitation given throughout this specification will include every higher numerical limitation, as if such higher numerical limitations were expressly written herein. Every numerical range given throughout this specification will include every narrower numerical range that falls within such broader numerical range, as if such narrower numerical ranges were all expressly written herein.

Composition comprising a metal oxide and a metal oxide

The present invention relates to compositions comprising benefit agent delivery particles and adjunct materials, such as consumer product adjunct materials.

The composition may be a consumer product. The consumer product may be used as an infant care, beauty care, fabric and home care, feminine care, health care, snack and/or beverage product or appliance. The composition may be a cosmetic care composition, a fabric and a household care composition, or a combination thereof.

The composition may be a cosmetic care composition such as a hair care product (including shampoos and/or conditioners), a skin care product (including creams, lotions or other topically applied products for consumer use), a shaving care product (including shaving water, lather, or pre-or post-shave care), a personal cleansing product (including liquid body washes, liquid hand soaps and/or bar soaps), a deodorant and/or antiperspirant, or mixtures thereof.

The composition may be a fabric treatment composition, such as a laundry detergent composition (including heavy duty laundry detergents), a fabric conditioning composition (including fabric softening and/or enhancing compositions), a wash and rinse additive, a fabric pretreatment composition, a fabric freshening composition, or mixtures thereof.

The composition may be a household care composition, such as air care, automotive care, dishwashing, hard surface cleaning and/or treatment, and other cleaning for consumer or institutional use.

The composition may be in any suitable form. For example, the composition may be in the form of a liquid composition, a granular composition, a single-compartment pouch, a multi-compartment pouch, a dissolvable tablet, a lozenge or bead, a fibrous article, a tablet, a bar, a flake, a dry tablet, or a mixture thereof. The composition may be selected from a liquid, a solid, or a combination thereof.

The composition may be in the form of a liquid. The liquid composition may comprise from about 30%, or from about 40%, or from about 50% to about 99%, or to about 95%, or to about 90%, or to about 75%, or to about 70%, or to about 60%, by weight of the composition, of water. The liquid composition may be a liquid laundry detergent, a liquid fabric conditioner, a liquid detergent, a shampoo, a conditioner, or a mixture thereof.

The composition may be in the form of a solid. The solid composition may be a powder or a granular composition. Such compositions may be agglomerated or spray dried. Such compositions may include a plurality of particles or granules, at least some of which include different compositions. The composition may be a powder or granular cleaning composition, which may include a bleaching agent.

The composition may be in the form of a unitized dose article such as a tablet, sachet, tablet or fibrous article. Such pouches typically include a water-soluble film, such as a polyvinyl alcohol water-soluble film, which at least partially encapsulates the composition. Suitable films are available from MonoSol, LLC (Indiana, usa). The composition may be enclosed in a single or multi-compartment pouch. The multi-compartment pouch may have at least two, at least three, or at least four compartments. A multi-compartment pouch may comprise side-by-side and/or overlapping compartments. The composition contained in the pouch or compartment thereof may be a liquid, a solid (such as a powder), or a combination thereof. The bagged composition may have a relatively small amount of water, for example less than about 20%, or less than about 15%, or less than about 12%, or less than about 10%, or less than about 8% water by weight of the detergent composition.

The composition may have a composition of 20s^-1And a viscosity of 1 to 1500 cps (1-1500 mPas), 100 to 1000 cps (100-.

Other components and/or features of the composition, such as the benefit agent delivery particles and consumer product adjunct materials, are discussed in more detail below.

Benefit agent delivery particles

The compositions and products of the present invention comprise benefit agent delivery particles. The particles typically comprise a core and a shell, wherein the shell encapsulates the core. As described in more detail below, the core may include a benefit agent and optionally a partitioning modifier, and the shell may include certain polymers. Optionally, the composition additionally comprises auxiliary materials, such as consumer product auxiliary materials.

The benefit agent delivery particle may have a median volume weighted particle size of from about 0.5 microns to about 100 microns, or even 10 to 100 microns, preferably from about 1 micron to about 60 microns, or even 10 microns to 50 microns, or even 20 microns to 45 microns, or even 20 microns to 60 microns.

a. Shell

The particles of the present invention comprise a shell. The shell may comprise certain polymers, which may be the reaction product of certain monomers.

For example, the shell of the particles described herein can comprise a poly (meth) acrylate polymer comprising the reaction product of at least one monomer or oligomer thereof. The monomer comprises a structure according to formula I:

wherein R is¹Is selected from C₁To C₈，R²Is hydrogen or methyl, wherein n is an integer from 1 to 3, and a is a ring structure selected from:

the core comprises a benefit agent. Additionally, the benefit agent delivery particle comprises from about 0% to about 80%, preferably from 0% to 50%, more preferably from about 0% to about 30%, most preferably 20% or less of the partitioning modifier based on the total core weight.

In the present specification and claims, for ease of reference, the term "monomer" as used herein is to be understood to mean a monomer, and includes oligomers or monomers, and prepolymers formed from the specified monomers.

In another aspect, the present invention teaches a composition comprising benefit agent delivery particles having a volume weighted median particle size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, said benefit agent delivery particles comprising a core and a shell, said shell encapsulating said core, with the proviso that when a of formula I is structure II, said shell is free of polymers formed from monofunctional ethylenically unsaturated monomers. The shell comprises a poly (meth) acrylate polymer comprising the reaction product of at least three monomers or oligomers thereof. The first monomer comprises a structure according to formula I:

wherein R is¹Is selected from C₁To C₈Alkyl radical, R²Is hydrogen or methyl, n is an integer from 1 to 3, and a is a ring structure selected from:

the second monomer and/or oligomer or prepolymer thereof may comprise a basic (meth) acrylate monomer, and the third monomer may comprise an acidic (meth) acrylate monomer.

The basic (meth) acrylate monomer and/or oligomer or prepolymer thereof may comprise one or more of the following: amine-modified methacrylates, amine-modified acrylates, monomers such as mono-or diacrylate amines, mono-or dimethacrylate amines, amine-modified polyether acrylates, amine-modified polyether methacrylates, aminoalkyl acrylates, or aminoalkyl methacrylates. The amine may be a primary, secondary or tertiary amine. Preferably, the alkyl moiety of the basic (meth) acrylate monomer is C1 to C12.

Amine (meth) acrylates suitable for use in the particles of the present invention may include aminoalkyl acrylates or methacrylates, including for example but not limited to ethyl aminoethyl acrylate, ethyl aminoethyl methacrylate, aminoethyl acrylate, aminoethyl methacrylate, t-butyl urethane acrylate, t-butyl urethane methacrylate, t-butyl aminoethyl acrylate, t-butyl aminoethyl methacrylate, diethyl urethane acrylate, diethyl urethane methacrylate, diethylaminoethyl acrylate, diethylaminoethyl methacrylate, dimethylaminoethyl acrylate, and dimethylaminoethyl methacrylate. Preferably, the amine (meth) acrylate is aminoethyl acrylate or methacrylate, or t-butylaminoethyl methacrylate.

The acidic (meth) acrylate may comprise, for example, one or more of a carboxy-substituted acrylate or methacrylate, preferably a carboxy-substituted alkyl acrylate or a carboxy-substituted alkyl methacrylate, such as a carboxyalkyl acrylate, a carboxyalkyl methacrylate, a carboxyaryl acrylate, a carboxyaryl methacrylate, and preferably C1 to C10 with the alkyl moiety being straight or branched. The carboxyl moiety may be bound to any carbon, preferably the terminal carbon, of the C1 to C10 alkyl moieties. It is also possible to use carboxyl-substituted aryl acrylates or methacrylates or even (meth) acryloxyphenylalkyl carboxylic acids. The alkyl moiety of the (meth) acryloyloxyphenylalkylcarboxylic acid may be C1 to C10.

Carboxyl esters of (meth) acrylic acid suitable for use in the particles of the present invention may include 2-carboxyethyl acrylate, 2-carboxyethyl methacrylate, 2-carboxypropyl acrylate, 2-carboxypropyl methacrylate, carboxyoctyl acrylate, carboxyoctyl methacrylate. The carboxyl-substituted aryl acrylate or the carboxyl-substituted aryl methacrylate may include 2-acryloyloxybenzoic acid, 3-acryloyloxybenzoic acid, 4-acryloyloxybenzoic acid, 2-methacryloyloxybenzoic acid, 3-methacryloyloxybenzoic acid, and 4-methacryloyloxybenzoic acid. The (meth) acryloyloxyphenylalkyl carboxylic acid may include, for example, but is not limited to, 4-acryloyloxyphenylacetic acid or 4-methacryloyloxyphenylacetic acid.

The basic (meth) acrylate monomer or oligomer may be present at less than 1% by weight of the benefit agent delivery particle. The acidic (meth) acrylate monomer or oligomer may be present at less than 1% by weight of the benefit agent delivery particle.

The composition benefit agent delivery particle may have a percent one week leakage of the core of less than 25 wt% measured at 35 ℃.

In one useful embodiment, in formula I, n ═ 3, R¹Is selected from C₂To C₅Alkyl, and a is:

the monomer according to formula I may be selected from:

optionally, in the composition of the present invention, any of the first, second, and third monomers may be an oligomer, a monomer, or a prepolymer.

The benefit agent delivery particle may comprise from about 0.5% to about 40%, more preferably from 0.8% to 5% emulsifier by weight of the total benefit agent delivery particle. Preferably the emulsifier is selected from the group consisting of: polyvinyl alcohol, carboxylated or partially hydrolyzed polyvinyl alcohol, methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, methylhydroxypropyl cellulose, salts or esters of stearic acid, lecithin, organic sulfonic acids, 2-acrylamido-2-alkylsulfonic acids, styrenesulfonic acids, polyvinylpyrrolidone, copolymers of N-vinylpyrrolidone, polyacrylic acid, polymethacrylic acid, copolymers of acrylic acid and methacrylic acid, and water-soluble surfactant polymers which lower the surface tension of water. The emulsifier preferably comprises polyvinyl alcohol, and the polyvinyl alcohol preferably has a degree of hydrolysis of from about 55% to about 99%, preferably from about 75% to about 95%, more preferably from about 85% to about 90%, and most preferably from about 87% to about 89%. The polyvinyl alcohol may have a viscosity of from about 40cps to about 80cps, preferably from about 45cps to about 72cps, more preferably from about 45cps to about 60cps, and most preferably from 45cps to 55cps in a 4% aqueous solution at 20 ℃. The polyvinyl alcohol may have a degree of polymerization of from about 1500 to about 2500, preferably from about 1600 to about 2200, more preferably from about 1600 to about 1900, and most preferably from about 1600 to about 1800. The polyvinyl alcohol may have a weight average molecular weight of from about 130,000 to about 204,000 daltons, preferably from about 146,000 to about 186,000, more preferably from about 146,000 to about 160,000, and most preferably from about 146,000 to about 155,000; and/or have a number average molecular weight of from about 65,000 to about 110,000 daltons, preferably from about 70,000 to about 101,000, more preferably from about 70,000 to about 90,000, and most preferably from about 70,000 to about 80,000.

The benefit agent delivery particles of the present invention may comprise a coating. The shell may comprise a coating, for example the coating may be on the outer surface of the shell. The particles may be manufactured and subsequently coated with a coating material. The coating may be used as a deposition aid. Non-limiting examples of coating materials include, but are not limited to, materials selected from the group consisting of: poly (meth) acrylates, polyethylene-maleic anhydride, polyamines, waxes, polyvinylpyrrolidone copolymers, polyvinylpyrrolidone-ethyl acrylate, polyvinylpyrrolidone-vinyl acrylate, polyvinylpyrrolidone-methacrylic acid ester, polyvinylpyrrolidone/vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxanes, polypropylene maleic anhydride, maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, styrene-butadiene latex, gelatin, gum arabic, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, other modified celluloses, sodium alginate, chitosan, casein, pectin, modified starch, polyvinyl acetal, polyvinyl butyral, polyvinyl methyl ether/maleic anhydride, polyvinylpyrrolidone and its copolymers, poly (vinylpyrrolidone/methacrylamidopropyltrimethylammonium chloride), polyvinylpyrrolidone/vinyl acetate, polyvinylpyrrolidone/dimethylaminoethyl methacrylate, polyvinylamine, polyvinylformamide, polyallylamine, and copolymers of polyvinylamine, polyvinylformamide and polyallylamine, and mixtures thereof. The coating material may be a cationic polymer.

b. Benefit agent

The particles of the present invention comprise a core comprising a benefit agent. Suitable benefit agents located in the core may include benefit agents that provide benefits to surfaces such as fabric or hair.

The benefit agent may be selected from the group consisting of: perfume raw materials, lubricants, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, skin cooling agents, vitamins, sunscreens, antioxidants, glycerin, catalysts, bleach particles, silica particles, odor reducing agents, odor control materials, chelating agents, antistatic agents, softeners, insect and moth repellents, agricultural actives, colorants, antioxidants, chelating agents, thickeners, drape and form control agents, smoothing agents, wrinkle control agents, detergents, disinfectants, bacteria control agents, mildew control agents, antiviral agents, desiccants, antifouling agents, detergents, fabric fresheners and preservatives, chlorine bleach odor control agents, color fixatives, dye transfer inhibitors, color maintenance agents, optical brighteners, color reduction/restoration agents, anti-fading agents, whiteness enhancers, anti-abrasion agents, abrasion resistance agents, fabric integrity agents, anti-wear agents, anti-pilling agents, anti-foaming agents, UV protection agents, solar fade inhibitors, anti-allergic agents, enzymes, water repellents, fabric comfort agents, anti-shrinkage agents, anti-stretch agents, elastic recovery agents, skin care agents, glycerin, synthetic or natural actives, antibacterial actives, antiperspirant actives, cationic polymers, dyes, and mixtures thereof.

The encapsulated benefit agent may comprise perfume raw materials. As used herein, the term "perfume raw material" (or "PRM") refers to a compound that has a molecular weight of at least about 100g/mol and can be used alone or in combination with other perfume raw materials to impart an odor, fragrance, flavor, or aroma. Typical PRMs include, inter alia, alcohols, ketones, aldehydes, esters, ethers, nitrites, and alkenes, such as terpenes. A list of common PRMs can be found in various reference sources, such as "Perfun and Flavor Chemicals", volumes I and II, Steffen Arctander Allwred pub. Co. (1994), and "Perfuns: Art, Science and Technology", Miller, P.M. and Lamparsky, D., Black Academic and Professional (1994).

PRMs can be characterized by their boiling point (b.p.) as measured at atmospheric pressure (760mm Hg) and an octanol/water partition coefficient (P) as determined according to the test method below, which can be described in terms of logP. Based on these characteristics, PRMs can be classified as quadrant I, quadrant II, quadrant III, or quadrant IV fragrances, as described in more detail below.

The perfume raw material may comprise a perfume raw material selected from the group consisting of: perfume raw materials having a boiling point (b.p.) of less than about 250 ℃ and a ClogP of less than about 3, perfume raw materials having a boiling point of greater than about 250 ℃ and a ClogP of greater than about 3, perfume raw materials having a boiling point of greater than about 250 ℃ and a ClogP of less than about 3, perfume raw materials having a boiling point of less than about 250 ℃ and a ClogP of greater than about 3, and mixtures thereof. Perfume raw materials having a boiling point b.p. below about 250 ℃ and a ClogP below about 3 are referred to as quadrant I perfume raw materials. Quadrant 1 perfume raw materials are preferably limited to less than 30% of the perfume composition. Perfume raw materials having a b.p. above about 250 ℃ and a ClogP above about 3 are referred to as quadrant IV perfume raw materials, perfume raw materials having a b.p. above about 250 ℃ and a ClogP below about 3 are referred to as quadrant II perfume raw materials, and perfume raw materials having a b.p. below about 250 ℃ and a ClogP above about 3 are referred to as quadrant III perfume raw materials. Suitable quadrant I, II, III and IV perfume raw materials are disclosed in us patent 6,869,923B 1.

c. Partition modifiers

The core of the particles of the present invention may comprise a partitioning modifier. In addition to the encapsulated benefit agent, the core may comprise from more than 0% to about 80%, preferably from more than 0% to about 50%, more preferably from more than 0% to about 30%, most preferably from more than 0% to about 20%, based on total core weight, of a partitioning modifier.

The partitioning modifier may comprise a material selected from the group consisting of: vegetable oil, modified vegetable oil, C₄-C₂₄Mono-, di-and triesters of fatty acids, propane-2-yltetradecanoate, isopropyl myristateEsters, lauryl benzophenone, lauryl laurate, methyl behenate, methyl laurate, methyl palmitate, methyl stearate, and mixtures thereof. The partitioning modifier may preferably comprise or consist of isopropyl myristate. The modified vegetable oil may be esterified and/or brominated. The modified vegetable oil may preferably comprise castor oil and/or soy bean oil. Patent application publication 20110268802, incorporated herein by reference, describes other partitioning modifiers that can be used in the benefit agent particles presently described.

Optionally, the encapsulate and/or the composition comprising the encapsulate may comprise (e.g., in addition to the polyvinyl alcohol disclosed above) an emulsifier, which may be used to form the encapsulate. Additional emulsifiers may include, for example, but are not limited to: water-soluble salts of alkyl sulfates, alkyl ether sulfates, alkyl isothionates, alkyl carboxylates, alkyl sulfosuccinates, alkyl succinamates, alkyl sulfates, alkyl derivatives such as sodium lauryl sulfate, alkyl sarcosinates, protein hydrolysates, acyl aspartates, alkyl or alkyl ether or alkylaryl ether phosphates, sodium lauryl sulfate, phospholipids or lecithins, or soaps, sodium, potassium or ammonium stearate, sodium, potassium or ammonium oleate, or sodium, potassium or ammonium palmitate, alkylaryl sulfonates, such as sodium dodecylbenzene sulfonate, sodium dialkyl sulfosuccinates, dioctyl sulfosuccinates, sodium dilauryl sulfosuccinates, sodium polystyrene sulfonates, olefin-maleic anhydride copolymers, such as isobutylene-maleic anhydride copolymers or ethylene-maleic anhydride copolymers, gum arabic, sodium alginate, carboxymethylcellulose, cellulose sulfates and pectins, polystyrene sulfonates, pectic acid, tragacanth, mandelic gum and agar-agar; semi-synthetic polymers such as carboxymethyl cellulose, sulfated methyl cellulose, carboxymethyl starch, phosphated starch, lignosulfonic acid; maleic anhydride copolymers (including their hydrolysis products), polyacrylic acid, polymethacrylic acid, acrylic acid-alkyl acrylate copolymers, such as acrylic acid-butyl acrylate copolymers, or crotonic acid homopolymers and copolymers, vinylbenzenesulfonic acid or 2-acrylamido-2-methylpropanesulfonic acid homopolymers and copolymers, and also partial amides or partial esters of such polymers and copolymers, carboxyl-modified polyvinyl alcohols, sulfonic acid-modified polyvinyl alcohols and phosphoric acid-modified polyvinyl alcohols, phosphorylated or sulfated tristyrylphenol ethoxylates. The amount of emulsifier can be selected anywhere from about 0.1 to about 40% by weight of all components, in one aspect 0.5 to about 10%, and in another aspect 0.5 to 5% by weight. In another aspect, the emulsifier is employed in 0.2 to about 10 weight percent based on the total formulation.

d. Method of making benefit agent delivery particles

The particles of the present invention can be made according to any known method using suitable starting materials. For example, the particles may be made by a process comprising heating an emulsion in one or more heating steps, the emulsion being produced by emulsifying a combination of:

a) a first composition formed by combining a first oil and a second oil, the first oil comprising a fragrance, an initiator, and a partitioning modifier; preferably the partitioning modifier comprises a material selected from the group consisting of a vegetable oil, a modified vegetable oil, which is esterified and/or brominated, a propane-2-yltetradecanoate, and mixtures thereof, preferably isopropyl myristate, preferably the vegetable oil comprises castor oil and/or soybean oil; preferably the partitioning modifier comprises propane-2-yltetradecanoate;

the second oil comprises:

(i) oil-soluble aminoalkyl acrylate and/or aminoalkyl methacrylate monomers,

(ii) a carboxyalkyl acrylate monomer and/or oligomer,

(iii) a material selected from the group consisting of a multifunctional acrylate monomer, a multifunctional methacrylate oligomer, a multifunctional acrylate oligomer, and mixtures thereof,

(iv) a fragrance; and

b) a second composition comprising water, a pH adjusting agent, an emulsifier, preferably an anionic emulsifier, preferably the emulsifier comprises polyvinyl alcohol and optionally an initiator.

In the method, the heating step comprises heating the emulsion for about 1 hour to about 20 hours, preferably about 2 hours to about 15 hours, more preferably about 4 hours to about 10 hours, most preferably about 5 to about 7 hours, sufficient to deliver about 500 joules/kg to about 5000 joules/kg to the emulsion, about 1000 joules/kg to about 4500 joules/kg to the emulsion, about 2900 joules/kg to about 4000 joules/kg to the emulsion.

Prior to the heating step, the emulsion has a median volume weighted particle size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, more preferably from about 10 microns to about 25 microns, or from about 0.5 microns to about 10 microns.

The weight ratio of the first composition to the second composition in the above process is from about 1:9 to about 1:1, preferably from about 3:7 to about 4: 6; and the ratio of the first oil to the second oil is from 99:1 to about 1:99, preferably from 9:1 to about 1:9, more preferably from 6:4 to about 8: 2.

A slurry can be made by combining benefit agent delivery particles made by the above process. One or more perfumes different from the one or more perfumes contained in the core of the benefit agent delivery particle may be applied externally to the core-shell benefit agent delivery particle.

Consumer product adjunct material

The compositions of the present invention, which may be consumer products, may comprise consumer product adjunct materials. The consumer product adjunct material can provide a benefit in the intended end use of the composition, or can be a processing and/or stabilizing aid.

Suitable consumer product adjunct materials can include: surfactants, conditioning actives, deposition aids, rheology modifiers or structurants, bleach systems, stabilizers, synergists, chelants, dye transfer inhibitors, dispersants, enzymes, and enzyme stabilizers, catalytic metal complexes, polymeric dispersants, desliming and soil/anti-redeposition agents, brighteners, suds suppressors, silicones, toners, aesthetic dyes, additional perfumes and perfume delivery systems, structure elasticizing agents, carriers, hydrotropes, processing aids, structurants, anti-agglomeration agents, coatings, formaldehyde scavengers, and/or pigments.

Depending on the intended form, formulation and/or end use, the compositions of the present invention may or may not contain one or more of the following auxiliary materials: bleach activators, surfactants, builders, chelating agents, dye transfer inhibiting agents, dispersants, enzymes, and enzyme stabilizers, catalytic metal complexes, polymeric dispersing agents, desliming and soil removal/anti-redeposition agents, brighteners, suds suppressors, dyes, additional perfumes and perfume delivery systems, structure elasticizing agents, fabric softeners, carriers, hydrotropes, processing aids, structurants, anti-agglomeration agents, coatings, formaldehyde scavengers and/or pigments. Benefit agents suitable for location in the core of a particle or microcapsule as described above may additionally or alternatively be suitable for inclusion as an adjunct material.

The exact nature of these additional components and the levels at which they are incorporated will depend on the physical form of the composition and the nature of the operation in which it is to be used. However, when one or more adjuncts are present, such one or more adjuncts may be present as detailed below. The following is a non-limiting list of suitable other adjuncts.

a. Surface active agent

The compositions of the present invention may comprise a surfactant. Surfactants can be used to provide, for example, cleaning benefits. The composition may comprise a surfactant system, which may contain one or more surfactants.

The compositions of the present invention may comprise from about 1% to about 70%, or from about 2% to about 60%, or from about 5% to about 50%, by weight of the composition, of the surfactant system. The liquid composition may comprise from about 5% to about 40%, by weight of the composition, of the surfactant system. A dense formulation comprising a dense liquid, gel, and/or composition suitable for unit dosage form may comprise from about 25% to about 70%, or from about 30% to about 50%, by weight of the composition, of a surfactant system.

The surfactant system may include an anionic surfactant, a nonionic surfactant, a zwitterionic surfactant, a cationic surfactant, an amphoteric surfactant, or a combination thereof. The surfactant system may include linear alkylbenzene sulfonates, alkyl ethoxylated sulfates, alkyl sulfates, nonionic surfactants, such as ethoxylated alcohols, amine oxides, or mixtures thereof. The surfactant may be at least partially derived from natural sources, such as natural feedstock alcohols.

Suitable anionic surfactants can include any conventional anionic surfactant. This may include sulphate detersive surfactants, such as alkoxylated and/or non-alkoxylated alkyl sulphate materials, and/or sulphonic detersive surfactants, such as alkyl benzene sulphonate. The anionic surfactant can be linear, branched, or a combination thereof. Preferred surfactants include linear alkyl benzene sulfonate (LAS), Alkyl Ethoxylated Sulfate (AES), Alkyl Sulfate (AS), or mixtures thereof. Other suitable anionic surfactants include branched modified alkyl benzene sulfonates (MLAS), Methyl Ester Sulfonates (MES), Sodium Lauryl Sulfate (SLS), sodium lauryl ether Sulfate (SLE), and/or Alkyl Ethoxylated Carboxylates (AEC). The anionic surfactant may be present in the acid form, salt form, or mixtures thereof. Anionic surfactants can be partially or fully neutralized, for example, with alkali metals (e.g., sodium) or amines (e.g., monoethanolamine).

The surfactant system may include a nonionic surfactant. Suitable nonionic surfactants include alkoxylated fatty alcohols, such as ethoxylated fatty alcohols. Other suitable nonionic surfactants include alkoxylated alkylphenols, alkylphenol condensates, mid-chain branched alcohols, mid-chain branched alkyl alkoxylates, alkyl polysaccharides (e.g., alkyl polyglycosides), polyhydroxy fatty acid amides, ether terminated polyalkoxylated alcohol surfactants, and mixtures thereof. The alkoxylated units may be ethyleneoxy units, propyleneoxy units, or mixtures thereof. The nonionic surfactant can be linear, branched (e.g., mid-chain branched), or a combination thereof. Specific nonionic surfactants can include alcohols having an average of about 12 to about 16 carbons and an average of about 3 to about 9 ethoxy groups, such as C12-C14 EO7 nonionic surfactants.

Suitable zwitterionic surfactants may include any conventional zwitterionic surfactant, such as betaines, including alkyl dimethyl betaine and coco dimethyl amidopropyl betaine, C₈To C₁₈(e.g. C)₁₂To C₁₈) Amine oxides (e.g. C)_12-14Dimethylamine oxide), and/or sulfo and hydroxy betaines, such as N-alkyl-N, N-dimethylamino-1-propane sulfonate, where the alkyl group may be C₈To C₁₈Or C₁₀To C₁₄. The zwitterionic surfactant can include an amine oxide.

Depending on the formulation and/or intended end use, the composition may be substantially free of certain surfactants. For example, liquid fabric enhancer compositions, such as fabric softeners, may be substantially free of anionic surfactants, as such surfactants may negatively interact with cationic ingredients.

b. Modulating active agents

The compositions of the present invention may include a modulating active. Compositions containing a conditioning active may provide softness, anti-wrinkle, anti-static, conditioning, stretch-resistance, color, and/or appearance benefits.

The conditioning active may be present at a level of from about 1% to about 99% by weight of the composition. The composition may comprise from about 1%, or from about 2%, or from about 3% to about 99%, or to about 75%, or to about 50%, or to about 40%, or to about 35%, or to about 30%, or to about 25%, or to about 20%, or to about 15%, or to about 10%, by weight of the composition, of the conditioning active. The composition may comprise from about 5% to about 30% of a conditioning active, by weight of the composition.

Conditioning actives suitable for the compositions of the present invention may include quaternary ammonium ester compounds, silicones, non-ester quaternary ammonium compounds, amines, fatty esters, sucrose esters, silicones, dispersible polyolefins, polysaccharides, fatty acids, softening or conditioning oils, polymer latexes, or combinations thereof.

The composition may include a quaternary ammonium ester compound, a silicone, or a combination thereof, preferably a combination. The combined total amount of quaternary ammonium ester compound and silicone may be from about 5% to about 70%, or from about 6% to about 50%, or from about 7% to about 40%, or from about 10% to about 30%, or from about 15% to about 25%, by weight of the composition. The composition may include the quaternary ammonium ester compound and the silicone in a weight ratio of about 1:10 to about 10:1, or about 1:5 to about 5:1, or about 1:3 to about 1:3, or about 1:2 to about 2:1, or about 1:1.5 to about 1.5:1, or about 1:1.

The composition may contain a mixture of different types of conditioning active agents. The compositions of the present invention may contain certain conditioning actives substantially free of others. For example, the composition can be free of quaternary ammonium ester compounds, silicones, or both. The composition can comprise a quaternary ammonium ester compound and be substantially free of silicone. The composition can comprise a silicone and be substantially free of quaternary ammonium ester compounds.

c. Deposition aid

The compositions of the present invention may comprise a deposition aid. The deposition aid may facilitate deposition of benefit agent delivery particles, conditioning actives, perfumes, or combinations thereof, thereby improving the performance benefits of the composition and/or allowing for more efficient formulation of such benefit agents. The composition may comprise from 0.0001% to 3%, preferably from 0.0005% to 2%, more preferably from 0.001% to 1%, or from about 0.01% to about 0.5%, or from about 0.05% to about 0.3%, by weight of the composition, of the deposition aid. The deposition aid may be a cationic or amphoteric polymer, preferably a cationic polymer.

Cationic polymers in general and processes for their preparation are known from the literature. Suitable cationic polymers may include quaternary ammonium polymers known as "polyquaternium" polymers, such as polyquaternium-6 (polydiallyldimethylammonium chloride), polyquaternium-7 (a copolymer of acrylamide and diallyldimethylammonium chloride), polyquaternium-10 (quaternized hydroxyethylcellulose), polyquaternium-22 (a copolymer of acrylic acid and diallyldimethylammonium chloride), and the like, as designated by International Nomenclature for Cosmetic Ingredients (International Nomenclature for Cosmetic Ingredients).

The deposition aid may be selected from the group consisting of: polyvinyl formamide, partially hydroxylated polyvinyl formamide, polyvinyl amine, polyethyleneimine, ethoxylated polyethyleneimine, polyvinyl alcohol, polyacrylate, and combinations thereof. The cationic polymer may comprise a cationic acrylate.

The deposition aid may be added simultaneously with the particles (simultaneously with, for example, the encapsulated benefit agent) or directly/independently in the fabric treatment composition. The weight average molecular weight of the polymer may be from 500 to 5000000, or from 1000 to 2000000, or from 2500 to 1500000 daltons, as determined by size exclusion chromatography using Refractive Index (RI) detection relative to polyethylene oxide standards. The cationic polymer may have a weight average molecular weight of 5000 to 37500 daltons.

d. Rheology modifier/structurant

The compositions of the present invention may contain rheology modifiers and/or structurants. Rheology modifiers can be used to "thicken" or "thin" the liquid composition to a desired viscosity. Structuring agents may be used to promote phase stability and/or to suspend or inhibit particles in liquid compositions, such as benefit agent delivery particle aggregates as described herein.

Suitable rheology modifiers and/or structurants can include non-polymeric crystalline hydroxyl functional structurants (including those based on hydrogenated castor oil), polymeric structurants, cellulosic fibers (e.g., microfibrillated cellulose, which can be derived from bacterial, fungal, or plant sources, including from wood), diamido gelling agents, or combinations thereof.

The polymeric structurant may be of natural origin or synthetic. Polymeric structurants of natural origin may comprise hydroxyethyl cellulose, hydrophobically modified hydroxyethyl cellulose, carboxymethyl cellulose, polysaccharide derivatives and mixtures thereof. The polysaccharide derivative may comprise pectin, alginate, arabinogalactan (gum arabic), carrageenan, gellan gum, xanthan gum, guar gum and mixtures thereof. Synthetic polymeric structurants may comprise polycarboxylates, polyacrylates, hydrophobically modified ethoxylated polyurethanes, hydrophobically modified nonionic polyols and mixtures thereof. The polycarboxylate polymer may comprise polyacrylate, polymethacrylate, or mixtures thereof. The polyacrylates may contain C of unsaturated mono-or dicarbonic acids and (meth) acrylic acid₁-C₃₀Copolymers of alkyl esters. Such copolymers are available from Noveon Inc under the tradename Carbopol Aqua 30. Another suitable structurant is sold under the tradename Rheovis CDE, available from BASF.

Method for making a composition

The present invention relates to methods of making any of the compositions described herein. A method of making a composition may comprise the step of combining benefit agent delivery particles as described herein with an adjunct material which may be a consumer product adjunct material as described herein.

When the particles are in one or more forms including slurry form, neat particle form, and/or spray dried particle form, the particles can be combined with one or more auxiliary materials such as consumer product auxiliary materials. The particles may be combined with auxiliary materials, such as consumer product auxiliary materials, by methods including mixing and/or spraying.

The compositions of the present invention may be formulated in any suitable form and prepared by any method chosen by the formulator. The particles and auxiliary materials may be combined in a batch process, in a circulating loop process, and/or by an in-line mixing process. Equipment suitable for use in the processes disclosed herein may include continuous stirred tank reactors, homogenizers, turbine mixers, circulation pumps, paddle mixers, plow shear mixers, ribbon mixers, vertical axis granulators and drum mixers (in both batch and continuous process (where applicable) configurations), spray dryers and extruders.

Method for treating a surface or an article

The invention further relates to a method for treating a surface or an article with a composition according to the invention. Such methods can provide cleaning, conditioning, and/or freshening benefits.

Suitable surfaces or articles may include fabrics (including cloth, towel or linen), hard surfaces (such as tile, porcelain, linoleum or wood flooring), tableware, hair, skin, or mixtures thereof.

The method may comprise the step of contacting a surface or article with a composition of the invention. The composition may be in neat form or diluted in a liquid such as a wash or rinse liquor. The composition may be diluted in water before, during or after contacting the surface or article. The surface or article may optionally be washed and/or rinsed before and/or after the contacting step.

A method of treating and/or cleaning a surface or article may comprise the steps of:

a) optionally washing, rinsing and/or drying the surface or article;

b) contacting a surface or article with a composition as described herein, optionally in the presence of water;

c) optionally washing and/or rinsing the surface or article; and is

d) Optionally by passive drying and/or via active methods such as a clothes dryer.

For purposes of the present invention, washing includes, but is not limited to, scrubbing and mechanical agitation. The fabric may comprise most any fabric that is capable of being laundered or otherwise treated under normal consumer use conditions.

Liquids that can include the disclosed compositions can have a pH of about 3 to about 11.5. Upon dilution, such compositions are typically employed at concentrations of about 500ppm to about 15,000ppm in solution. When the wash solvent is water, the water temperature is typically from about 5 ℃ to about 90 ℃, and when the location contains fabric, the water to fabric ratio is typically from about 1:1 to about 30: 1.

The present invention further relates to a surface or article treated with a composition as described herein. A surface or article treated with a composition according to the invention may comprise particles according to the invention in or on the surface, e.g. after treatment.

Test method

It is to be understood that the test methods disclosed in the test methods section of the present application are to be used to determine the corresponding values for the parameters of the subject matter described and claimed herein.

Combination of

Particularly contemplated combinations of the present invention are described herein in the following paragraphs labeled with letters. These combinations are intended to be illustrative in nature and are not intended to be limiting.

A. A composition comprising an adjunct material and/or an encapsulate having a volume weighted median encapsulate size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, said encapsulate comprising a core and a shell, said shell encapsulating said core, (a) said shell comprising a poly (meth) acrylate polymer comprising the reaction product of at least one monomer or oligomer thereof, (I) the monomer comprising a structure according to formula I:

wherein R is¹Is selected from C₁To C₈Alkyl radical, wherein R²Is hydrogen or methyl, wherein n is an integer from 1 to 3, wherein a is a ring structure selected from:

(b) the core comprises a benefit agent; the core also comprises from more than 0% to about 80%, preferably from more than 0% to 50%, more preferably from more than 0% to about 30%, most preferably from more than 0% to about 20%, based on total core weight, of a partitioning modifier. In any or all combinations herein, the adjunct material can be a consumer adjunct material or a non-consumer, such as industrial, adjunct material.

B. The composition of claim 1, wherein the poly (meth) acrylate polymer of the shell comprises the reaction product of at least three monomers or oligomers thereof, the monomers comprising a first monomer, a second monomer, and a third monomer, (a) the first monomer comprises a structure according to formula I, (b) the second monomer comprises a basic (meth) acrylate monomer, and (c) the third monomer comprises an acidic (meth) acrylate monomer.

C. A composition comprising an adjunct material and an encapsulate having a volume weighted median encapsulate size of from about 0.5 microns to about 100 microns, preferably from about 1 micron to about 60 microns, said encapsulate comprising a core and a shell, said shell encapsulating said core, (a) said shell comprising a poly (meth) acrylate polymer comprising the reaction product of at least a first, second and third monomer or oligomer thereof, (I) the first monomer comprising a structure according to formula I in paragraph a, wherein R is¹Is selected from C₁To C₈Alkyl radicalWherein R is²Is hydrogen or methyl, wherein n is an integer from 1 to 3, wherein a is a ring structure selected from any one of formulae II, III, IV, V or VI in paragraph a, with the proviso that when a of formula I is structure II, the shell is free of polymers formed from monofunctional ethylenically unsaturated monomers; (ii) the second monomer comprises a basic (meth) acrylate monomer; (iii) the third monomer comprises an acidic (meth) acrylate monomer; and (b) the core comprises a benefit agent; wherein the composition is a consumer product.

D. The composition of claim 3, wherein the core further comprises a partitioning modifier, preferably from more than 0% to about 80%, more preferably from more than 0% to 50%, even more preferably from more than 0% to about 30%, and even more preferably from more than 0% to about 20%, based on total core weight.

E. The composition of any one of the preceding claims, wherein the volume weighted median encapsulate size is from 25 microns to 60 microns.

F. The composition of any one of the preceding claims, wherein the encapsulate has a one-week leakage percentage of core of less than 25 wt% measured after one week of storage at 35 ℃.

G. The composition of any of the preceding claims, wherein the basic (meth) acrylate monomer or oligomer thereof comprises less than 1 weight percent of the encapsulate and the acidic (meth) acrylate monomer or oligomer thereof comprises less than 1 weight percent of the encapsulate.

H. A composition according to any one of the preceding claims, wherein in formula I, n-3, R¹Is selected from C₂To C₅Alkyl, and A is

I. The composition according to any one of the preceding claims, wherein the monomer according to formula I is selected from:

or oligomers of any such monomer.

J. The composition of any of the preceding claims, wherein the partitioning modifier comprises a compound selected from the group consisting of vegetable oils, modified vegetable oils, C₄-C₂₄Mono-, di-and triesters of fatty acids, propane-2-yltetradecanoate (i.e., isopropyl myristate), lauryl benzophenone, lauryl alcohol laurate, methyl behenate, methyl laurate, methyl palmitate, methyl stearate, and mixtures thereof, preferably isopropyl myristate.

K. The composition according to any of the preceding claims, wherein the encapsulate comprises from about 0.5% to about 40%, more preferably from 0.8% to 5%, based on total encapsulate weight, of an emulsifier, preferably said emulsifier is selected from the group consisting of polyvinyl alcohol, carboxylated or partially hydrolyzed polyvinyl alcohol, methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, methylhydroxypropyl cellulose, salts or esters of stearic acid, lecithin, organic sulfonic acids, 2-acrylamido-2-alkylsulfonic acids, styrenesulfonic acid, polyvinylpyrrolidone, copolymers of N-vinylpyrrolidone, polyacrylic acid, polymethacrylic acid, copolymers of acrylic acid and methacrylic acid, and water-soluble surfactant polymers that lower the surface tension of water, more preferably the emulsifier comprises polyvinyl alcohol, preferably the polyvinyl alcohol has at least one of the following properties:

(i) a degree of hydrolysis of from about 55% to about 99%, preferably from about 75% to about 95%, more preferably from about 85% to about 90%, most preferably from about 87% to about 89%; and/or

(ii) A viscosity of from about 40cps to about 80cps, preferably from about 45cps to about 72cps, more preferably from about 45cps to about 60cps, most preferably from 45cps to 55cps in a 4% aqueous solution at 20 ℃; and/or

(iii) A degree of polymerization of from about 1500 to about 2500, preferably from about 1600 to about 2200, more preferably from about 1600 to about 1900, most preferably from about 1600 to about 1800; and/or

(iv) A weight average molecular weight of from about 130,000 to about 204,000 daltons, preferably from about 146,000 to about 186,000, more preferably from about 146,000 to about 160,000, most preferably from about 146,000 to about 155,000; and/or

(v) A number average molecular weight of from about 65,000 to about 110,000 daltons, preferably from about 70,000 to about 101,000, more preferably from about 70,000 to about 90,000, most preferably from about 70,000 to about 80,000.

L. the composition of any of the preceding claims, wherein any of the first, second, and third monomers is an oligomer or prepolymer of monomers.

A composition according to any preceding claim wherein the basic (meth) acrylate monomer or oligomer comprises an aminoalkyl acrylate or methacrylate wherein the alkyl moiety is one to twelve carbons.

The composition of any preceding claim, wherein the basic (meth) acrylate monomer is selected from the group consisting of: ethylaminoethyl acrylate, ethylaminoethyl methacrylate, aminoethyl acrylate, aminoethyl methacrylate, t-butylaminoethyl acrylate, t-butylaminoethyl methacrylate, diethylamino acrylate, diethylamino methacrylate, diethylaminoethyl acrylate, diethylaminoethyl methacrylate, dimethylaminoethyl acrylate and dimethylaminoethyl methacrylate.

A composition according to any of the preceding claims wherein the acidic (meth) acrylate monomer or oligomer comprises a carboxyl substituted acrylate or methacrylate monomer.

P. the composition of any of the preceding claims wherein the acidic (meth) acrylate monomer comprises a carboxyalkyl acrylate, a carboxyalkyl methacrylate, a carboxyaryl acrylate, a carboxyaryl methacrylate, or a (meth) acryloxyphenyl alkyl carboxylic acid wherein the alkyl moiety is one to twelve carbons.

A composition according to any preceding claim wherein the acidic (meth) acrylate monomer is selected from the group consisting of: 2-carboxyethyl acrylate, 2-carboxyethyl methacrylate, 2-carboxypropyl acrylate, 2-carboxypropyl methacrylate, carboxyoctyl acrylate, carboxyoctyl methacrylate, 2-acryloxybenzoic acid, 3-acryloxybenzoic acid, 4-acryloxybenzoic acid, 2-methacryloxybenzoic acid, 3-methacryloxybenzoic acid, and 4-methacryloxybenzoic acid, 4-acryloxyphenylacetic acid, and 4-methacryloxyphenylacetic acid.

The composition according to any one of the preceding claims, wherein the encapsulate comprises a coating on said shell, preferably said coating comprises a coating material selected from the group consisting of: poly (meth) acrylates, polyethylene-maleic anhydride, polyamines, waxes, polyvinylpyrrolidone copolymers, polyvinylpyrrolidone-ethyl acrylate, polyvinylpyrrolidone-vinyl acrylate, polyvinylpyrrolidone-methacrylic acid ester, polyvinylpyrrolidone/vinyl acetate, polyvinyl acetal, polyvinyl butyral, polysiloxanes, polypropylene maleic anhydride, maleic anhydride derivatives, copolymers of maleic anhydride derivatives, polyvinyl alcohol, styrene-butadiene latex, gelatin, gum arabic, carboxymethyl cellulose, carboxymethyl hydroxyethyl cellulose, other modified celluloses, sodium alginate, chitosan, casein, pectin, modified starch, polyvinyl acetal, polyvinyl butyral, polyvinyl methyl ether/maleic anhydride, polyvinylpyrrolidone and its copolymers, poly (vinylpyrrolidone/methacrylamidopropyltrimethylammonium chloride), polyvinylpyrrolidone/vinyl acetate, polyvinylpyrrolidone/dimethylaminoethyl methacrylate, polyvinylamine, polyvinylformamide, polyallylamine, copolymers of polyvinylamine, polyvinylformamide, polyallylamine, and mixtures thereof.

S. the composition of any of the preceding claims, wherein the adjunct material comprises from about 0.1% to about 50%, 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%, by weight of the total composition, of a conditioning active, preferably the conditioning active is selected from the group consisting of: quaternary ammonium compounds, amines, fatty esters, sucrose esters, silicones, dispersible polyolefins, clays, polysaccharides, fatty acids, softening oils, polymer latexes, and mixtures thereof.

The composition of any of the preceding claims, wherein the adjunct material comprises from about 1% to about 70%, or from about 2% to about 60%, or from about 5% to about 50%, by weight of the composition, of a surfactant system.

A composition according to any preceding claim wherein the benefit agent is selected from the group consisting of: perfume raw materials, lubricants, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, skin cooling agents, vitamins, sunscreens, antioxidants, glycerin, catalysts, bleach particles, silica particles, odor reducing agents, odor control materials, chelating agents, antistatic agents, softeners, insect and moth repellents, agricultural actives, colorants, antioxidants, chelating agents, thickeners, drape and form control agents, smoothing agents, wrinkle control agents, detergents, disinfectants, bacteria control agents, mildew control agents, antiviral agents, desiccants, antifouling agents, detergents, fabric fresheners and preservatives, chlorine bleach odor control agents, color fixatives, dye transfer inhibitors, color maintenance agents, optical brighteners, color reduction/restoration agents, anti-fading agents, whiteness enhancers, anti-abrasion agents, abrasion resistance agents, fabric integrity agents, anti-wear agents, anti-pilling agents, anti-foaming agents, UV protection agents, solar fade inhibitors, anti-allergic agents, enzymes, water repellents, fabric comfort agents, anti-shrinkage agents, anti-stretch agents, elastic recovery agents, skin care agents, synthetic or natural actives, antibacterial actives, antiperspirant actives, cationic polymers, dyes, and mixtures thereof; perfume raw materials are preferred.

The composition of any preceding claim, the consumer product adjunct material being selected from the group consisting of: surfactants, conditioning actives, deposition aids, rheology modifiers or structurants, bleach systems, stabilizers, synergists, chelants, dye transfer inhibitors, dispersants, enzymes, enzyme stabilizers, catalytic metal complexes, polymeric dispersants, desliming and soil/anti-redeposition agents, brighteners, suds suppressors, silicones, toners, aesthetic dyes, additional perfumes and perfume delivery systems, structure elasticizing agents, carriers, hydrotropes, processing aids, structurants, anti-agglomeration agents, coatings, formaldehyde scavengers, pigments, and mixtures thereof; preferably at least a structuring agent, a deposition aid or a mixture thereof.

The composition of any preceding claim, wherein at least 75% of the encapsulates have a diameter of greater than 15 microns, preferably greater than 20 microns, more preferably greater than 25 microns, as determined according to the encapsulate size (diameter) test method described herein.

The composition of any one of the preceding claims, wherein at least 75% of the encapsulates have an encapsulate wall thickness of from about 10nm to about 350nm, from about 20nm to about 200nm, or from 25nm to about 180nm, as determined by the encapsulate wall thickness test method disclosed herein.

Composition according to any one of the preceding claims, having a molecular weight distribution in the range of 20s^-1And a viscosity at 21 ℃ of 1 to 1500 cps (1-1500 mPas), or 100 to 1000 cps (100-.

The composition of any of the preceding claims comprising from about 0.001 wt% to about 25 wt% of the encapsulate, based on total consumer quality.

The composition of any preceding claim, wherein the composition is in the form of a liquid composition, a granular composition, a single compartment pouch, a multi-compartment pouch, a dissolvable tablet, a lozenge or bead, a fibrous article, a tablet, a bar, a flake, a dry tablet, or a mixture thereof.

BB. the composition according to any preceding claim, wherein the product is a consumer product, is a fabric and home care product, a beauty care product, or mixtures thereof, wherein where the consumer product is a fabric and home care product, preferably the fabric and home care product is selected from a laundry detergent composition, a fabric conditioning composition, a wash and rinse additive, a fabric pre-treatment composition, a fabric freshening composition, or mixtures thereof; and wherein in case the consumer product is a cosmetic care product, preferably the cosmetic care product is selected from a hair care product, a skin care product, a shaving care product, a personal cleansing product, a deodorant and/or antiperspirant, or mixtures thereof.

A method of treating a surface or article, the method comprising: (a) optionally washing, rinsing and/or drying the surface or article; (b) contacting the surface or article with a composition according to any one of the preceding claims, optionally in the presence of water; and (c) optionally washing, rinsing and/or drying the surface or article, wherein the drying step comprises active drying and/or passive drying.

(1)Extraction of benefit agent delivery particles from finished products

Unless otherwise specified herein, the preferred method of separating the benefit agent delivery particles from the finished product is based on the fact that the density of most such particles is different from that of water. The finished product is mixed with water to dilute and/or release the granules. The diluted product suspension is centrifuged to accelerate particle separation. Such particles tend to float or sink in the dilute solution/dispersion of the finished product. Using a pipette or spatula, the top and bottom layers of the suspension are removed and subjected to additional rounds of dilution and centrifugation to separate and enrich the particles. The particles were observed at total magnifications of 100 x and 400 x using an optical microscope equipped with cross-polarization filters or Differential Interference Contrast (DIC). Microscopic observation provides a preliminary indication of the presence, size, quality and aggregation of the delivery particles.

For the extraction of the delivery particles from the finished liquid fabric enhancer product, the following procedure was performed:

1. three aliquots of about 20ml of liquid fabric enhancer are placed in three separate 50ml centrifuge tubes and each aliquot is diluted 1:1 with deionized water (e.g., 20ml of fabric enhancer plus 20ml of deionized water), mixed well and centrifuged at about 10000 xg for 30 minutes.

2. After centrifugation as in step 1, the bottom aqueous layer (about 10ml) in each 50ml centrifuge tube was discarded, and then 10ml deionized water was added to each 50ml centrifuge tube.

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

4. Removing the top layer with a spatula or pipette, and

5. the top layer was transferred to a 1.8ml centrifuge tube and centrifuged at approximately 20000 Xg for 5 minutes.

6. The top layer was removed with a spatula and transferred to a new 1.8ml centrifuge tube and deionized water was added until the tube was completely filled and then centrifuged at approximately 20000 × g for 5 minutes.

7. Remove the bottom layer with a fine pipette and add deionized water until the tube is completely filled and centrifuge at about 20000 × g for 5 minutes.

8. Repeat step 7 another 5 times (6 total times).

If both top and bottom layer enriched particles are present in step 1 above, move immediately to step 3 (i.e. omit step 2) and proceed to steps 4 to 8. Once those steps were completed, the bottom layer was also removed from the 50ml centrifuge tube of step 1 using a spatula and/or pipette. The bottom layer was transferred to a 1.8ml centrifuge tube and centrifuged at approximately 20000 Xg for 5 min. The bottom layer in the new tube was removed and deionized water was added until the tube was completely filled, followed by centrifugation at approximately 20000 × g for 5 minutes. The top layer (water) was removed and deionized water was added again until the tube was full. This was repeated 5 more times (6 total times). The top and bottom layers, which are enriched and separated from the particles, are recombined back together.

If the fabric enhancer is white or a particle-rich layer is difficult to distinguish, 4 drops of dye (such as Liquitint Blue JH 5% premix from Milliken & Company, Spartanburg, South Carolina, usa) are added to the centrifuge tube of step 1 and the separation is continued as described.

To extract the delivery particles from a solid finished product that is readily dispersible in water, 1L of deionized water is mixed with 20g of finished product (e.g., detersive foams, films, gels and granules; or water-soluble polymers; soap chips and bars; and other readily water-soluble bases such as salt, sugar, clay and starch). When extracting particles from finished products that are not readily dispersible in water (such as waxes, drying plates, drying sticks, and oily materials), it may be desirable to add detergents, agitate, and/or gently heat the product and diluent to release the particles from the matrix. The use of organic solvents or drying out of the particles during the extraction step should be avoided as these actions may damage the delivery particles at this stage.

To extract the delivery particles from a liquid finished product that is not a fabric softener or fabric enhancer (e.g., liquid laundry detergents, liquid dishwashing detergents, liquid hand soaps, lotions, shampoos, conditioners, and hair dyes), 20ml of the finished product is mixed with 20ml of deionized water. If desired, NaCl (e.g., 100-200g NaCl) may be added to the diluted suspension to increase the density of the solution and to promote particle flotation to the top layer. If the product is white, making it difficult to distinguish the particle layers formed during centrifugation, a water-soluble dye may be added to the diluent to provide visual contrast.

The water and product mixture is subjected to successive rounds of centrifugation involving removal of the top and bottom layers, resuspension of those layers in fresh dilution, followed by further centrifugation, separation and resuspension. Each round of centrifugation occurs in tubes of volume 1.5 to 50ml, using centrifugal forces up to 20,000 × g, for 5 to 30 minutes. At least six rounds of centrifugation are typically required to extract and clean enough particles for testing. For example, a first round of centrifugation can be performed in 50ml tubes, spun at 10,000 × g for 30 min; followed by five more rounds of centrifugation, where the top and bottom layer of material were resuspended in fresh dilution in 1.8ml tubes, respectively, and spun at 20,000 Xg for 5min per round.

If the delivery particles are observed microscopically in the top and bottom layers, the particles of the two layers are recombined after the final centrifugation step to produce a single sample containing all the delivery particles extracted from the product. The extracted particles should be analyzed as soon as possible and may also be stored as a suspension in deionized water for up to 14 days.

Those skilled in the art will recognize that various other protocols may be constructed for the extraction and separation of delivery particles from finished products, and will recognize that such methods are validated via a comparison of the resulting measurements, as measured before and after the particles are added to and extracted from the finished product.

(2)Breaking strength

To calculate the percentage of delivery particles that fall within the required breaking strength range, three different measurements were made and two resulting graphs were utilized. Three separate measurements are required: i) volume weighted Particle Size Distribution (PSD); ii) the diameter of 10 individual particles within each of 3 specified size ranges; and iii) breaking force of the above 30 single particles. Two graphs were generated: the above i) collected volume weighted particle size distribution data plot; and a simulated distribution plot of the relationship between particle diameter and fracture strength derived from the data collected in ii) and iii) above. The simulated relationship plot enables particles within the desired intensity range to be identified as a specific region below the volume weighted PSD curve and then calculated as a percentage of the total area below the curve.

a.) volume weighted Particle Size Distribution (PSD) was determined via Single Particle Optical Sensing (SPOS), also known as Optical Particle Counting (OPC), using an AccuSizer 780AD instrument and accompanying software CW788 version 1.82(Particle Sizing Systems, Santa Barbara, California, usa). The instrument is configured to the following conditions and options: flow rate 1 ml/s, lower size threshold 0.50 μm, sensor model LE400-05SE, auto-dilution open, collection time 120 seconds, number of channels 512, volume of container fluid 50ml, maximum coincidence 9200. The measurement was started by flushing the sensor with water until the background count was below 100. A sample of the delivery particles in suspension is introduced and its particle density adjusted with deionized water via automated dilution as necessary to yield a particle count of at least 9200 particles per ml. The suspension was analyzed over a period of 120 seconds. The resulting volume weighted PSD data was plotted and recorded and the median, 5 th percentile and 90 th percentile values were determined.

b.) the diameter and fracture force values (also known as burst force values) of individual particles are measured via a computer-controlled micromanipulator system having a lens and camera capable of imaging the delivered particles, and having a fine flat-ended probe (such as model 403A, available from Aurora Scientific Inc, canada) attached to a load cell, such as Zhang, Z, et al (1999) "Mechanical strain of single microcapsules specified by a novel micromanipulation technique," j.microencapsulation, volume 16, phase 1, phase 117 @, and Sun, g, and Zhang, Z. (2001) "Mechanical Properties of membrane-formed microcapsules," j.microencapsulation, volume 18, phase 5, phase 593, and as described in bighamm, biodheim, available from biodistribution, bib, available from yom.

c.) drop the delivery particle suspension onto a microscope slide and dry for a few minutes at ambient conditions to remove water and achieve a sparse monolayer of individual particles on the dry slide. The concentration of particles in the suspension is adjusted as needed to achieve the appropriate particle density on the slide. It may be desirable to prepare more than one slide.

d.) the slide is then placed on the sample holding stage of the micromanipulation instrument. Thirty beneficial delivery particles on one or more slides were selected for measurement such that ten particles were selected within each of three pre-sized strips. Each size band refers to the diameter of the particle as deduced from the volume weighted PSD generated by the AccuSizer. The three size bands of particles were: mean diameter +/-2 μm, 5 th percentile diameter +/-2 μm and 90 th percentile diameter +/-2 μm. Particles that appear to be crushed, leaking or broken are excluded from the selection process and are not measured.

e.) for each of the 30 selected particles, the diameter of the particle was measured from the image on the micromanipulator and recorded. The particles were then compressed between two flat surfaces, a flat end force probe and a microscope slide, at a speed of 2 μm/sec until the particles broke. During the compression step, probe forces are continuously measured and recorded by the data acquisition system of the micromanipulation instrument.

f.) Using the measured diameters and assuming spherical particles, the cross-sectional area (π r) of each of the selected particles was calculated²Where r is the radius of the particles before compression). The force to break of each selected particle was determined from recorded force probe measurements as shown in Zhang, Z et al (1999) "Mechanical strain of single microcapsules determined by a novel micromanipulation technique" J.Microencapsidation, Vol.16, No. 1, page 117 and Sun, G. and Zhang, Z. (2001) "Mechanical Properties of Membrane-formed microcapsules" J.Microencapsidation, Vol.18, No. 5, page 593-602.

g.) the breaking strength of each of the 30 particles was calculated by dividing the breaking force (in newtons) by the calculated cross-sectional area of the respective particle.

h.) on a plot of particle diameter versus fracture strength, a power regression trend line was fitted to all 30 raw data points to generate a simulated distribution of the relationship between particle diameter and fracture strength.

i.) the percentage of particles having a fracture strength value within a particular strength range is determined by observing the simulated relationship to locate where the curve intersects the associated fracture strength limit, and then reading the particle size limits corresponding to those strength limits. These particle size limits are then located on the volume weighted PSD graph and thus identify the area under the PSD curve corresponding to the portion of particles that fall within the specified intensity range.

j.) the identified area under the PSD curve is then calculated as a percentage of the total area under the PSD curve. The percentage indicates the percentage of the delivery particle that falls within the specified range of breaking strength.

(3)ClogP

The logP values of various perfume ingredients have been reported, for example the Pomona92 database available from dailyght Chemical Information Systems, Inc (dailyght CIS, Irvine, California), contains many, along with references to the original literature. The logP value is most conveniently calculated by the "CLOGP" program (also available from dayright CIS). The program also enumerates experimental logP values as they are available in the Pomona92 database. "calculated logP" (ClogP) is determined by the fragment format of Hansch and Leo (see a.leo, Comprehensive Medicinal Chemistry, volume 4, c.hansch, p.g.sammens, j.b.taylor and c.a.ramsden, eds., page 295, Pergamon Press, 1990, incorporated herein by reference). Fragmentation is based on the chemical structure of each perfume ingredient and takes into account the number and type of atoms, atomic connectivity and chemical bonding. ClogP values can be used in selecting perfume ingredients useful in the present invention. Alternatively, logP values may be used in certain embodiments.

(4)Boiling point

The Boiling points of the perfume ingredients were measured according to Standard Test Method ASTM D2887-04a, "Standard Test Method for binding Range Distribution of Petroleum Fractions by Gas Chromatography" (ASTM International, West Conshohock, Pennsylvania, USA). Section 5.2 of the method indicates that: "the boiling range distribution obtained by this test method is substantially equivalent to the distribution obtained by a True Boiling Point (TBP) distillation (see test method D2892). They are not equivalent to results obtained from inefficient distillation, such as with test methods D86 or D1160. "

(5)Particle size (particle diameter)

The particle suspension or finished droplet is placed on a microscope slide and dried for a few minutes at ambient conditions to remove water and achieve a sparse monolayer of individual particles on the dry slide. The concentration of particles in the suspension is adjusted as needed to achieve the appropriate particle density on the slide. The slide glass was placed on a sample stage of an equipped optical microscope and examined at a total magnification of 100 × or 400 ×. Images were captured and calibrated for accurate measurement of particle diameter. Three replicate slides were prepared and analyzed.

For particle size measurement, at least 50 benefit agent delivery particles per slide were selected for measurement in a manner that was unbiased in their size, and thus a representative sample of the particle size distribution present was generated. This can be accomplished by examining fields of view selected randomly or according to a predefined grid pattern and measuring the diameter of all the delivery particles present in each field of view examined. Delivery particles that appear to be significantly non-spherical, collapsed, leaking or broken are not suitable for measurement, are excluded from the selection process and their diameters are not recorded. The diameter of each suitable delivery particle examined was measured using a microscope and the value recorded. The recorded particle diameter measurements are used to calculate the percentage of particles having a particle size within the required size range or ranges, and also to calculate the median particle size.

(6)Thickness of particle wall

Particle wall thickness was measured in nanometers for 50 benefit agent delivery particles using cryofracture cryoscanning electron microscopy (FF cryoSEM) at magnifications between 50,000 x and 150,000 x. Samples were prepared by flash freezing a suspension of small volumes of particles or finished product. Flash freezing can be achieved by immersion in liquid ethane or by using equipment such as a high pressure refrigerator 706802EM Pact model (Leica Microsystems, Wetzlar, germany). The frozen samples were fractured at-120 ℃ and then cooled to below-160 ℃ and lightly sputter coated with gold/palladium. These steps may be accomplished using a cryogenic preparation device such as that available from Gatan Inc. The frozen, fragmented and coated samples are then transferred to a suitable cryoSEM microscope, such as a Hitachi S-5200SEM/STEM (Hitachi High Technologies, Tokyo, Japan), at-170 ℃ or lower. In Hitachi S-5200, imaging was performed using 3.0KV accelerating voltage and 5 μ A-20 μ A tip emission current.

Images of the fractured walls were obtained from cross-sectional views of 50 beneficial delivery particles selected in a random manner without size deviation to produce representative samples of the particle size distribution present. The wall thickness of each of the 50 particles was measured by drawing a measurement line perpendicular to the outer surface of the particle wall using calibrated microscope software. 50 individual wall thickness measurements were recorded and used to calculate the average thickness, and the percentage of particles having a wall thickness within the required range.

(7)Leakage of beneficial agent

The amount of benefit agent leaking from the delivery particle is determined according to the following method:

a.) obtain an amount of two samples of the raw slurry of encapsulates such that 1g (or other amount as indicated) of encapsulated perfume (e.g. 1g perfume oil, excluding shell and/or partitioning modifier (if present)) is present in each sample.

b.) add one sample of the raw slurry of encapsulates to a suitable amount of product matrix (e.g. liquid detergent product or LFE product), where the encapsulates will be used to form a total of 100g (e.g. 5g slurry and 95g product matrix), and label the mixture as sample 1. In step d below, a second sample of the raw encapsulate slurry was used directly in its pure form without contacting the product matrix and labeled as sample 2.

c.) the particle-containing product matrix (sample 1) was aged at 35 ℃ for one week (or other times and/or temperatures as indicated) in a sealed glass jar.

d.) using filtration, particles were recovered from both samples. The particles of sample 1 (in the product matrix) were recovered after the aging step. The particles in sample 2 (pure feed slurry) were recovered at the same time as the aging step was initiated for sample 1.

e.) treating the recovered particles with a solvent to extract the beneficial agent material from the particles.

f.) analyzing the solvent containing the beneficial agent extracted from each sample via chromatography. The resulting benefit agent peak areas under the curve were integrated and these areas were summed to determine the total amount of benefit agent extracted from each sample.

g.) the percent of benefit agent leakage was determined by subtracting the difference of sample 1 from the value obtained for the total amount of benefit agent extracted from sample 2, expressed as a percentage of the total amount of benefit agent extracted from sample 2, as expressed in the following equation:

percent benefit agent leakage ═ ((sample 2-sample 1)/sample 2) × 100

(8)Viscosity of the oil

The measurement was carried out using an AR 550 rheometer/viscometer from TA instruments (New Castle, DE, USA) using parallel steel plates of 40mm diameter and a gap size of 500 μmViscosity of the finished liquid product. From 0.1s at 21 ℃ within 3 minutes^-1To 25s^-1Log shear rate scan of (2) to obtain (20) s^-1High shear viscosity at Low and 0.05s^-1Low shear viscosity.

(9) Spices and fragrance raw materials (PRM)

To determine the identity and quantify the weight of the encapsulated perfume, perfume ingredient or Perfume Raw Material (PRM) within the delivery agent particle, gas chromatography and mass spectrometry/flame ionization detector (GC-MS/FID) were employed. Suitable devices include: agilent Technologies G1530A GC/FID, Hewlett packager Mass selector 5973, and 5% phenylmethylpolysiloxane column J & W DB-5 (length 30 m. times. inner diameter 0.25 mm. times. film thickness 0.25 μm). About 3g of the suspension of finished product or delivery particles was weighed and the weight recorded, then the sample was diluted with 30mL of deionized water and filtered through a 5.0 μm pore size nitrocellulose filter membrane. The material captured on the filter was dissolved in 5mL of an ISTD solution (25.0 mg/L tetradecane in anhydrous ethanol) and heated at 60 ℃ for 30 minutes. The cooled solution was filtered through a 0.45 μm pore size PTFE syringe filter and analyzed via GC-MS/FID. Three known fragrance oils were used as control reference standards. Data analysis involved summing the total area number minus the ISTD area number and calculating the average Response Factor (RF) for 3 standard fragrances. The product encapsulated perfume response factor and total area number, along with the weight of the sample, are then used to determine the total weight percent of each PRM in the encapsulated perfume. PRMs are identified by mass spectral peaks.

(10) Volume weighted median particle size

Particle size was measured using an Accusizer 780A manufactured by Particle Sizing Systems, Santa Barbara CA. The instrument was calibrated to 0 to 300 μ using Duke particle size standards. Samples for particle size evaluation were prepared by the following steps: in about 5g of deionized water, about 1g of the emulsion is diluted if the volume weighted median particle size of the emulsion to be determined, or 1g of the capsule slurry if the final capsule volume weighted median particle size to be determined, and about 1g of this solution is further diluted in about 25g of water.

About 1g of the most dilute sample was added to the Accusizer and the test was started using the auto-dilution feature. Accusizer should read over 9200 counts/second. If the count is less than 9200, additional samples should be added. Accusizer will dilute the sample until 9200 counts/second and begin evaluation. Accusizer will display the results, including the volume weighted median size, after 2 minutes of testing.

The breadth index can be calculated by determining the particle size above 95% cumulative particle volume (95% size), the particle size above 5% cumulative particle volume (5% size), and the median volume weighted particle size (50% size, 50% particle volume above and below this size). Breadth index (5) ═ ((95% size) - (5% size)/50% size).

(11) Head space ratio

(a) A non-perfumed consumer product preparation (e.g. shampoo or leave-on conditioner) is obtained.

(b) Flavour microcapsules are obtained with a water content adjusted to reach a perfume content of 25 wt% in the aqueous slurry.

(c) Sample a was prepared by adding 2.0 grams of the aqueous slurry of flavor microcapsules to 95 grams of the non-flavored consumer product formulation. Then 3.0 grams of deionized water was added to balance the formulation to 100 grams. The formulation was aged at 40 degrees celsius for 1 week.

(d) Sample B was prepared by adding 0.50 grams of neat fragrance to 95 grams of a non-scented consumer product formulation. Then 4.5 grams of deionized water was added to balance the formulation to 100 grams. The formulation was aged at 40 degrees celsius for 1 week.

The headspace ratio is defined as the headspace concentration of sample A divided by the headspace concentration of sample B, H_{Sample A}/H_{Sample B}In which H is_{Sample A}Is the headspace concentration of consumer product formulation sample A, and H_{Sample B}Is the headspace concentration of consumer product formulation sample B.

Solid Phase Microextraction (SPME) -gas chromatography/mass spectrometry was used to measure the amount of perfume raw material in the headspace of the product. 1.0 gram of a sample (shampoo or conditioner) aged at 40 degrees celsius for 1 week is placed in a clean 20ml headspace vial and allowed to equilibrate at room temperature for at least 2 hours.

The samples were then analyzed using the MPS2-SMPE-GC-MS analysis system (GC-02001-.

Equipment:

1.20 ml headspace vial

2. Time-meter

3. Gas Chromatograph (GC): agilent model 6890 with CIS-4 sampler (Gerstel, Mulheim, Germany) and MPS-2 auto-sampler and TDU. For SPME analysis, a split/splitless injector (non-CIS-4 injector) was used.

GC column: j & W DB-5MS, 30M × 0.25mm ID, 1.0 μ M film thickness, available from J & W Scientific, Folsom, California, USA.

5. The carrier gas was helium at a flow rate of 1.5 ml/min.

6. The injector liner was a special SPME liner (ID 0.75mm) from Supelco.

7. The detector was a model 5973 mass selective detector from Agilent Technologies, inc., Wilmington, DE, usa, having a source temperature of about 230 ℃ and a MS Quad temperature of about 150 ℃.

And (3) analysis program:

1. the sample was transferred to the appropriate sample tray and SPME-GC-MS analysis was continued.

2. The sequence of sample loading and analysis was started. In this step, the sample is equilibrated on the auto-sampler tray for at least two hours, and then directly sampled from the tray. The SPME fiber bundle was DVB/CAR/PDMS (50/30 μm, 24ga, 1cm long). The sampling time was 5 minutes.

3. The injector temperature was 260 ℃.

4. The GC-MS analysis run was then started. The desorption time was 5 minutes.

5. The following temperature program was used:

i) the initial temperature was about 50 c, held for 3 minutes,

ii) increasing the initial temperature at a rate of about 6 ℃/min until a temperature of about 250 ℃ is reached, then increasing to 275 ℃ at 25 ℃/min, and holding at about 275 ℃ for 4.67 minutes.

6. Perfume compounds were identified using MS libraries from John Wiley & Sons and National Institute of Standards and Technology (NIST), purchased and licensed by Hewlett Packard.

7. Chromatographic peak integration for specific ions was performed using Chemstation software available from Agilent Technologies, inc.

8. The ratio of each PRM was calculated by dividing the peak area of the perfume raw material in sample a by the peak area in sample B.

9. Each ratio is then weighted by the weight composition of the perfume raw material in the perfume.

10. The headspace ratio is calculated as the sum of the individual perfume raw material ratios obtained in step 9.

(12) Odor Detection Threshold (ODT)

ODT was determined using a gas chromatograph. The gas chromatograph is calibrated to determine the exact volume of material injected by the syringe, the exact split ratio, and the hydrocarbon response using hydrocarbon standards with known concentrations and chain length distributions. The air flow rate was accurately measured and the sample volume was calculated assuming that the duration of human inhalation lasted 12 seconds. Since the exact concentration of the detector at any point in time is known, the mass per inspired volume, and therefore the concentration of the material, is known.

For example, to determine if a material has a threshold below 50 parts per billion, the solution is delivered to the aspiration orifice at a calculated concentration. Panelists inhaled the GC effluent and identified the retention time when odor was noted. The average of 6 panelists determines the threshold of attention. The desired amount of analyte was injected into the column to achieve a concentration of 50 parts per billion at the detector. Typical gas chromatograph parameters for determining the odor detection threshold are listed below:

GC: 5890Series II with FID detector, 7673 auto sampler

Column: j & W Scientific DB-1

Length 30m, inner diameter 0.25mm, film thickness 1 micron

The method comprises the following steps:

-split injection: split ratio 17/1

-an auto sampler: 1.13 microliter of each sample injection

-column flow rate: 1.10 ml/min

-air flow rate: 345 ml/min

-inlet temperature: 245 degree centigrade

Detector temperature: 285 degree centigrade

-initial temperature 50 degrees celsius, ramp rate 5 degrees celsius per minute, final temperature 280 degrees celsius, end time 6 minutes

The main assumptions: GC air increased sample dilution for 12 seconds per inspiration

(13) Test method for determining logP

The log (logP) of the octanol/water partition coefficient of each PRM in the perfume mixture tested was calculated. The logP of a single PRM was calculated using the Consensus logP comparative Model version 14.02(Linux), available from Advanced Chemistry Development Inc. (ACD/Labs) (Toronto, Canada), to provide a unitless logP value. The Consensus logP Computational Model of ACD/Labs is part of the ACD/Labs Model program suite.

Examples

While particular embodiments of the present subject matter have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Particle preparation-procedure 1:

a first oil phase consisting of 37.50g of aromatic oil, 0.22g of t-butylaminoethyl methacrylate, 0.22g of 2-carboxyethyl acrylate and 18.00g of multifunctional acrylate monomer or oligomer was prepared with mixing at room temperature for 30 minutes.

A second oil phase consisting of 112.50g of aromatic oil, 37.50g of isopropyl myristate, 1.00g of 2,2 '-azobis (2-methylbutyronitrile) and 0.80g of 4,4' -azobis [ 4-cyanovaleric acid ] was added to a jacketed steel reactor. The reactor was maintained at 35 ℃ under a nitrogen blanket and the oil solution was mixed at 600 RPM. The solution was heated to 70 ℃ and held at 70 ℃ for 45 minutes, after which it was cooled to 50 ℃. The first oil phase was added to the reactor at 50 ℃ and the combined oils were mixed for 10 minutes at 50 ℃.

An aqueous phase containing 70.03g Selvol 540PVA (Sekisui Specialty Chemicals, Dallas, TX) with 5% solids, 221.06g water, 1.10g 4,4' -azobis [ 4-cyanovaleric acid ], and 1.20g 21.5% NaOH was prepared and mixed until complete dissolution. After pre-reacting the oil phases together for 10 minutes at 50 ℃, the mixing was discontinued and the aqueous phase mixture was added to the oil phase. High shear agitation is applied to produce an emulsion having the desired dimensional characteristics. The temperature was raised to 75 ℃, maintained at 75 ℃ for 4 hours, raised to 95 ℃, and maintained at 95 ℃ for 6 hours. The batch was allowed to cool to room temperature.

Examples 1 to 11

According to particle preparation procedure 1, the polyfunctional monomer used was tris- (2-hydroxyethyl) isocyanurate triacrylate. The resulting particles had varying median particle sizes, as depicted in table 1.

Comparative example 12

Following particle preparation procedure 1, the polyfunctional monomer was a commercially available hexafunctional aromatic urethane acrylate CN975(Sartomer, Exton, PA).

Comparative example 13

According to particle preparation procedure 1, the polyfunctional monomer is an aliphatic urethane acrylate Ebecryl 8602(Allnex, Frankfurt, Germany).

Comparative example 14

According to particle preparation procedure 1, the polyfunctional monomer is a hexafunctional aromatic urethane acrylate Ebecryl 220(Allnex, Frankfurt, Germany).

Comparative example 15

According to particle preparation procedure 1, the polyfunctional monomer is an aliphatic urethane acrylate Ebecryl 8701(Allnex, Frankfurt, Germany).

Comparative example 16

According to particle preparation procedure 1, the polyfunctional monomer is the aliphatic urethane acrylate Ebecryl 8301R (Allnex, Frankfurt, Germany).

Example 17

Following particle preparation procedure 1, the polyfunctional monomer was 90 weight percent tris (2-hydroxyethyl) isocyanurate triacrylate and 10 weight percent 2-trifunctional acrylate SR517HP (Sartomer, Exton, Pa.).

Comparative example 18

According to particle preparation procedure 1, the polyfunctional monomer is aliphatic urethane acrylate Ebecryl 8415(Allnex, Frankfurt, Germany).

Comparative example 19

According to particle preparation procedure 1, the polyfunctional monomer is the aliphatic urethane acrylate Ebecryl 2221(Allnex, Frankfurt, Germany).

Examples 20 to 24

The particles were prepared according to particle preparation procedure 1 and the polyfunctional monomer used was tris- (2-hydroxyethyl) isocyanurate triacrylate, maintained at a constant amount, to which was added 20% by weight of two monomers as indicated in table 1.

Comparative examples 25 to 26

Following particle preparation procedure 1, the polyfunctional monomer was a commercially available hexafunctional aromatic urethane acrylate CN975(Sartomer, Exton, PA). Table 1 contains the data for all examples generated according to procedure 1.

To obtain the leakage data in table 1, the encapsulates were tested in a liquid detergent product matrix. The encapsulate is provided in a suitable amount to provide 1g of encapsulated perfume. The resulting liquid detergent product had the following formulation as provided in table a.

TABLE A

	The active agent is calculated by weight percent
		Alkyl Ether Sulfates (AES)	4.0
Dodecyl benzene sulfonic acid (HLAS)	9.2
		Ethoxylated alcohols	4.1
Amine oxide	0.5
		Fatty acids	1.7
Citric acid	2.8
		Diethylenetriamine penta (methylene phosphonic acid) sodium salt	0.5
Calcium chloride	0.01
		Sodium formate	0.03
Ethoxylated sulfated quaternized hexamethylenediamine	0.7
		Copolymers of polyethylene glycol and vinyl acetate	1.3
Optical brightener 49	0.05
		Perfume oils in microcapsules	1.0
1, 2-benzisothiazolin-3-one and 2-methyl-4-isothiazolin-3-one	0.005
		Ethanol	0.4
1, 2-propanediol	1.3
		Sodium cumene sulfonate	1.7
Monoethanolamine	0.2
		NaOH	3.1
Structuring agent (hydrogenated castor oil)	0.3
		Silicone emulsions	0.0025
Dye material	0.005
		Water (W)	Remainder value

TABLE 1

Particle preparation-procedure 2:

a first oil phase consisting of 44.50g of aromatic oil, 0.74g of t-butylaminoethyl methacrylate, 0.74g of 2-carboxyethyl acrylate and 41.30g of multifunctional acrylate monomer or oligomer was prepared with mixing at room temperature for 30 minutes.

A second oil phase consisting of 142.67g of aromatic oil, 1.29g of 2,2 '-azobis (2-methylbutyronitrile) and 0.98g of 4,4' -azobis [ 4-cyanovaleric acid ] was fed to a jacketed steel reactor. The reactor was maintained at 35 ℃ under a nitrogen blanket and the oil solution was mixed at 600 RPM. The solution was heated to 70 ℃ and held at 70 ℃ for 45 minutes, after which it was cooled to 50 ℃. The first oil phase was added to the reactor at 50 ℃ and the combined oils were mixed for an additional 10 minutes at 50 ℃.

An aqueous phase containing 70.03g Selvol 540PVA (Sekisui Specialty Chemicals, Dallas, TX) with 5% solids, 221.06g water, 0.42g 4,4' -azobis [ 4-cyanovaleric acid ], and 0.46g 21.5% NaOH was prepared and mixed until complete dissolution. After pre-reacting the oil phases together for 10 minutes at 50 ℃, mixing was discontinued and the aqueous phase mixture was added to the mixed oil phases. High shear agitation is applied to produce an emulsion having the desired dimensional characteristics. The temperature was raised to 75 ℃, maintained at 75 ℃ for 4 hours, raised to 95 ℃, and maintained at 95 ℃ for 6 hours. The batch was allowed to cool to room temperature.

Example 27

According to particle preparation procedure 2, the polyfunctional monomer used was tris- (2-hydroxyethyl) isocyanurate triacrylate.

Comparative example 28

Following particle preparation procedure 2, the polyfunctional monomer used was a blend of 45% by weight of tris- (2-hydroxyethyl) isocyanurate triacrylate and 55% by weight of ethylene glycol dimethacrylate.

Comparative example 29

Following particle preparation procedure 2, the polyfunctional monomer used was a blend of 45% by weight of tris- (2-hydroxyethyl) isocyanurate triacrylate and 55% by weight of pentaerythritol tetraacrylate.

Comparative example 30

The polyfunctional monomer used was a blend of 60% by weight of tris- (2-hydroxyethyl) isocyanurate triacrylate and 40% by weight of tricyclodecane dimethanol diacrylate according to particle preparation procedure 2.

Comparative example 31

Following particle preparation procedure 2, the polyfunctional monomer used was a blend of 70% trimethylolpropane triacrylate and 30% tris- (2-hydroxyethyl) isocyanate triacrylate by weight.

Comparative example 32

According to particle preparation procedure 2, the polyfunctional monomer used was pentaerythritol tetraacrylate.

Table 2 contains the data for all examples generated according to procedure 2.

TABLE 2

Example 33: production of spray-dried particles

1200g of perfume particle slurry containing one or more of the variants of the microcapsules disclosed in this specification was mixed with 700g of water for 10 minutes at a speed of 180rpm using an IKA eurostat mixer with R1382 attachment. The mixture was then transferred to a feed vessel for spray drying in a Niro Production Minor of 1.2m diameter. The slurry was fed to the tower using a Watson-Marlow 504U peristaltic pump and atomized using a 100mm diameter rotary atomizer operating at 18000rpm, dried using co-current air flow. The slurry was dried to form a fine powder using an inlet temperature of 200 ℃ and an outlet temperature of 95 ℃. The equipment used for the spray drying process is available from the following suppliers: IKA Werke GmbH & co.kg, Janke and Kunkel-str.10, D79219 Staufen, germany; niro a/S Gladsaxevej 305, p.o. box 45, 2860Soeborg, denmark, and Watson-Marlow Bredel Pumps Limited, Falmouth, Cornwall, TR 114 RU, uk.

Example 34: encapsulated performance in liquid fabric enhancer products

To test the performance benefits of the encapsulates of the present invention, liquid fabric enhancer ("LFE") products were made. The LFE product contained 0.4% perfume oil added via the encapsulate. In this experiment, two types of encapsulates were tested: the encapsulates made according to example 2 of USPA 2008/0305982 (as comparative example) and the encapsulates made according to example 1 of the present application (as inventive example).

Each wash test contained ballast load and tracer. The loaded ballast fraction was 3kg and contained: 600g polyester, 600g polyester cotton, 600g muslin (muslin), 600g knitted cotton and 600g terry towel. The ballast load was pretreated according to the following conditions: 2X 70g Ariel Sensitive, 95 ℃ wash + 2X nil powder, 95 ℃ short cotton cloth wash. After each wash test, the ballast load was rewashed according to the following conditions: 2X 70g Ariel Sensitive, 95 ℃ wash + 2X nil powder, 95 ℃ short cotton cloth wash.

For each wash test, six loop tracers (Maes textile) were added to the load. The tracer was pretreated according to the following conditions: 2X 70g Ariel Sensitive, 95 ℃ wash + 2X nil powder, 95 ℃ short cotton cloth wash. The tracer is not reused.

Prior to each test, the washing machine was "boiled" (short cotton wash cycle at 95 ℃). The test conditions were as follows. The machine used was a Miele Novotronic W526 automatic washing machine. The load is placed into the washing machine. A50 g dose of Ariel Sensitive powder was added to the appropriate dispenser. A 35mL dose of the LFE product to be tested is added to the appropriate dispenser. The load was treated with a wash cycle according to the following conditions: the short cotton cloth is washed periodically at 60 ℃ and the rotating speed is 1200 rpm.

After treatment, loop tracers were evaluated by perfumers and ranked on Primavera scale. The tracer was evaluated at various "touch points" while wet (wet fabric odor, or "WFO") and after one day (dry fabric odor, or "DFO") of hanging dry (without rubbing the fabric). The encapsulates were also tested for perfume leakage in LFE products after one week of storage at 35 ℃. The results are shown in Table 3.

Table 3.

The data show that the odor performance of the wet fabric of the encapsulates according to the present application is improved without any loss of performance of the dry fabric when compared to the encapsulates of example 2 of USPA 2008/0305982 a 1. Example B also shows relatively less leakage than example a.

The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Rather, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as "40 mm" means "about 40 mm".

All documents cited in the detailed description of the invention are incorporated by reference herein in relevant part, and citation of any document is not to be construed as an admission that it is prior art with respect to the present invention. To the extent that any meaning or definition of a term herein conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term herein will prevail.

While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.