Use of microcapsules in laundry compositions for improving hand feel of fabrics
By using microcapsules of protein or polysaccharides in the laundry composition, the feel of the fabric is improved, the problems of complexity and high cost in the prior art are solved, and environmentally friendly requirements are met.
Patent Information
- Application Number
- CN202380043943.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Priority Date
- 2022-05-31
- Filing Date
- 2023-05-22
- Publication Date
- 2025-03-28
AI Technical Summary
Existing laundry compositions have problems with increasing complexity of formulations, high cost, and the use of ingredients that may not meet the environmental certificate when improving the feel of fabrics.
Microcapsules containing protein or polysaccharides are used as components of the laundry composition to improve the feel of the fabric by microcapsule wall materials such as protein polymers, polysaccharide polymers or combinations thereof.
By using microcapsules of protein or polysaccharides, the feel of the fabric is significantly improved, solving the problems of composition complexity and high cost in the prior art, while meeting environmentally friendly requirements.
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Abstract
Description
Technical Field
[0001] The present invention is in the field of laundry compositions, in particular laundry compositions for improving the feel of fabrics. Background Art
[0002] Fabric hand is a common assessment of fabrics in the laundry field. This measurement includes the sensory perception of the fabric by the consumer and combines measurements of fabric properties that the consumer associates with quality.
[0003] Various ingredients have been added to laundry products to improve the relative feel of fabrics. However, adding ingredients to laundry compositions has the disadvantages of increased formulation complexity, increased cost and ingredients that may not meet the environmental credentials desired by consumers.
[0004] Microcapsules are used in various laundry applications to deliver active materials to fabrics. Microcapsules are known to provide various benefits, such as delayed release of the active material or protection of the active material from other ingredients in the laundry composition. Conventional microcapsules typically have a microcapsule wall formed from a synthetic polymer such as a melamine formaldehyde polymer or a polyacrylate polymer. Summary of the invention
[0005] It has been found that the use of microcapsules comprising proteins or polysaccharides results in an improved fabric hand.
[0006] Therefore, in a first aspect of the present invention, there is provided a use of microcapsules in a laundry composition for improving the feel of fabrics, wherein the microcapsules have a microcapsule wall, and the microcapsule wall comprises a protein polymer, a polysaccharide polymer or a combination thereof. DETAILED DESCRIPTION OF THE INVENTION
[0008] By reading the following detailed description and the appended claims, these and other aspects, features and advantages will become clear to those of ordinary skill in the art. For the avoidance of doubt, any feature of one aspect of the present invention may be used for any other aspect of the present invention. The word "comprising" is intended to mean "including", but not necessarily "consisting of" or "consisting of". In other words, the steps or options listed do not have to be exhaustive. It should be noted that the examples given in the following description are intended to illustrate the present invention and are not intended to limit the present invention to those examples themselves. Similarly, unless otherwise indicated, all percentages are weight / weight percentages. Except in the operating examples and comparative examples, or in other clearly indicated places, all numbers indicating the amount or reaction conditions of the material, the physical properties of the material and / or the use in this specification should be understood to be modified by the word "about". The numerical range represented by the format "x to y" should be understood to include x and y. When multiple preferred ranges are described in the format "x to y" for a particular feature, it should be understood that all ranges combining different endpoints are also contemplated.
[0009] Laundry compositions are understood herein to mean consumer products suitable for use in a laundry process. Examples of such compositions include liquid laundry detergents, laundry detergent powders, fabric conditioners, auxiliary laundry compositions such as perfumers and fabric spray compositions.
[0010] A microcapsule composition is understood herein to mean a composition comprising microcapsules added to a laundry composition.The microcapsule composition may comprise microcapsules alone or may be in the form of a slurry comprising microcapsules.
[0011] Microcapsules are understood herein to mean microcapsules (wall and core), ie without solvent or slurry.
[0012] The laundry product of the present invention comprises microcapsules. The microcapsules can be provided simply as microcapsules, but are preferably provided as microcapsule compositions comprising microcapsules in a slurry. The microcapsules comprise a microcapsule core containing an active ingredient and a microcapsule wall encapsulating the core. The microcapsule wall comprises a wall polymer and preferably a crosslinking agent. Typically, the microcapsules comprise 10 to 98 wt % of a core material, 1 to 20 wt % of a wall polymer and optionally 0.2 to 6 wt % of a crosslinking agent.
[0013] The microcapsules can be prepared by any suitable method, including those exemplary methods described herein.
[0014] Microcapsule wall material
[0015] The microcapsule wall may also be referred to as a microcapsule shell. The microcapsule wall comprises a protein polymer, a polysaccharide polymer, or a combination thereof. The protein and / or polysaccharide may be treated by various methods to provide a derivative, including but not limited to hydrolysis, condensation, functionalization such as ethoxylation, cross-linking, etc. Without wishing to be bound by theory, it is believed that the use of protein or polysaccharide improves the "hand feel" of the fabric when treated with a composition comprising the microcapsules described herein. The microcapsule wall material is preferably in an aqueous solution. The microcapsule wall preferably comprises 20% to 100% by weight, more preferably 30% to 98% by weight, more preferably 35% to 95% by weight, and most preferably 65% to 90% by weight of protein, polysaccharide, or a combination thereof, based on the weight of the microcapsule wall.
[0016] As conventional in the art, a "polypeptide" or "protein" is a linear organic polymer consisting of amino acid residues bonded together in a chain, forming part (or all) of a protein molecule. As used herein, "polypeptide" or "protein" refers to a natural polypeptide, a polypeptide derivative and / or a modified polypeptide. A polypeptide may exhibit an average molecular weight of 1,000 Da to 40,000,000 Da, preferably greater than 10,000 Da, more preferably 100,000 Da, most preferably greater than 1,000,000 Da and preferably less than 3,000,000 Da.
[0017] Suitable proteins for the present invention include whey protein, vegetable protein and gelatin. Preferably, vegetable protein is used. Suitable preferred proteins include proteins selected from: pea, potato protein, brown rice, white rice, wheat, egg, barley, pumpkin seed, oat, almond, whey, casein, silk, gelatin, algae, rye, spelt, gluten, rapeseed, sunflower, corn, soybean, kidney bean, chickpea, lentil, lupine, peanut, alfalfa, protein produced by fermentation, protein from food residues and combinations thereof. Particularly preferred proteins include proteins selected from chickpea, pea protein, potato protein, brown rice protein, white rice protein, wheat protein, barley protein, pumpkin seed protein, oat protein, almond protein and combinations thereof. This includes derivatives of the above-mentioned proteins.
[0018] As used herein, "whey protein" refers to the protein contained in whey, a dairy liquid obtained as the supernatant of curd when milk or a dairy liquid containing milk components is processed into cheese curd to obtain semi-solid cheese curd. Whey protein is generally understood in principle to include globular proteins b-lactoglobulin and a-lactalbumin in various ratios such as 1:1 to 5:1 (e.g. 2:1). It may also include lower amounts of serum albumin, immunoglobulins and other globulins. The term whey protein is also intended to include partially or completely modified or denatured whey proteins. Purified b-lactoglobulin and / or a-lactalbumin polypeptides can also be used to prepare microcapsules of the present invention.
[0019] Gelatin refers to a mixture of proteins produced by partial hydrolysis of collagen extracted from the skin, bones and connective tissue of animals. Gelatin can be derived from any type of collagen, such as type I, II, III or IV collagen. Such proteins are characterized by including Gly-Xaa-Yaa triplets, where Gly is the amino acid glycine and Xaa and Yaa can be the same or different and can be any known amino acid. At least 40% of the amino acids are preferably present in the form of consecutive Gly-Xaa-Yaa triplets.
[0020] One preferred class of proteins is vegetable proteins. Vegetable proteins are proteins that accumulate in various plant tissues. Preferred vegetable proteins can be divided into two categories: seed or grain proteins and vegetable proteins. Seed / grain proteins are a group of proteins that accumulate to high levels in seeds / grains during the later stages of seed / grain development, while vegetable proteins are proteins that accumulate in vegetative tissues such as leaves, stems, and (depending on the plant species) tubers.
[0021] Preferred examples of seed / cereal / legume storage proteins are proteins from soy, lupin, pea, chickpea, alfalfa, faba bean, lentil and broad bean; oilseed plants such as rapeseed, cottonseed and sunflower; cereals such as wheat, corn, barley, malt, oats, rye and rice (e.g. brown rice protein) or combinations thereof.
[0022] Preferred examples of vegetable proteins are proteins from potato or sweet potato tubers.
[0023] The term vegetable protein is intended to include vegetable protein isolates, vegetable protein concentrates or combinations thereof. Vegetable protein isolates and concentrates are generally understood to be composed of several proteins. For example, pea protein isolates and concentrates may include legumin, pea globulin and convicin proteins. Similarly, brown rice protein isolates may include albumin, globulin and gluten proteins. The term "vegetable protein" is also intended to include partially or completely modified or denatured plant storage proteins. Individual polypeptides (e.g., legumin, pea globulin, convicin, albumin, globulin or gluten) may also be used to prepare microcapsules of the present invention.
[0024] Native proteins may be preferred. However, the method may include the step of denaturing the protein by pH adjustment, heating or adding a dispersing agent to the oil-in-water emulsion or the protein prior to addition to the oil-in-water emulsion.
[0025] Denaturation is the process by which a protein (polypeptide) loses its quaternary, tertiary, and secondary structures present in its native state by applying denaturing conditions. During denaturation, the protein changes its conformational structure by unfolding, thereby making amine and hydroxyl groups available for crosslinking (e.g., with polyisocyanates) to form the microcapsule wall. Exemplary conditions for protein denaturation include, but are not limited to, radiation, exposure to heat or cold, pH changes with acids or bases, exposure to denaturants such as detergents, inorganic salts, organic solvents (e.g., alcohols, ethyl acetate, and chloroform), urea or other dispersants, or mechanical stress including shear. Exemplary dispersing agents are guanidine salts (e.g., guanidine hydrochloride and guanidine carbonate), urea, polysorbate, sodium benzoate, vanillin, o-cresol, phenol, propanol, formamide, ethanol, fructose, ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium phosphate, potassium sulfate, potassium chloride, potassium iodide, potassium nitrate, potassium phosphate, sodium sulfate, sodium chloride, sodium bromide, sodium nitrate, sodium phosphate, guanidine thiocyanate, xylose, glycerol, benzyl alcohol, ethyl acetate, triton X-100, ethyl acetate, hexadecyl trimethyl ammonium halide, acetone, sodium dodecyl sulfate (SDS), hydrochloric acid, sulfuric acid, polyethylene glycol, glutaraldehyde, and combinations thereof. Any amount of dispersing agent can be used.
[0026] It may be preferred that the protein is denatured with a disintegrating agent such that 20 to 100 wt %, preferably 40 to 100 wt %, more preferably 60 to 100 wt %, most preferably 90 to 100 wt % of the protein used to prepare the microcapsules is denatured.
[0027] The proteins used in the microcapsules can also be derivatized or modified (e.g., derivatized or chemically modified). For example, the proteins can be modified by covalently attaching sugars, lipids, cofactors, peptides, or other chemical groups including phosphates, acetates, methyl groups, and other natural or non-natural molecules.
[0028] Polysaccharides are a class of carbohydrates containing multiple monosaccharide units. As used herein, "polysaccharide" refers to natural polysaccharides, polysaccharide derivatives and / or modified polysaccharides. Suitable polysaccharides can be selected from the group consisting of fiber, starch, sugar alcohol, sugar and mixtures thereof.
[0029] Examples of suitable fibers include: specific celluloses, cellulose derivatives such as hydroxyethylcellulose (especially quaternized hydroxyethylcellulose), carboxymethylcellulose (CMC) and microcrystalline cellulose (MCC), hemicelluloses, lichen, chitin, chitosan, lignin, xanthan gum, plant fibers, especially cereal fibers, potato fibers, apple fibers, citrus fibers, bamboo fibers, extracted beet fibers; oat fibers and soluble dietary fibers (especially inulin, especially natural inulin, highly soluble inulin, granulated inulin, high-performance inulin), pectin, alginates, agar, carrageenan, gum arabic (Senegal type, Seyal type), konjac gum, gellan gum, curdlan (paramylon), guar gum, locust bean gum, xanthan gum, raffinose, xylose, polydextrose and lactulose and combinations thereof. This includes derivatives of the above polysaccharides.
[0030] Examples of suitable starches include starches from wheat, potato, corn, rice, tapioca and oats, modified starches and starch derivatives, such as dextrins or maltodextrins (especially dextrins and maltodextrins from wheat, potato, corn, rice, peas, chickpeas and oats), oligosaccharides (especially oligofructose). Preferred starches are selected from the group consisting of corn starch, potato starch, rye starch, wheat starch, barley starch, oat starch, rice starch, pea starch, chickpea starch, tapioca starch and mixtures thereof.
[0031] Examples of suitable sugar alcohols include: sorbitol, mannitol, isomalt, maltitol, maltitol syrup, lactitol, xylitol, erythritol.
[0032] Examples of suitable sugars include: glucose.
[0033] Particularly preferred polysaccharides include: gum arabic, dextrin and maltodextrin are particularly preferred.
[0034] The polysaccharides used in the microcapsules can also be derivatized or modified (e.g., derivatized or chemically modified). For example, proteins can be modified by covalently attaching sugars, lipids, cofactors, peptides, or other chemical groups (including phosphates, acetates, methyl groups, and other natural or non-natural molecules). Examples of suitable polysaccharide derivatives include: glycolic acid starch, carboxymethyl starch, hydroxyalkyl cellulose, and cross-linked modified cellulose.
[0035] The microcapsules as described herein may optionally comprise additional polymers in the microcapsule wall. Such additional polymers may include: sol-gel polymers (e.g., silica), polyacrylates, polyacrylamides, poly(acrylate-co-acrylamides), polyureas, polyurethanes, starches, gelatin and gum arabic, poly(melamine-formaldehyde), poly(urea-formaldehyde), and combinations thereof. Preferably, however, the microcapsule wall polymer consists essentially of a protein, a polysaccharide, or a combination thereof.
[0036] The microcapsules preferably comprise 0.1 to 30 wt. % of microcapsule wall, preferably 0.5 to 25 wt. %, more preferably 1 to 20 wt. % and 2 to 15 wt. % of microcapsule wall, based on the weight of the microcapsule.
[0037] The microcapsule wall polymer described herein is preferably crosslinked. Suitable crosslinking methods include: isocyanate crosslinking, salt bridge crosslinking, and internal crosslinking within the microcapsule wall polymer structure (including the formation of coacervates). Where a crosslinking agent is used, such as a polyisocyanate crosslinking agent or an ionic crosslinking agent, the crosslinking agent is preferably present at a level of 0.1 wt % to 10 wt % based on the weight of the microcapsule, preferably 0.5 wt % to 9 wt % based on the weight of the microcapsule, and even more preferably 1 to 8 wt % based on the weight of the microcapsule.
[0038] One preferred crosslinking method is the use of polyisocyanates. Without wishing to be bound by theory, the choice of isocyanate crosslinking agent improves the softening of fabrics treated with the composition comprising the microcapsules.
[0039] The polyisocyanates each have at least two isocyanate (-NCO) groups reactive toward proteins or polysaccharides. The polyisocyanate may be aromatic, aliphatic, linear, branched or cyclic, preferably, the polyisocyanate comprises a polyisocyanate selected from aliphatic, alicyclic, hydrogenated aromatic, aromatic or heterocyclic polyisocyanates, their substitution products and mixtures thereof, most preferably a polyisocyanate selected from aromatic, aliphatic polyisocyanates and combinations thereof. It is particularly preferred that more than one polyisocyanate is present. The isocyanate may be water-soluble or water-dispersible, alternatively, it may be soluble in an organic solvent or aromatic oil. Preferably, the polyisocyanate is water-insoluble. Preferably, the polyisocyanate comprises 2 to 4 isocyanate groups. More preferably, the polyisocyanate comprises 3 to 4 isocyanate functional groups.
[0040] Examples of suitable polyisocyanates include trimer of hexamethylene diisocyanate, trimer of isophorone diisocyanate, biuret of hexamethylene diisocyanate, polyisocyanurate of toluene diisocyanate, trimethylolpropane adduct of toluene diisocyanate, trimethylolpropane adduct of xylylene diisocyanate, and combinations thereof.
[0041] Preferably, the polyisocyanate used in the present invention is an aromatic polyisocyanate. Preferably, the aromatic polyisocyanate includes a phenyl, tolyl, xylyl, naphthyl or diphenyl moiety as an aromatic component. Particularly preferably, the aromatic polyisocyanate is a polyisocyanurate of toluene diisocyanate, a trimethylolpropane adduct of toluene diisocyanate or a trimethylolpropane adduct of xylyl diisocyanate.
[0042] One class of suitable aromatic polyisocyanates are those having the general structure shown below and structural isomers thereof:
[0043]
[0044] Where n can vary from zero to a desired number (e.g., 0-50, 0-20, 0-10, and 0-6) depending on the type of crosslinking agent used. Preferably, the number of n is limited to less than 6. The starting polyisocyanate can also be a mixture of polyisocyanates, where the value of n can vary from 0 to 6. In the case where the starting polyisocyanate is a mixture of various polyisocyanates, the average value of n preferably falls between 0.5 and 1.5.
[0045] Commercially available polyisocyanates include products sold under the following trade names: M20 (chemical name: polymeric methylene diphenyl diisocyanate, i.e., "PMDI"; commercially available from BASF, containing 31.5% by weight of isocyanate groups "NCO"), wherein the average value n is 0.7; PAPI TM 27 (PMDI commercially available from Dow Chemical having an average molecular weight of 340 and containing 31.4 wt % NCO), wherein the average n is 0.7; MR (PMDI containing 31 wt % or more NCO, commercially available from Covestro, Pittsburg, Pennsylvania), wherein the average n is 0.8; MR Light (PMDI containing 31.8 wt. % NCO, commercially available from Covestro), where the average n is 0.8; 489 (PMDI containing 30 to 31.4 wt. % NCO commercially available from Covestro), wherein the average value n is 1; poly[(phenylisocyanate)-co-formaldehyde] (Aldrich Chemical, Milwaukee, WI), other isocyanate monomers, such as N3200 (poly(hexamethylene diisocyanate) commercially available from Covestro), and Takenate TMD110N (trimethylolpropane adduct of xylylenediisocyanate, Mitsui Chemicals America, Inc., Rye Brook, NY, containing 11.5 wt% NCO), L75 (a toluene diisocyanate-based polyisocyanate commercially available from Covestro) and IL (another polyisocyanate based on toluene diisocyanate commercially available from Covestro).
[0046] Another class of suitable polyisocyanates are diisocyanates having the general structure O=C=N—R—N=C=O, wherein R represents an aliphatic, alicyclic or aromatic group. Preferably, the group has five or more carbon atoms.
[0047] Other examples of aromatic polyisocyanates include 1,5-naphthylene diisocyanate, 4,4'-diphenylmethane diisocyanate (MDI), hydrogenated MDI, xylylene diisocyanate (XDI), tetramethylxylene diisocyanate, 4,4'-diphenyldimethylmethane diisocyanate, di- and tetraalkyl-diphenylmethane diisocyanates, 4,4'-dibenzyl diisocyanate, 1,3-phenylene diisocyanate, 1,4-phenylene diisocyanate, isomers of tolylene diisocyanate (TDI), 4,4'-diisocyanatophenyl-perfluoroethane, diisocyanatoethyl phthalate, and polyisocyanates having reactive halogen atoms, such as 1-chloromethylphenyl 2,4-diisocyanate, 1-bromomethylphenyl 2,6-diisocyanate and 3,3-bischloromethyl ether 4,4'-diphenyl diisocyanate, and combinations thereof.
[0048] The weight average molecular weight of the polyisocyanates that can be used is preferably from 200 Da to 2500 Da, more preferably from 250 Da to 1000 Da, most preferably from 275 Da to 500 Da.
[0049] The polyisocyanate is preferably present in the wall in an amount of 0.1 to 40 wt %, more preferably 0.2 to 25 wt %, even more preferably 0.25 to 15 wt %, and most preferably 0.5 to 5 wt % based on the weight of the microcapsule wall. Preferably, the ratio of polysaccharide and / or protein to polyisocyanate is from 1:1 to 10:1.
[0050] In the process of preparing the microcapsule composition of the present invention, the polyisocyanate may be added to the water phase, the oil phase or the oil-in-water emulsion.
[0051] Further examples of suitable polyisocyanates can be found in WO 2004 / 054362 and WO 2017 / 192648.
[0052] An alternative crosslinking agent suitable for use in the present invention is an ionic crosslinking agent. An ionic crosslinking agent is a multivalent ion capable of forming a salt bridge with a functional group of a protein or polysaccharide polymer. Without wishing to be bound by theory, it is believed that the use of an ionic crosslinking agent results in improved drape and elasticity of fabrics treated with a composition comprising microcapsules as described herein.
[0053] Suitable ionic crosslinking agents can be selected from: calcium cations, copper cations, aluminum cations, magnesium cations, strontium cations, barium cations, zinc cations, tin cations, organic cations, poly(amino acids), poly(ethylene imine), poly(ethylene amine), poly(allyl amine), polysaccharides, dicarboxylic acids, sulfate ions, carbonate ions, poly(acrylic acid), poly(methacrylic acid), copolymers of acrylic acid or methacrylic acid, sulfonated poly(styrene) and poly(styrene) with carboxylic acid groups and mixtures thereof. Particularly preferred are calcium salts, magnesium salts, sodium salts, potassium salts, strontium salts, barium salts, zinc salts.
[0054] Internal crosslinks are crosslinks between microcapsule wall polymers where no crosslinking agent is used. Internal crosslinks can be crosslinks with the same polymer (i.e., a polymer with a positive and negative charge) or between two different polymers forming the microcapsule wall. When two different polymers with opposite charges are used, this is referred to as a coacervate formed by coacervation.
[0055] Preferably, a coacervate is formed between a first protein or polysaccharide having one charge and a second protein or polysaccharide having the opposite charge. The ratio between the polymer having a positive charge and the polymer having a negative charge is preferably between 10 / 0.1 and 0.1 / 10, more preferably between 10 / 1 and 1 / 10, and most preferably between 6 / 1 and 1 / 6.
[0056] An example of a positively charged protein may be gelatin, and the negatively charged protein or polysaccharide may be selected from gum arabic, xanthan gum, alginates, pectinates, carrageenan, polyacrylic and methacrylic acids, xanthan gum and vegetable gums and mixtures thereof.
[0057] Internally crosslinked microcapsules, ie, microcapsules having electrostatic interactions between the positive and negative monomers within the microcapsule wall polymer, can be further crosslinked or "hardened" using salt bridges or isocyanates as described above.
[0058] The microcapsules may optionally contain an additional cross-linking agent. The additional cross-linking agent may be selected from the group consisting of transglutaminase, peroxidase, secondary plant substances selected from the group consisting of polyphenols (particularly tannins), gallic acid, ferulic acid, hesperidin, cinnamaldehyde, vanillin, carvacrol, and mixtures of two or more of the above cross-linking agents.
[0059] Microcapsule core material
[0060] The core may also be referred to as the internal phase. The core of the microcapsule comprises the active material and optionally further comprises a solvent, a cross-linking agent as described above, or a combination thereof. The core is preferably non-aqueous.
[0061] The inner non-aqueous phase may preferably comprise 20 to 80 wt. %, preferably 25 to 75 wt. %, even more preferably 33 to 50 wt. % of the active material to be encapsulated, and preferably 0.1 to 5 wt. %, preferably 0.15 to 3.5 wt. %, even more preferably 0.5 to 2.5 wt. % of the crosslinking agent and the remaining composition solvent.
[0062] Exemplary active materials include: fragrances; malodorants, such as: uncomplexed cyclodextrins, odor blockers, reactive aldehydes, flavonoids, zeolites, activated carbon and mixtures thereof; dye transfer inhibitors; hueing dyes; silicone oils, resins and modifications thereof, such as linear and cyclic polydimethylsiloxanes, amino-modified alkyl (allcyl), aryl and alkylaryl silicone oils, preferably having a viscosity greater than 50,000 cSt; insect repellents; organic sunscreen actives, such as octyl methoxycinnamate; antimicrobial agents, such as 2-hydroxy-4,2,4-trichlorodiphenyl ether; ester solvents, such as isopropyl myristate; lipids and lipid-like substances, such as cholesterol; hydrocarbons such as paraffin, petrolatum and mineral oil; fish oils and vegetable oils; hydrophobic plant extracts; waxes; pigments, including inorganic compounds having a hydrophobically modified surface and / or dispersed in an oil or hydrophobic liquid; sugar esters, such as sucrose polyesters (SPE); and combinations thereof.
[0063] The beneficial agent may be dissolved in a solvent. Examples of suitable solvents include vegetable oils, glycerides, esters of fatty acids and branched alcohols, hydrocarbons, and the like. Specific examples include: diethyl phthalate, isopropyl myristate, (rosin resin, available from Eastman), benzyl benzoate, ethyl citrate, limonene or other terpenes, triacetin or isoparaffins, preferably Benzyl benzoate, limonene or other terpenes, isoparaffins or combinations thereof. Preferably, if present, the solvent is 0 to 30% by weight of the active material, more preferably 0 to 20% by weight of the active material, most preferably 0 to 10% by weight of the active material.
[0064] Most preferably, the active material comprises a fragrance. Fragrance components are well known in the art. Available fragrance components may include materials of natural and synthetic origin. They include single compounds and mixtures. Specific examples of such components may be found in existing literature, for example, Fenaroli's Handbook of Flavor Ingredients, 1975, CRC Press; Synthetic Food Adjuncts, 1947 by MB Jacobs, edited by Van Nostrand; or Perfume and Flavor Chemicals by S. Arctander 1969, Montclair, NJ (USA). These substances are well known to those skilled in the art of flavoring, seasoning and / or aromatizing consumer products.
[0065] Particularly preferred perfume components are blooming perfume components and substantive perfume components. Blooming perfume components are defined by a boiling point below 250°C and a LogP greater than 2.5. Preferably, the encapsulated perfume composition comprises at least 20% by weight of blooming perfume ingredients, more preferably at least 30% by weight and most preferably at least 40% by weight of blooming perfume ingredients. Substantive perfume components are defined by a boiling point above 250°C and a LogP greater than 2.5. Preferably, the encapsulated perfume composition comprises at least 10% by weight of substantive perfume ingredients, more preferably at least 20% by weight and most preferably at least 30% by weight of substantive perfume ingredients. The boiling point is measured at standard pressure (760 mm Hg). Preferably, the perfume composition will comprise a mixture of blooming perfume components and substantive perfume components. The perfume composition may comprise other perfume components.
[0066] It is common for a variety of perfume components to be present in the microcapsules. In the compositions for use in the present invention, it is envisioned that three or more, preferably four or more, more preferably five or more, most preferably six or more different perfume components will be present in the microcapsules. An upper limit of 300 perfume components may be used.
[0067] Preferably, the amount of encapsulated active material is 5 to 95 wt%, preferably 10 to 90 wt%, more preferably 15 to 85 wt%, and most preferably 20 to 80 wt%, based on the weight of the microcapsule.
[0068] Additional microencapsulated ingredients
[0069] The microcapsule composition may include additional ingredients. Preferred additional ingredients are polyphenols. Particularly preferred are phenols having 3,4,5-trihydroxyphenyl or 3,4-dihydroxyphenyl groups, such as tannic acid. In addition to polyphenols, other polyols may also be used to prepare the microcapsule composition of the present invention. Examples include pentaerythritol, dipentaerythritol, glycerol, polyglycerol, ethylene glycol, polyethylene glycol, trimethylolpropane, neopentyl glycol, sorbitol, erythritol, threitol, arabitol, xylitol, ribitol, mannitol, galactitol, fucitol, iditol, inositol, heptyl alcohol, isomalt, maltitol, lactitol, maltotriitol, maltotetraitol, polyglycitol, polyphenols and combinations thereof.
[0070] The polyphenols, polyols and polyfunctional aldehydes are preferably present at levels of 0 to 40 wt%, preferably 1 to 35 wt%, more preferably 5 to 35 wt%, most preferably 10 to 30 wt%.
[0071] Microcapsule composition
[0072] The microcapsules described herein preferably have a diameter of 0.1 micrometer to 1000 micrometers, more preferably 0.5 micrometer to 500 micrometers, even more preferably 1 micrometer to 200 micrometers, and most preferably 1 micrometer to 100 micrometers.
[0073] The microcapsule can be positively charged or negatively charged, and the zeta potential is preferably -200mV to +200mV, more preferably 25mV to 200mV and most preferably 40mV to 100mV. Preferably, the microcapsule is positively charged. The zeta potential is a measure of the electrokinetic potential in the microcapsule. From a theoretical point of view, the zeta potential is the potential difference between the aqueous phase (i.e., the dispersion medium) and the stable layer of water attached to the surface of the microcapsule. The zeta potential can be calculated using a theoretical model and an electrophoretic mobility or a dynamic electrophoretic mobility determined by experiment. The zeta potential is usually measured by methods such as microelectrophoresis, or electrophoretic light scattering, or electroacoustic phenomena. For a more detailed discussion of measuring the zeta potential, see Dukhin and Goetz, "Ultrasound for characterizing colloids", Elsevier, 2002.
[0074] The microcapsule composition of the present invention may be a slurry containing a solvent (preferably water). The microcapsules are preferably present in the slurry at 0.1 wt % to 80 wt %, more preferably 1 wt % to 65 wt %, and most preferably 5 wt % to 45 wt %, based on the weight of the microcapsule composition. The slurry may contain a thickener or suspending agent, such as xanthan gum, carboxymethyl cellulose (CMC), microcrystalline cellulose (MCC) or guar gum.
[0075] Alternatively, the microcapsule composition of the present invention may also be dried (eg, spray-dried, heat-dried, and belt-dried) into a solid form.
[0076] The microcapsule composition can be purified by washing the capsule slurry with water until a neutral pH (pH 6 to 8) is reached. For the purposes of the present invention, the capsule suspension can be washed using any conventional method, including using a separatory funnel, filter paper, centrifugation, etc. The capsule suspension can be washed once, twice, three times, four times, five times, six times or more times until a neutral pH, such as pH 6-8 and 6.5-7.5, is reached. The pH of the purified capsule can be measured using any conventional method (including but not limited to pH paper, pH indicator or pH meter). In certain embodiments of the present invention, the purification of the capsule includes an additional step of adding a salt to the capsule suspension before the step of washing the capsule suspension with water. Exemplary salts used in this step of the present invention include but are not limited to sodium chloride, potassium chloride or bisulfite. See US2014 / 0017287.
[0077] Preparation of microcapsules
[0078] When preparing the microcapsules, the polymer may be provided in a solvent. Suitable solvents for preparing the microcapsule wall include water or a mixture of water and at least one water-miscible organic solvent. Suitable organic solvents include glycerol, 1,2-propylene glycol, 1,3-propylene glycol, ethylene glycol, diethylene glycol, triethylene glycol and other similar. Preferably, the solvent is water.
[0079] A stabilizer may also be present. The stabilizer may be selected from acrylic copolymers (preferably with sulfonate groups), copolymers of acrylamide and acrylic acid, copolymers of alkyl acrylates and N-vinyl pyrrolidone, for example K15, K30 or K90 (BASF); sodium polycarboxylate, sodium polystyrene sulfonate, vinyl and methyl vinyl ether-maleic anhydride copolymers and ethylene, isobutylene or styrene-maleic anhydride copolymers, microcrystalline cellulose (which can be obtained, for example, under the name commercially available), diutan gum, xanthan gum or carboxymethyl cellulose.
[0080] The crosslinking of the microcapsules preferably involves a catalyst. The catalyst may be present in the microcapsule core active material or added separately to the oil-in-water emulsion or dispersion. A preferred catalyst for forming the microcapsules according to the invention is diazabicyclo[2.2.2]octane (DABCO), also known as triethylenediamine (TEDA). Also suitable are bismuth- or tin-based catalysts, transglutaminases, peroxidases, secondary plant compounds selected from the group consisting of polyphenols (particularly tannins), gallic acid, ferulic acid, hesperidin, cinnamaldehyde, vanillin, carvacrol, and mixtures thereof.
[0081] Alternatively or additionally, the formation of the microcapsules may be catalysed by heating the oil-in-water emulsion or dispersion, for example, to a temperature in the range of 60°C to 90°C.
[0082] Various suitable production methods can be implemented to produce microcapsules suitable for use in the present invention.
[0083] One suitable method is interfacial polymerization. An example of interfacial polymerization involves the following steps:
[0084] (i) providing a microcapsule core material comprising at least one first crosslinking agent, wherein the crosslinking agent is substantially dissolved with the core material. This is the oil phase. A non-aqueous solvent may optionally be present;
[0085] (ii) providing a microcapsule wall material comprising at least one protein, polysaccharide or combination thereof. This is the aqueous phase. An aqueous solvent may optionally be present;
[0086] (iii) emulsifying or dispersing the microcapsule core material with the microcapsule wall material. Preferably in a ratio in the range of 70:30 to 60:40, preferably in the range of 30:70 to 60:40. Optionally, an emulsifier may be used. Emulsification may be achieved by using high speed mixing. After completion of this stage, there is an oil-in-water emulsion or dispersion in which the inner phase with the active material to be encapsulated is finely emulsified or dispersed in the outer wall material phase in the form of droplets;
[0087] (iv) a first crosslinking, optionally by adding at least one catalyst to obtain a microcapsule slurry, optionally adding additional protein polymers, polysaccharide polymers or a combination thereof;
[0088] (v) curing the microcapsule slurry, preferably at a temperature of at least 60° C., preferably for at least 30 minutes, followed by cooling;
[0089] (vi) optionally drying using methods such as spray drying, filtration or freeze drying.
[0090] An alternative approach involves 3D printing microcapsules. Both the microcapsule shell and the microcapsule core can be printed using a printing system. See WO 2016 / 172699 A1. The printing step typically involves depositing the active material and the microcapsule shell material in a layer-by-layer manner, preferably by separate print heads.
[0091] Laundry composition
[0092] The composition of the present invention comprises from 0.05 to 20 wt% microcapsules by weight of the composition, more preferably from 0.075 to 10 wt% microcapsules, most preferably from 0.1 to 6 wt% microcapsules.
[0093] The laundry composition described herein can be any suitable laundry composition. The composition can be selected from: liquid detergents, powder detergents, fabric conditioners, auxiliary compositions such as liquid fragrance enhancers or perfume beads, and fabric sprays. Preferably, the composition is a fabric conditioner, an auxiliary composition, or a fabric spray. More preferably, the composition is a fabric conditioner.
[0094] Liquid and powder detergents are cleaning compositions intended for the washing stage of a laundry process. The detergent comprises anionic and / or nonionic surfactants for cleaning fabrics. Preferably, the liquid detergent comprises at least 3%, preferably 5 to 60%, and more preferably 6 to 50% (by weight based on the total weight of the composition) of one or more anionic and / or nonionic surfactants. Preferred anionic surfactants include: alkylbenzene sulfonates, preferably linear alkylbenzene sulfonates (LAS); alkyl ethers, preferably sulfate sodium lauryl ether sulfate (SLES); alkyl sulfate surfactants, preferably primary alkyl sulfates (sulfanant) (PAS). Particularly preferred anionic surfactants are selected from: linear alkylbenzene sulfonates, sodium lauryl ether sulfonates with 1 to 3 moles (average) of ethoxylation, primary alkyl sulfonates, methyl ether sulfates and secondary alkyl sulfonates or mixtures thereof. Preferred nonionic surfactants are polyoxyalkylene compounds. Particularly preferred nonionic surfactants are selected from: C8 to C22 alkylphenol ethoxylates having an average of 5 to 25 moles of ethylene oxide per mole of alkylphenol; and C8 to C18 aliphatic alcohol ethoxylates having an average of 2 to 40 moles of ethylene oxide per mole of alcohol.
[0095] The detergent may further comprise: co-surfactants other than anionic and / or nonionic surfactants such as amphoteric (zwitterionic) and / or cationic surfactants; builders such as hydroxides, carbonates, silicates, zeolites and mixtures thereof; fatty acids such as aliphatic carboxylic acids; dye transfer inhibitors; anti-redeposition polymers; soil release polymers; transition metal chelators; hydrotropes; hueing dyes; fluorescent agents; enzymes; and combinations thereof.
[0096] Fabric conditioners are compositions used in the rinse stage of a laundry process. Fabric conditioners contain fabric softening actives. Fabric softening actives may be selected from: quaternary ammonium compounds, silicone polymers, polysaccharides, clays, amines, fatty esters, dispersible polyolefins, polymer latexes and mixtures thereof. Preferably, the fabric softening active is a quaternary ammonium compound, preferably an ester-linked quaternary ammonium compound, such as an ester-linked triethanolamine (TEA) quaternary ammonium compound or diethyl dialkyl ester dimethyl ammonium chloride.
[0097] The fabric conditioner may further comprise: nonionic surfactants; co-softeners such as fatty esters and fatty alcohols; cationic polymers; rheology modifiers; and combinations thereof.
[0098] Auxiliary compositions are compositions intended to be used in addition to detergent or fabric conditioner compositions. Auxiliary compositions deliver additional benefit agents during the laundry process. As separate products, these compositions allow consumers to customize benefit agents to suit the laundry load and their personal preferences. Auxiliary laundry compositions can be liquid or solid.
[0099] The liquid auxiliary laundry composition comprises a liquid carrier, preferably water, and the microcapsules described herein.The liquid auxiliary laundry composition may preferably comprise ingredients such as: nonionic surfactants, emulsifiers, rheology modifiers, unencapsulated benefit agents.
[0100] The solid auxiliary laundry composition comprises a solid carrier. The carrier material may be selected from the group consisting of synthetic polymers (e.g., polyethylene glycol, ethylene oxide / propylene oxide block copolymers, polyvinyl alcohol, polyvinyl acetate and derivatives thereof), proteins (e.g., gelatin, albumin, casein), carbohydrates (e.g., dextrose, fructose, galactose, glucose, isoglucose, sucrose), polysaccharides (e.g., starch, xanthan gum, cellulose or derivatives thereof), water-soluble or water-dispersible fillers (e.g., sodium chloride, sodium sulfate, sodium carbonate / bicarbonate, zeolite, silica, clay), vegetable soaps (e.g., coconut soap beads or palm soap), ethoxylated nonionic surfactants (having the formula R1O(R2O)xH, wherein R1 preferably contains 12 to 20 carbon atoms, R2 is C2H4 or a mixture of C2H4 and C3H6 units, and x=8 to 120), urea and combinations thereof. Preferred carrier materials may be selected from the group consisting of synthetic polymers (e.g., polyethylene glycol, ethylene oxide / propylene oxide block copolymers, polyvinyl alcohol, polyvinyl acetate and derivatives thereof), polysaccharides (e.g., starch, xanthan gum, cellulose or derivatives thereof), sugars (e.g., dextrose, fructose, galactose, glucose, isoglucose, sucrose), vegetable soaps (e.g., coconut soap beads or palm soap), ethoxylated nonionic surfactants (having the formula R1O(R2O)xH, wherein R1 preferably contains 12 to 20 carbon atoms, R2 is C2H4 or a mixture of C2H4 and C3H6 units, and x=8 to 120) and combinations thereof. The solid auxiliary composition may preferably contain ingredients such as: unencapsulated benefit agents and dyes.
[0101] Fabric sprays are compositions suitable for spraying onto fabrics. The sprays comprise a liquid carrier, preferably water, and the microcapsules described herein. The spray compositions may preferably comprise ingredients such as nonionic surfactants, unencapsulated benefit agents, lubricants, structured polymers, anti-malodor ingredients, and combinations thereof.
[0102] The laundry compositions described herein preferably comprise 0.01 to 20 wt% perfume microcapsules, more preferably 0.05 to 15 wt% perfume microcapsules, more preferably 0.1 to 10 wt% perfume microcapsules, more preferably 0.5 to 8 wt% perfume microcapsules, based on the weight of the laundry composition.
[0103] In addition to the microcapsules described herein, the laundry compositions described herein preferably comprise free perfume. The composition preferably comprises from 0.1 to 15 wt% free perfume, more preferably from 0.5 to 8 wt% free perfume.
[0104] Particularly preferred perfume components are aroma-releasing perfume components and substantial perfume components. Aroma-releasing perfume components are defined by a boiling point below 250°C and a LogP greater than 2.5. Substantial perfume components are defined by a boiling point above 250°C and a LogP greater than 2.5. The boiling point is measured at standard pressure (760 mm Hg). Preferably, the perfume composition will contain a mixture of aroma-releasing perfume components and substantial perfume components. The perfume composition may contain other perfume components.
[0105] It is common for a variety of fragrance components to be present in free oil fragrance compositions. In compositions for use in the present invention, it is envisaged that three or more, preferably four or more, more preferably five or more, most preferably six or more different fragrance components will be present. An upper limit of 300 fragrance components may be used.
[0106] The laundry composition may further comprise other ingredients of laundry compositions as known to those skilled in the art. Among such materials, mention may be made of: defoamers, insect repellents, sunscreen or hueing dyes, preservatives (e.g., bactericides), pH buffers, hydrotropes, anti-redeposition agents, detergents, polyelectrolytes, anti-shrinkage agents, anti-wrinkle agents, antioxidants, dyes, colorants, sunscreens, corrosion inhibitors, drape-imparting agents, antistatic agents, chelating agents, pearlescent agents, sunscreens and ironing aids.
[0107] Use of the composition
[0108] The microcapsules in the composition described herein are used to improve the hand feel of fabrics. The composition is applied to fabrics during the laundry process and an improved hand feel of fabrics is achieved. Fabric hand feel is defined as the estimated quality of a fabric evaluated when a consumer touches the fabric. Important components of fabric hand feel include the smoothness, compressibility, and elasticity of a textile sample. The improvement in fabric hand feel can be measured using AATCC TM202-2012 (2020), Relative Hand Value of Textiles: Instrumental Method. A suitable machine for measuring relative hand value is supplied by NuCybertek, Inc. DETAILED DESCRIPTION
[0109] Example
[0110] Preparation of microcapsules
[0111] The following microcapsules were used to evaluate the effects of the compositions described herein:
[0112] Microcapsule A – Melamine formaldehyde microcapsules
[0113] Microcapsule 1 – pea protein and sodium alginate mixture with salt cross-linking
[0114] Microcapsule 2 – pea protein and cross-linked with polyisocyanate (poly[(phenylisocyanate-co-formaldehyde])
[0115] The same model fragrance composition was used in all microcapsules.
[0116] Microcapsules A were prepared by dispersing formalin in water and adjusting the pH to 9. Melamine and 0.28 g of sodium chloride were added. The mixture was heated to ~65°C for 1 hour. Additional water was added and the solution was heated to ~75°C. The pH was adjusted to 4. The fragrance was then added under homogenization. Heating and stirring were continued for 3 hours. The mixture was then cooled and the pH was adjusted to 7.
[0117] Table 1: Microcapsule A composition
[0118]
[0119] Microcapsules 1 were prepared as follows: A 10% w / v pea protein solution was prepared in deionized water and the pH was adjusted to pH 9 using a few drops of sodium carbonate solution. This was heated to 85°C and mixed on a tornado mixer at 300 rpm for 2 hours. After 2 hours, the pH was lowered to pH 7 using a few drops of 2M HCl solution and 1.5 g of sodium alginate was added.
[0120] It was further mixed at 300 rpm for 90 minutes until homogeneous and then left overnight to cool. Once cooled the next day, 22.5 g of fragrance oil was added and mixed at 300 rpm for 1 hour. The prepolymer mixture was then added to 80 ml of a solution containing different concentrations of Tween 80, calcium chloride and DI water. The solution was homogenized to produce a suspension.
[0121] Table 2: Microcapsule 1 composition
[0122]
[0123] Microcapsule 2 was prepared as follows: First, an oil phase was prepared by mixing 23.2 g of model fragrance and 4.8 g of caprylic / capric triglyceride, 0.38 g of benzyl benzoate, and 0.38 g of aromatic polyisocyanate. In a separate beaker, an aqueous solution was obtained by mixing 1.182 g of pea protein isolate in 170 g of water. The oil phase was then emulsified into the water phase using an ultra turrax mixer at a shear rate of 5000 revolutions per minute (RPM) to form an oil-in-water emulsion. The oil-in-water emulsion was then cured at 55° C. for 2 hours.
[0124] Table 3: Microcapsule 2 composition
[0125]
[0126] Preparation of fabric conditioner
[0127] Table 4: Fabric Conditioner Composition
[0128]
[0129] Fabric softening actives 1 ——Dialkoxyethyl hydroxyethyl methyl ammonium methyl sulfate
[0130] The fabric conditioner is prepared by melting the fabric softening active at ~65°C. The water is heated to ~40°C. The trace materials and the fabric softening active are added under stirring. The water is then cooled slightly. The composition is then cooled to room temperature. The perfume microcapsules are then added to the composition. The 2 wt% is based on the weight of the microcapsules.
[0131] Washing method
[0132] Washing was performed in a Terg-O-Tometer jar. 0.5 ml of the test fabric conditioner composition and 1 L of water were added to the Tergo jar followed by 40 g of knitted cotton. The test monitor was rinsed in the liquid for 10 minutes and spun for 30 seconds. The fabric was then hung to dry under ambient conditions.
[0133] analyze
[0134] The properties of the fabrics were evaluated using a Phabrometer from NUCybertek*. 11.3 cm discs were cut from the test fabrics. Fabric measurements were performed using the Phabrometer and according to AATCC Standard TM202. Ten replicates were measured for each fabric and the results were averaged.
[0135] Table 5: Results
[0136] Microcapsule Type Relative feel value Microcapsule A 1.4682 Microcapsule 1 1.9391 Microcapsule 2 1.5633
[0137] A higher score indicates an improved relative hand value.Compared to conventional melamine formaldehyde microcapsules, the microcapsules according to the present invention provide an improved relative hand value.
Claims
1. Use of microcapsules in laundry compositions for improving the feel of fabrics, wherein the microcapsules have microcapsule walls, and the microcapsule walls comprise protein polymers, polysaccharide polymers or a combination thereof.
2. The use according to claim 1, wherein the microcapsules encapsulate a fabric benefit agent.
3. Use according to any one of the preceding claims, wherein the microcapsules encapsulate a fabric benefit agent comprising a perfume.
4. Use according to any one of the preceding claims, wherein the laundry composition comprises 0.05 to 20 wt% of microcapsules.
5. Use according to any one of the preceding claims, wherein the laundry composition is selected from the group consisting of liquid laundry detergents, powder laundry detergents, fabric conditioners, auxiliary laundry compositions and fabric sprays.
6. Use according to any one of the preceding claims, wherein the laundry composition is a fabric conditioner composition.
7. Use according to any of the preceding claims, wherein the microcapsule wall comprises 20% to 100% by weight of protein, polysaccharide or a combination thereof, based on the weight of the microcapsule.
8. The use according to any of the preceding claims, wherein the microcapsule wall comprises a protein selected from the group consisting of pea, potato protein, brown rice, white rice, wheat, egg, barley, pumpkin seeds, oats, almonds, whey, casein, silk, gelatin, algae, rye, spelt, gluten, rapeseed, sunflower, corn, soy, bean, chickpea, lentil, lupin, peanut, alfalfa, chitosan, protein produced by fermentation, protein from food waste and combinations thereof.
9. Use according to any one of the preceding claims, wherein the microcapsule wall comprises a polysaccharide selected from the group consisting of fibers, starches, sugar alcohols, sugars and mixtures thereof.
10. The use according to any one of the preceding claims, wherein the microcapsules are crosslinked.
11. The use according to claim 10, wherein the microcapsule crosslinking agent is selected from the group consisting of isocyanate crosslinking, salt bridge crosslinking, internal crosslinking and combinations thereof.
12. Use according to claim 10 or 11, wherein the microcapsules comprise from 0.1% to 10% by weight of a crosslinking agent, based on the weight of the microcapsules.
Citation Information
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