Compositions containing microcapsules for solid consumer products
Patent Information
- Application Number
- JP2024547561
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2022-02-11
- Publication Date
- 2025-02-28
Smart Images

Figure 2025505727000001_ABST
Abstract
Description
[Technical field]
[0001] The present invention relates to the field of fragrance particles, especially for solid consumer product formulations such as fabric care products. More specifically, the present invention relates to a composition comprising or consisting of at least one pastille, the pastille comprising or consisting of at least one microcapsule and a polymer matrix in which at least one microcapsule is embedded. The present invention also relates to a composition further comprising or consisting of at least one adhesive in said matrix. The present invention also relates to a method for producing such a composition, the use of the composition for the production of a consumer product, and a consumer product comprising or consisting of the composition. [Background technology]
[0002] Today, many consumer products, such as detergents, fabric softeners, soap powders, deodorants, lotions, etc., are scented with fragrance ingredients or contain cosmetic ingredients to provide certain benefits.
[0003] However, in many cases, for example, fragrances and cosmetic ingredients of such products tend to interact with other components of the product formulation, and many volatile components of fragrance formulations tend to evaporate early. This can result in undesirable changes and / or deterioration of the fragrance impression, or the cosmetic ingredients can be "consumed" too quickly over time, or can react unfavorably with other components of the product formulation, which can impair the quality and / or stability of the product. In order to prevent possible interactions between active ingredients, such as perfumes, and other components of the product, and to prevent, for example, the evaporation of the perfume, which would distort or reduce the desired olfactory impression, it is possible to add active ingredients, such as perfumes, to the formulation in encapsulated form. In this way, for example, the desired olfactory impression can be guaranteed, based on a targeted release of the active ingredients. Furthermore, the interactions between the product components can be reduced, which can increase the quality and storage stability of the product.
[0004] Thus, a wide variety of consumer products contain active ingredients, such as encapsulated fragrances, in their formulations. For example, fabric care formulations, such as liquid detergents and fabric softeners, contain a number of such fragrance microcapsules. Furthermore, these formulations require the addition of preservatives, such as methylisothiazolinone (MIT), to enhance their stability and persistence, which can cause allergic reactions and skin irritation. Powder detergents, on the other hand, do not require the addition of preservatives, reducing environmental pollution. However, the incorporation of microcapsules into powder formulations is quite disadvantageous, since the mixing of the microcapsule ingredients with other detergent ingredients can break the fragile microcapsules, compromising, for example, the olfactory performance. It is particularly difficult to produce microcapsules that have both good stability and good release characteristics. The ability of the capsules to retain the active ingredients and prevent the loss of volatile ingredients is particularly dependent on the stability of the capsules in the product. However, very stable microcapsules, e.g., those with thick capsule walls, usually tend to perform poorly, since the breakdown of the microcapsules and the associated release of the active ingredient(s) is hindered. However, if they are too unstable, they will collapse during storage, resulting in leakage of the active ingredient and failure to perform.Thus, if the capsule wall is made thicker, i.e., using multiple microcapsule shells or thicker shells, the targeted release of the active ingredient will be reduced, and thus the performance will be reduced as well.In addition, such microcapsules usually require complex multi-step manufacturing processes.
[0005] Furthermore, in view of the growing social awareness of ecology (reduction of waste, reduction of preservatives, etc.), there is a growing new trend for solid consumer products such as solid hair care products, soap, solid body wash, etc., so that solid consumer products will become increasingly important not only in the cosmetics industry but also in other fields.
[0006] As a result, there is a need to more efficiently incorporate active ingredients, such as fragrance ingredients, into solid consumer product formulations while at the same time providing for efficient, targeted release of these active ingredients.
[0007] The present invention has been made in consideration of the above-mentioned shortcomings. To solve the above-mentioned shortcomings, the present invention provides a composition and a method for its preparation, which allows for efficient incorporation of active ingredients into solid consumer product formulations in consumer product manufacturers.
[0008] In a first aspect, the present invention relates to a composition comprising or consisting of at least one pastille, said pastille comprising (based on the total weight of the pastille): (a) at least one microcapsule containing 0.5 to 10% by weight of an active ingredient, the active ingredient being preferably a fragrance or a mixture of fragrances; (b) 92 to 98% by weight of a polymer, preferably a polyethylene glycol; It comprises or consists of:
[0009] In a preferred embodiment of the composition, the polymer is preferably polyethylene glycol.
[0010] According to a second aspect, the present invention relates to a composition comprising or consisting of at least one pastille, said pastille having (based on the total weight of the pastille): (a) at least one microcapsule containing 0.5 to 10% by weight of an active ingredient, the active ingredient being preferably a fragrance or a mixture of fragrances; (b) 60 to 80% by weight of at least one polymer, preferably a polyethylene glycol; (c) 2-32 wt. % of at least one adhesive, preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; It comprises or consists of:
[0011] In a preferred embodiment of said composition, the polymer is preferably polyethylene glycol and the adhesive is selected from the group consisting of animal and / or vegetable waxes, preferably beeswax.
[0012] According to a third aspect, the present invention relates to a method for the manufacture of a composition comprising or consisting of a plurality of pastilles, the method comprising the steps of: (i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule; (ii) melting at least one polymer and, optionally, an adhesive; (iii) mixing said at least one microcapsule into the polymer melt of step (ii); (iv) forming a pastille by dropwise addition of the mixture of step (iii); (v) optionally cooling; Including, Optionally, the method further comprises the step of adding at least one plasticizer and / or structurant during or after step (ii) or (iii).
[0013] Additionally, in another aspect, the present invention relates to compositions produced by the methods of the present invention.
[0014] Finally, the present invention relates to the use of the composition according to the invention for the manufacture of consumer products and consumer product formulations, and to consumer products and consumer product formulations comprising or consisting of the composition according to the invention.
[0015] That is, the inventors have found that the composition according to the invention allows the active ingredient to be efficiently incorporated into a wide range of solid consumer product formulations and solid consumer products in an encapsulated form that exhibits excellent release properties. The polymer matrix acts as a buffer and protects the fragile microcapsules from mechanical, chemical and / or thermal influences during the manufacture of the final consumer product without adversely affecting the performance of the microcapsules in the consumer product. On this basis, the dosage form overcomes the drawbacks of the known art, since it allows the efficient incorporation of the active ingredient via the microcapsules into the solid consumer product formulation and at the same time allows the efficient and targeted release of the active ingredient. The fragile microcapsules are embedded in a protective matrix that is resistant to harsh chemical and physical conditions, such as elevated temperatures and acidic or basic conditions.
[0016] The problem is solved by the subject matter of the independent patent claims. Preferred embodiments are evident from the wording of the dependent patent claims and from the following description.
[0017] Unless otherwise noted, all percentages are expressed by weight. Numerical examples stated in the form "x to y" are inclusive of the stated values. When multiple preferred numerical ranges are expressed in this form, all ranges combining the various endpoints are also included.
[0018] As used herein, the term "at least one" or "one or more" refers to one or more, for example, 2, 3, 4, 5, 6, 7, 8, 9 or more.
[0019] The term "and / or" denotes a conjunctive or alternative. [Brief description of the drawings]
[0020] [Figure 1] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of laundry soap samples with samples comprising a composition according to the present invention containing melamine-formaldehyde based core-shell microcapsules and polyethylene glycol.
[0021] [Diagram 2] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of laundry soap samples with samples comprising a composition according to the present invention containing melamine-formaldehyde based core-shell microcapsules, polyethylene glycol, and beeswax.
[0022] [Diagram 3] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of a sample in tablet form with a sample comprising a composition according to the invention containing melamine-formaldehyde based core-shell microcapsules and polyethylene glycol.
[0023] [Figure 4] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of a sample in tablet form with a sample comprising a composition according to the invention containing melamine-formaldehyde based core-shell microcapsules, polyethylene glycol and beeswax.
[0024] [Diagram 5] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of powder detergent samples with samples comprising a composition according to the invention containing melamine-formaldehyde based core-shell microcapsules and polyethylene glycol.
[0025] [Figure 6] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of powder detergent samples with samples comprising a composition according to the present invention containing melamine-formaldehyde based core-shell microcapsules, polyethylene glycol and beeswax.
[0026] [Figure 7] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of laundry soap samples with samples comprising a composition according to the present invention containing biodegradable core-shell microcapsules and polyethylene glycol.
[0027] [Figure 8] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of laundry soap samples with samples comprising a composition according to the present invention containing biodegradable core-shell microcapsules, polyethylene glycol, and beeswax.
[0028] [Figure 9] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of powder detergent samples with samples comprising a composition according to the invention containing isocyanate-based core-shell microcapsules and polyethylene glycol.
[0029] [Figure 10] FIG. 1 shows the results of a sensory evaluation comparing the performance (release profile) of powder detergent samples with samples comprising a composition according to the present invention containing isocyanate-based core-shell microcapsules, polyethylene glycol and beeswax.
[0030] [Figure 11] Figures 11A (left) and 11B (right) show the uniform distribution of 2 mm particle size pastilles according to the present invention in a bar of laundry soap, as well as the pastilles themselves. The size of the pastilles was 3.3 cm.
[0031] [Figure 12] Figures 12A (left) and 12B (right) show the non-uniform distribution of 5 mm particle size pastilles according to the present invention in a bar of laundry soap, as well as the pastilles themselves. The size of the tablets was 3.3 cm.
[0032] [Figure 13] Figures 13A (left) and 13B (right) show examples of pastilles made from the composition of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0033] The present invention will now be described in more detail.
[0034] In a first aspect, the present invention relates to a composition comprising or consisting of at least one pastille, said pastille comprising: (a) 0.5 to 10% by weight, based on the total weight of the pastille, of at least one microcapsule encapsulating an active ingredient, the active ingredient being preferably a flavor or a flavor mixture; (b) 92 to 98% by weight of a polymer, preferably a polyethylene glycol (PEG), based on the total weight of the pastille; It comprises or consists of:
[0035] Optionally, in a further preferred embodiment, the pastille of the composition according to the first aspect further comprises: (c) 0.5 to 10% by weight of at least one plasticizer, preferably water or polyethylene glycol, based on the total weight of the pastille. It comprises or consists of.
[0036] In a second aspect, the present invention relates to a composition comprising or consisting of at least one pastille, said pastille comprising: (a) 0.5 to 10% by weight, based on the total weight of the pastille, of at least one microcapsule encapsulating an active ingredient, the active ingredient being preferably a flavor or a flavor mixture; (b) 60 to 80% by weight of at least one polymer, preferably a polyethylene glycol, based on the total weight of the pastille; (c) 2 to 32% by weight of at least one adhesive, based on the total weight of the pastille, preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; It comprises or consists of:
[0037] According to a further preferred embodiment, the pastille of the composition according to the second form further optionally comprises (d) 0.5 to 10% by weight, based on the total weight of the pastille, of at least one plasticizer, preferably water or polyethylene glycol; and / or (f) 0.1% to 10% by weight of a structuring agent, based on the total weight of the pastille, preferably selected from the group consisting of an ester such as isopropyl myristate, or another emulsifier. It comprises or consists of:
[0038] Microcapsules and active ingredients
[0039] Microcapsules are particles that have a core and a wall material surrounding the core. The core may be a solid, liquid, or gaseous substance, or a mixture of these, surrounded by a dense, permeable or semi-permeable wall material of a polymer. The wall is usually formed by emulsification and precipitation of a polymer by coacervation or interfacial polymerization. The core is also called the internal phase. The wall is also called the external phase, shell, or coating. The shell wall may include one or more layers and may include another coating of a coating material. The diameter of a microcapsule typically ranges from 1 to 1,000 μm. The wall thickness is typically 0.5 to 150 μm, but can be as small as 5 × 10 -9 m~5×10 -6 The amount of the core material is typically 25 to 95% by weight, but may be 1 to 99% by weight.
[0040] For example, hydrophobic active ingredients such as perfumes and fragrances can be readily incorporated into a wide variety of application formulations through encapsulation.
[0041] Based on their properties, microcapsules are used in the printing industry, food industry (vitamins, flavorings, plant extracts, enzymes, microorganisms), agrochemicals (fertilizers, pesticides), feed industry (minerals, vitamins, enzymes, drugs, microorganisms), pharmaceutical industry, detergent industry, cosmetics industry, etc.
[0042] A wide variety of capsule wall and coating materials are known for the production of microcapsules. The capsule wall may be formed of natural, semi-synthetic or synthetic materials. Natural shell materials include gum arabic, agar, agarose, maltodextrin, alginic acid and its salts, such as sodium alginate and calcium alginate, lipids and fatty acids, cetyl alcohol, collagen, chitosan, lecithin, gelatin, albumin, shellac, polysaccharides such as starch and dextran, polypeptides, protein hydrolysates, sucrose and waxes. Semi-synthetic capsule wall materials include chemically modified celluloses, especially cellulose esters and cellulose ethers, such as cellulose acetate, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose and carboxymethyl cellulose, as well as starch derivatives, especially starch ethers and starch esters. Synthetic shell materials are polymers, such as polyacrylates, polyamides, polyvinyl alcohol or polyvinylpyrrolidone.
[0043] Depending on the capsule wall material and manufacturing method, microcapsules are formed with different properties in terms of diameter, size distribution, and physical and / or chemical properties.
[0044] The microcapsules according to component a) of the composition according to the first aspect may be any microcapsule known to those skilled in the art.
[0045] Preferably, the microcapsules used within the scope of the present invention are such that the shell of the at least one microcapsule comprises or consists of a shell material selected from the group consisting of sol-gel polymers (e.g. silica), polysiloxanes, polyacrylates, polyacrylamides, poly(acrylate-co-acrylamide), polyureas, polyurethanes, polyamides, polypeptides, polysulfonates, polysaccharides, polyphenolic polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), poly(melamine-urea), or combinations thereof.
[0046] The compositions according to the first and second aspects of the invention comprise at least one of said microcapsules, i.e. one of the microcapsules may be embedded in the polymer matrix of the invention, or two or more of the microcapsules may be embedded in the polymer matrix. All the microcapsules may be of the same type, i.e. all the microcapsules may be, for example, poly(melamine-formaldehyde) based. Alternatively, some of the microcapsules of component a) may be, for example, poly(melamine-formaldehyde) based and other microcapsules may be polyurea based. That is, component a) may comprise or consist of a mixture of different types of microcapsules based on different encapsulation / shell materials.
[0047] Preferably, however, the microcapsules according to component a) of the first and / or second aspect of the present invention are selected from the group of capsule types consisting of poly(melamine-formaldehyde)-based microcapsules and isocyanate-based microcapsules, such as polyurea- and / or polyurethane-based microcapsules, which are preferably biodegradable.
[0048] Biodegradable microcapsule technology is known to those skilled in the art and is particularly preferred within the context of the present invention from the standpoint of environmental sustainability. Examples of such biodegradable microcapsules include isocyanate-based microcapsules and polysaccharide-based microcapsules.
[0049] Biodegradation of the microcapsule slurry in the environment includes the biological degradation of the polymer shell of the present invention. It may be possible to measure the bioactivity or degradation of the shell material in different environments in soil, seawater, or sludge, among others based on OECD guidelines. OECD tests that can be used to measure the ready biodegradability of organic chemicals include the following six test methods described in OECD Test Guideline No. 301A-F: DOC Die-Away Test (TG301A), CO2 Evolution Test (TG301B), Modified MITI Test (I) (TG301C), Closed Bottle Test (TG301D), Modified OECD Screening Test (TG301E) and Manometric Respirometry Test (TG301F). For further details, please refer to the official OECD guidelines on the testing of chemicals: OECD (2006), Preface to the revised OECD Guidelines on the Testing of Chemicals, Chapter 3, OECD Guidelines on the Testing of Chemicals, Chapter 3, OECD Publishing, Paris.
[0050] Within the context of the present invention, microcapsules are considered to be biodegradable if the requirements set out in the OECD 301F biodegradability standard are met (Standardized OECD 301F Test Method: Manometric Respirometry Test). According to OECD 301F, microcapsules are considered to be readily biodegradable if more than 60% of the wall material is degraded after 28 days.
[0051] Therefore, in the composition according to the invention, said at least one microcapsule is preferably biodegradable according to OECD 301F.
[0052] In the context of the present invention, microcapsules are understood to be microparticles that contain at least one active ingredient as a core material inside the capsule, the active ingredient being encapsulated by the capsule shell or capsule wall as described above. As the active ingredient to be encapsulated according to the present invention, essentially any material suitable as an inclusion in a microcapsule can be considered during the process of the present invention. Preferably, hydrophobic or lipophilic, i.e. water-insoluble or water-immiscible liquids or solids, as well as suspensions, can be considered as the active ingredient to be encapsulated. These are mainly non-polar substances. Such hydrophobic substances are mostly lipophilic, i.e. they dissolve well in oils and fats. The terms "microcapsule" and "capsule", "hydrophobic" and "lipophilic" are used synonymously within the context of the present invention.
[0053] In the context of the present invention, the core material is preferably a hydrophobic active substance, ie a substance that has a particular effect or causes a particular reaction, such as a drug, a pesticide, a cosmetic active ingredient, a food active ingredient, and the like.
[0054] In a particularly preferred variant of the invention, the at least one liposoluble or hydrophobic active ingredient is in particular a liposoluble or hydrophobic fragrance or aroma substance, a liposoluble or hydrophobic perfume oil or aroma oil (i.e. a mixture of aroma substances or a mixture of aroma substances, respectively), a cooling agent, a TRPV1 modulator or a TRPV3 modulator, a substance producing a pungent taste, a substance producing a sensation of warmth or heat on the skin or mucous membranes, a substance producing a tingling sensation in the mouth or throat, an active ingredient having an astringent effect, a pesticide, a biocide, an insecticide, a repellent, a food additive, a cosmetic active ingredient, a pharmaceutical active ingredient, a dye, a dye precursor, a pesticide, a dye, a luminescent paint, an optical brightener, a solvent, a wax, a silicone oil, a lubricant, a printing coating for paper, or a mixture of two or more of these active ingredients.
[0055] In a preferred embodiment according to the first and / or second aspect of the invention, the microcapsules have a core material in the form of a hydrophobic monofragrance or monoodorant, which core material comprises at least one monofragrance, monoodorant or mixture thereof, selected from one or more of the following groups: Extracts and fractions or isolated components thereof from natural sources;Single aroma substances from hydrocarbons;Aliphatic alcohols;Aliphatic aldehydes and acetals;Aliphatic ketones and oximes;Sulfur-containing aliphatic compounds;Aliphatic nitriles;Esters of aliphatic carboxylic acids;Formates, acetates, propionates, isobutyrates, butyrates, isovalerates, pentanoates, hexanoates, crotonates, tiglates and 3-methyl-2-butenoates of acyclic terpene alcohols;Acyclic terpene aldehydes and ketones, and their dimethyl acetals and diethyl acetals;Formates, acetates, propionates, isobutyrates, butyrates and isovalerates of cyclic terpene alcohols. acid esters, pentanoates, hexanoates, crotonates, tiglates and 3-methyl-2-butenoates;cyclic terpene aldehydes and ketones;cyclic alcohols;cyclic and alicyclic ethers;cyclic and macrocyclic ketones;alicyclic aldehydes;alicyclic ketones;esters of cyclic alcohols;esters of alicyclic carboxylic acids;aromatic hydrocarbons;araliphatic alcohols;esters of araliphatic alcohols and aliphatic carboxylic acids;araliphatic ethers;aromatic aldehydes and araliphatic aldehydes;aromatic ketones and araliphatic ketones;aromatic and araliphatic carboxylic acids and their esters;nitrogen-containing aromatic compounds;phenyl ethers and phenyl esters;heterocyclic compounds;lactones;and mixtures of the above active ingredients.
[0056] Specific examples of the above substances are known to those skilled in the art. Fragrances or odorants and mixtures of two or more of these substances are chemical substances or compositions used to impart, impart and / or modulate a particular odor or odor impression. Preferably, said odor (impression) is considered to be pleasant.
[0057] In another embodiment according to the invention, the microcapsules of the invention use as the encapsulated active ingredient or core material a fragrance or a perfume oil, i.e. a fragrance or an aromatic oil, respectively. These are compositions containing at least one fragrance or a fragrance. Such compositions, in particular a mixture of fragrances or perfume oils, preferably contain 2, 3, 4, 5, 6, 7, 8, 9, 10 or more fragrances. The fragrance mixture or perfume oil, respectively, is preferably an extract from a natural source, such as an essential oil, a coagulum, an absolute, a resin, a resinous substance, a balsam, a tincture, for example ambergris oil, amyris oil, angelica seed oil, angelica root oil, anise oil, valerian oil, basil oil, tree moss (Tree Moss), or a mixture of essential oils, coagulants, absolutes, resins, resinous substances, balsams, tinctures, etc. moss absolute, bay oil, mugwort oil, benzoin resin, bergamot oil, beeswax absolute, birch tar oil, bitter almond oil, savory oil, buco leaf oil, cabulba oil, cade oil, chalmers oil, cananga oil, cardamom oil, cascarilla oil, cassia oil, cassi absolute, castoreum absolute, cedar leaf oil, cedarwood oil, cis Tas oil, citronella oil, citron oil, copaiba balsam, copaiba balsam oil, coriander oil, costus root oil, cumin oil, cypress oil, davana oil, dill herb oil, dill seed oil, eau de brussels absolute, oakmoss absolute, elemi oil, tarragon oil, eucalyptus citriodora oil, eucalyptus oil, fennel oil, spruce needle oil, galbanum oil, galbanum resin, zea mays oil, Lamium oil, Grapefruit oil, Guaiac wood oil, Gurjun balsam, Gurjun balsam oil, Helichrysum absolute, Helichrysum oil, Ginger oil, Iris root absolute, Iris root oil, Jasmine absolute, Calamus oil, Chamomile oil blue, Chamomile oil Roman, Carrot seed oil, Cascarilla oil, Pine needle oil, Curly mint oil, Caraway seed oil, Labdanum oil, Labdanum absolute, Labdanum resin, Lavandin absolute, Lavandin oil, Lavender absolute, Lavender oil, Lemongrass oil, Lovage oil, Distilled lime oil, Pressed lime oil, Linal oil, Litsea cubeba oil, Bay leaf oil, Macis oil, Marjoram oil, Mandarin oil, Masso bark oil, Mimosa absolute, Musk grain oil,Mus tincture, Muscat sage oil, Muscat oil, Myrrh absolute, Myrrh oil, Myrtle oil, Clove leaf oil, Clove flower oil, Neroli oil, Olibanum absolute, Olibanum oil, Opopanax oil, Orange flower absolute, Orange oil, Origanum vulgare oil, Palmarosa oil, Patchouli oil, Perilla oil, Balsam of Peru oil, Parsley leaf oil, Parsley seed oil, Petitgrain oil, Peppermint oil, Pepper oil, Pimento oil, Pine oil, Poley oil, Rose absolute, Rosewood oil, Rose oil, Rosemary oil, Sage oil Dalmatia, Se The oils selected from the group consisting of oleander oil, sandalwood oil, celery seed oil, spicy lavender oil, star anise oil, styrax oil, tagetes oil, fir needle oil, tea tree oil, turpentine, thyme oil, tolu balsam, tonka absolute, tuberose absolute, vanilla extract, violet leaf absolute, verbena oil, vetiver oil, juniper berry oil, wine yeast oil, mugwort oil, wintergreen oil, ylang oil, hyssop oil, civet absolute, cinnamon leaf oil, cinnamon bark oil, and fractions or components isolated therefrom.
[0058] In a further variant of the invention according to the first and / or second aspect, the aromatic substance may be encapsulated in the form of a single aromatic oil as a core material, which core material comprises at least one single aromatic substance or a mixture thereof as active ingredient.
[0059] However, it is preferred that a single fragrance or odorant (i.e. a chemical compound having an odor or smell, any natural or synthetic substance that imparts an olfactory perceptible odor) or a mixture of fragrances or odorants (so-called perfume oils) is used as the active ingredient encapsulated by the microcapsule shell. More preferably, said substance or mixture of substances imparts a pleasant odor to the consumer product.
[0060] In a preferred variant of the invention, all microcapsules of component a) are loaded with the same active ingredient, for example all microcapsules contain one fragrance, even more preferably the same fragrance.
[0061] Preferably, the compositions according to the present invention do not contain free fragrances or fragrance oils, i.e., the compositions of the present invention preferably do not contain any unencapsulated fragrances or fragrance oils in order to achieve the benefits described herein when incorporated into a solid consumer product formulation.
[0062] According to another embodiment, the microcapsules according to component a) encapsulate different types of active ingredients or different substances of the same type of active ingredient, for example some microcapsules contain one particular fragrance and other microcapsules contain another fragrance.
[0063] The core material is preferably selected independently of the shell material.
[0064] Based on the total weight of the pastille, 0.5% to 10% by weight of the microcapsules can be incorporated into the composition. That is, one pastille of the composition according to the first and / or second form of the present invention contains 0.5% to 10% by weight of the above microcapsules. If the amount of component a) is within this range, the microcapsules can be uniformly distributed in the pastille. If the amount of component a) is within the above range, the active ingredient can be efficiently incorporated into the final solid consumer product formulation. This is due to the efficient protection by the surrounding polymer matrix. That is, since the microcapsules are not destroyed during the manufacturing process of the solid consumer product, the encapsulated active ingredient can be effectively retained without loss, and as a result, the performance of the microcapsules is significantly improved as shown in the examples.
[0065] According to a preferred embodiment, the amount of microcapsules is in the range of 0.5% to 10% by weight, based on the total weight of the pastille, and even more preferably in the range of 3% to 8% by weight, based on the total weight of the pastille.
[0066] The compositions of the present invention, including microcapsules encapsulating active ingredients, can be efficiently incorporated into a variety of solid consumer product formulations to efficiently release the active ingredients in a targeted manner, and the surrounding polymer matrix thus acts as a kind of shock absorbing layer that protects the microcapsules from damage due to mechanical, chemical and / or thermal influences and prevents premature release or degradation of the active ingredients during the manufacturing process of the consumer product.
[0067] Polymer or polymer matrix
[0068] As mentioned above, the composition / pascent according to the first and / or second aspect of the present invention comprises or consists of 92-98% by weight or 60-80% by weight, respectively, of at least one polymer, based on the total weight of the pastille.
[0069] A preferred polymer according to the present invention is a meltable polymer, such as polyethylene glycol ("PEG") having a molecular weight of about 3,000 to 20,000 Da, preferably about 4,000 to 12,000 Da, and even more preferably about 5,000 to 8,000 Da.
[0070] Component b) may comprise one specific polymer having a molecular weight in the ranges above, or two or more different polymers, which may be the same material with different molecular weights within the ranges above (such as PEG3000 and PEG4000), or may be different chemical entities with the same or different molecular weights.
[0071] If the molecular weight of the polymer used as component b) is within the above range, it can effectively protect the fragile microcapsules and make them effectively compatible in solid consumer product formulations.
[0072] In the context of this invention, a "meltable" polymer is a plastic polymer material that becomes pliable or moldable at a certain elevated temperature and solidifies upon cooling.
[0073] The polymers used within the context of the present invention can be water-soluble or water-insoluble polymers. According to another embodiment, component b) comprises a mixture of one or more water-soluble polymers, a mixture of one or more water-insoluble polymers or a mixture of one or more water-soluble and one or more water-insoluble polymers.
[0074] In a preferred variant of the invention, the melting point of the polymer according to the first and / or second embodiment of the invention (preferably having a molecular weight of about 3,000 to 20,000 Da) is preferably in the range of 25°C to 100°C, preferably 40°C to 80°C.
[0075] However, the polymers used as component b) in the context of the first and second aspects of the invention are preferably water-soluble: when incorporated into a fabric care formulation, such as, for example, a powder detergent, the polymeric protective matrix dissolves and releases the microcapsules, which can then be applied to the fabric.
[0076] Examples of suitable water-soluble polymers include polyvinyl alcohol, derivatives of polyvinyl alcohol (such as quaternary amine derivatives), polyethylene glycols (of various molecular weights), polyvinylpyrrolidones, (poly)acrylates, polyacrylic acids, acrylamides, polyamino acids and amine-functional polymers, monosaccharides and polysaccharides such as starch, modified starches, maltodextrins, carbohydrates, chitosan, and gum arabic, maleic anhydride copolymers, vinyl acids and vinyl ethers, styrene, polystyrene sulfonates, ethylene glycol-propylene glycol block copolymers, and mixtures thereof. Examples of suitable water-insoluble polymers include, in particular, waxes such as traditional capsules with coatings, beeswax, sunflower seed wax, rice bran wax, carnauba wax, pinova wax, rapeseed wax, soybean wax, candelilla wax, jojoba oil, cork wax, guaruma wax, cotton wax, foxwax, peat wax, rose wax, jasmine wax, peat-wax from winter melon, myrtle wax (Myrica cerifera), fig wax, berry wax, and mixtures of different waxes.
[0077] In a preferred embodiment of the invention, the polymer is preferably a polyethylene glycol (also known as polyethylene oxide (PEO) or polyoxyethylene (POE)) with a molecular weight of about 3,000 to 20,000 Da, preferably about 3,000 to 12,000 Da, even more preferably about 4,000 to 9,000 Da. According to another preferred embodiment, component b) comprises a mixture of two or more polyethylene glycols with different molecular weights.
[0078] Polyethylene glycol is an inexpensive, synthetic, hydrophilic, biocompatible polymer that is widely used in biomedical and other applications, such as as an excipient or laxative in pharmaceutical compositions, in the chemical industry as, for example, a lubricant coating, and in cosmetic formulations as a cream base or dispersing agent. Polyethylene glycol is a flexible, water-soluble polymer with low toxicity and is miscible in a wide variety of formulations. Its general formula is C 2n H 4n+2 O n+1 .
[0079] The composition of the invention according to the first aspect may comprise 91 to 98% by weight, preferably 92 to 98% by weight, even more preferably 92 to 96% by weight of polymer (component b), based on the total weight of the pastille.
[0080] The composition of the invention according to the second embodiment may comprise 60-80% by weight, preferably 92-98% by weight, even more preferably 92-96% by weight of polymer (component b), based on the total weight of the pastille.
[0081] When the polymer is contained within this range in the composition of the present invention, the fragile microcapsules can be effectively protected.
[0082] According to another preferred variant of the first and second aspects of the invention, the polymer exhibits a certain freezing point. The minimum freezing point of the water-soluble polymer-like particles, i.e. the final pastille, is preferably higher than 0° C., preferably higher than 20° C., particularly preferably higher than 35° C. On the other hand, the minimum freezing point of the water-insoluble polymer-like particles is higher than 0° C., preferably higher than 20° C., particularly preferably higher than 35° C. A freezing point within said range facilitates the formation of the pastille according to the invention without the need for low temperatures during the pastille manufacturing process or subsequent steps.
[0083] glue
[0084] Interestingly, it has been found that such polymers, when further combined with adhesives, can effectively protect the microcapsules during incorporation into solid consumer product formulations.
[0085] Thus, in a second aspect, the present invention relates to a composition comprising or consisting of a microcapsule component (component a), a polymer component (component b) and an adhesive component (component c) in a specific ratio, where components b) and c) form a protective matrix surrounding or embedding the fragile microcapsules.
[0086] Adhesives according to the present invention are defined as substances that enhance the adhesion of the microcapsules to external materials or surfaces such as textiles (adhesion promoters). The adhesion can be based on mechanical bonds, hydrogen bonds, chemical or covalent bonds, thermodynamic bonds, etc.
[0087] Preferably, the adhesive used as component c) according to the second aspect of the invention is a substance selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters and mixtures thereof, such as natural and synthetic waxes. The composition according to the invention may therefore contain, as component c) of the second aspect, one or a mixture of two or more of such adhesives.
[0088] Further suitable adhesives according to the second aspect of the invention are e.g. Long-chain, aliphatic, linear or branched, saturated or unsaturated carboxylic acids (fatty acids) having 12 to 30 carbon atoms, in particular lauric acid (12:0), tridecanoic acid (13:0), myristic acid (14:0), pentadecanoic acid (15:0), palmitic acid (16:0), margaric acid (17:0), stearic acid (18:0), nonadecanoic acid (19:0), arabinose (19:0), arachidonic acid (19:0), arachidonic acid (20:0), arachidonic acid (21:0), arachidonic acid (22:0), arachidonic acid (23:0), arachidonic acid (24:0), arachidonic acid (25:0), arachidonic acid (26:0), arachidonic acid (27:0), arachidonic acid (28:0), arachidonic acid (29:0), arachidonic acid (30:0), arachidonic acid (31:0), arachidonic acid (32:0), arachidonic acid (33:0), arachidonic acid (34:0), arachidonic acid (35:0), arachidonic acid (36:0), arachidonic acid (37:0), arachidonic acid (38:0), arachidonic acid (39:0), arachidonic acid (40:0), arachidonic acid (41:0), arachidonic acid (42:0), arachidonic acid (43:0), arachidonic acid (44:0), arachidonic acid (45:0), arachidonic acid (46:0), arachidonic acid (47:0), arachidonic acid (48:0), arachidonic acid (49:0), ar Kizic acid (20:0), heneicosanoic acid (21:0), behenic acid (22:0), lignoceric acid (24:0), cerotic acid (26:0), montanic acid (28:0), and melissic acid (30:0); myristoleic acid (14:1), palmitoleic acid (16:1), margaroleic acid (17:1), petroselinic acid (18:1), oleic acid (18: 1), elaidic acid (18:1), vaccenic acid (18:1), gadoleic acid (20:1), gondonic acid (20:1), cetoleic acid (22:1), erucic acid (22:1), nervonic acid (24:1), linoleic acid (18:2), α-linolenic acid (18:3), γ-linolenic acid (18:3), calendullic acid (18:3), punicic acid (18:3), α-eleo Stearic acid (18:3), β-eleostearic acid (18:3), stearidonic acid (18:4), arachidonic acid (20:4), eicosapentaenoic acid (20:5), docosatetraenoic acid (ADA) (22:4), docosapentaenoic acid (DPA-3) (22:5), docosahexaenoic acid (22:6), tetracosahexaenoic acid (24:6), phytanic acid; Long-chain, aliphatic, linear or branched, saturated or unsaturated primary alcohols (fatty alcohols) having 12 to 30 carbon atoms, in particular lauryl alcohol (12:0), myristyl alcohol (14:0), palmityl alcohol (16:0), margaryl alcohol (17:0), stearyl alcohol (18:0), arachidyl alcohol (20:0), behenyl alcohol (22:0), lignoceryl alcohol (24:0), ceryl alcohol (26:0), montanyl alcohol (28:0), and melissyl alcohol (30:0); palmitoleyl alcohol (16:1), oleyl alcohol (18:1), elaedyl alcohol (18:1), linoleyl alcohol (18:2), gamma-linoleyl alcohol (18:3); Esters of long-chain, aliphatic saturated carboxylic acids having 12 to 30 carbon atoms with long-chain, aliphatic primary alcohols having 12 to 30 carbon atoms, in particular lauryl palmitate, myricyl palmitate, cetyl arachinate, and stearyl behenate; Animal and vegetable waxes, especially wool wax, China wax, beeswax, sunflower seed wax, rice bran wax, carnauba wax, pinova wax, rapeseed wax, soy wax, candelilla wax, jojoba oil, cork wax, guaruma wax, cotton wax, flax wax, peat wax, rose wax, jasmine wax, peat wax from washed gourd, myrtle wax (Myrica cerifera), fig wax, berry waxes, As well as mixtures of two or more of the above adhesives.
[0089] Of the carboxylic acids listed above, the saturated fatty acids are preferred. The use of the above animal and vegetable waxes is most preferred in the context of the present invention, due to their low melting point and ease of incorporation into the composition.
[0090] According to another preferred embodiment, said at least one adhesive is selected from the group consisting of animal and / or vegetable waxes, with (natural) beeswax being preferred.
[0091] Surprisingly, it has been found that such natural or synthetic waxes, as well as animal and / or vegetable waxes, can be efficiently incorporated into the composition of the second form, and furthermore, the use of these substances improves the adhesion of the microcapsules onto the surface of another material, such as textile fibres, while at the same time providing a good protection for the polymer matrix.
[0092] The adhesive component is incorporated into a polymer matrix.
[0093] Preferably, the adhesive used as component c) according to the second embodiment of the present invention is contained in an amount of 2 to 32% by weight, preferably 3 to 20% by weight, more preferably 4 to 17% by weight, based on the total weight of the pastille.
[0094] Adhesive loadings within this range provide a good balance between protecting the microcapsules and promoting adhesion.
[0095] Plasticizer
[0096] The composition according to the first and / or second aspect may further comprise a certain amount of at least one plasticizer as an additive. Thus, the composition according to the invention may comprise one plasticizer or a mixture of two or more plasticizers.
[0097] A plasticizer is a substance used to increase the flexibility or plasticity of a particular substance or composition, which can also reduce the viscosity and friction of the substance or composition.
[0098] Suitable plasticizers are known to those skilled in the art and are, for example, water, polyethylene glycols, orthophthalates, phthalate esters, trimellitates and their esters, (organic) phosphates, aliphatic dibasic acid esters, benzoates, polyesters, citrates, bio-based plasticizers based on vegetable oils such as epoxidized soybean oil, epoxidized linseed oil, castor oil, palm oil, starch, sugars, chlorinated paraffins, alkylsulfonates, dicarbonates, fatty acid esters.
[0099] The plasticizer is preferably selected from water and polyethylene glycol, for example. Water as a plasticizer may originate from the pastilles manufacturing process or may be added later.
[0100] Preferably, the plasticizer used as an additive according to the first and / or second embodiment of the present invention is contained in an amount of 0.5 to 10% by weight, preferably 2 to 8% by weight, more preferably 3 to 6% by weight, based on the total weight of the pastille.
[0101] The amount of plasticizer added in this range can effectively adjust the viscosity and flexibility of the polymer matrix, making it less brittle, more flexible, and more cushioning, thus providing better protection for the fragile microcapsules and facilitating their incorporation into solid consumer product formulations without changing the fundamental chemical characteristics of the plasticized material.
[0102] Structuring Agent
[0103] Furthermore, one or more structuring agents may be added as a separate component or additive to the composition according to the first and / or second aspect of the invention, preferably to the composition according to the second aspect. Thus, the composition of the invention may comprise one structuring agent or a mixture of two or more structuring agents.
[0104] The structuring agent is preferably contained in an amount of 0.1 to 10% by weight, preferably 1 to 8% by weight, even more preferably 2 to 7% by weight, based on the total weight of the pastille.
[0105] Suitable structurants are commercially available emulsifiers known in the art and esters such as isopropyl myristate.
[0106] The addition of such structuring agents improves spherification during droplet formation, thereby increasing the homogeneity of incorporation of the microcapsules / pastry into the final product formulation. These agents are, for example, additives that increase the viscosity of the composition, resulting in a thick liquid, semi-solid or solid state.
[0107] Furthermore, the composition of the present invention may contain suitable additives, if necessary.
[0108] Composition / pastilles
[0109] The composition according to the first and second aspects of the invention comprises or consists of at least one pastille having the composition described above. Preferably, the composition is present as a plurality of pastilles. Alternatively, the composition is present as a single pastille of the composition described above.
[0110] In a preferred embodiment according to the present invention, the freezing point of the composition according to the first and second aspects of the present invention and the pastilles thereof is 25°C to 100°C, preferably 30°C to 90°C, more preferably 35°C to 85°C, and most preferably 40°C to 75°C.
[0111] When the solidification point is within this range, the composition of the present invention and pastilles thereof are easy to handle.
[0112] According to another preferred embodiment, the viscosity of the composition according to the first and / or second form of the present invention and of the pastilles thereof is in the range of 500 mPas to 1,000 mPas, preferably in the range of 760 mPas to 980 mPas, even more preferably in the range of 800 mPas to 950 mPas, at a temperature of 70° C. and a shear pressure of 6.4 Pa.
[0113] Even more preferably, the viscosity of the composition of the present invention is in the range of 750 mPas to 1,000 mPas, preferably in the range of 760 mPas to 980 mPas, and even more preferably in the range of 800 mPas to 950 mPas, at a temperature of 70° C. and a shear pressure of 6.4 Pa. If the viscosity of the composition is within this range, the composition is considered to be a "solid" at room temperature.
[0114] Therefore, the composition of the present invention is preferably a solid composition.
[0115] A viscosity within this range of compositions allows for ease of processing and incorporation into solid consumer product formulations, and may provide an ideal balance between microcapsule protection and microcapsule performance.
[0116] According to another preferred variant of the invention, the composition according to the first and / or second form of the invention and the pastilles thereof have a Young's modulus E of more than 100 Pa and less than 1 GPa, preferably between 1 kPa and 100 MPa, even more preferably between 10 kPa and 1 MPa.
[0117] Young's Modulus, E, indicates the tensile or compressive stiffness of a solid but elastic material when subjected to a force along its length, based on the tensile / compressive stress (force per unit area) and axial strain (proportional deformation) in the linear elastic region of the material.
[0118] This range of elasticity provides an ideal balance between protection of the microcapsules and efficient incorporation into solid consumer product formulations, while also providing excellent release characteristics.
[0119] In another preferred variant, the water content of the composition according to the first and second form of the invention and of the pastilles thereof is between 2 and 12% by weight, based on the total weight of the pastilles.Preferably, the water content is in the range of 3 to 9% by weight, even more preferably in the range of 4 to 8% by weight.
[0120] Such a water content is favorable in terms of flexibility, since the water component can act as a plasticizer, which is valuable in terms of improving the cushioning effect, thus providing better protection for the fragile microcapsules and facilitating incorporation into solid consumer product formulations without changing the basic chemical characteristics of the plasticized material. A high water content will result in an excessive decrease in viscosity, making incorporation into solid formulations difficult. A low water content will make the pastille material more likely to break when incorporated.
[0121] The above properties of the compositions according to the first and second aspects of the invention can be adjusted by the amounts of the ingredients, the molecular weight of the polymers and the inclusion or absence of additives such as the plasticizers and structurants mentioned above.
[0122] To ensure an optimal distribution of the pastilles and thus of the embedded microcapsules in the final solid consumer product formulation, it is furthermore advantageous if the composition according to the first and / or second aspect of the invention has a particle size of 1 μm to 1 cm, preferably 100 μm to 7 mm, even more preferably 500 μm to 5 mm. Too large pastilles will result in an uneven distribution (see figures 11 and 12).
[0123] In a further preferred variant of the invention, the ratio between the size of the microcapsules and the size of the final granules / pastry is in the range of 1:5 to 1:200, preferably 1:10 to 1:100.
[0124] Said pastilles or granules are preferably in the form of tablets, pills, balls, etc., having a spherical, hemispherical, compressed hemispherical, lentil-shaped, oval shape, and can be prepared by a person skilled in the art by methods known in the art.
[0125] Additionally, the compositions of the present invention and pastilles thereof may contain one or more ingredients, such as colorants, that enhance the aesthetic appeal of the final product. Additionally, the compositions may further contain additives and / or active ingredients, such as optical brighteners, detergents, laundry actives, etc.
[0126] Method for producing the composition of the present invention
[0127] According to a third aspect, the present invention relates to a method for the manufacture of a composition comprising or consisting of a plurality of pastilles, the method comprising the steps of: (i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule; (ii) melting at least one polymer and, optionally, an adhesive; (iii) mixing said at least one microcapsule into the polymer melt of step (ii); (iv) forming a pastille by dropwise addition of the mixture of step (iii); (v) optionally cooling; Including, Optionally, the method further comprises the step of adding at least one plasticizer and / or structurant during or after step (ii) or (iii).
[0128] In the context of the present invention, the ingredients defined in the first and second aspects also apply to the third aspect, i.e. the terms "microcapsules", "polymers", "adhesives", "plasticizers", "pastel", "structurants" etc. and their respective amounts and properties are as described above.
[0129] The process according to the third aspect defined herein is suitable for the preparation of compositions according to the first and second aspects of the invention, with the respective amounts adjusted as required.
[0130] In a first step (i) of the process according to the invention, a microcapsule as defined herein is provided, which may be present in its pure form or in the form of an aqueous dispersion comprising one or more microcapsules, preferably a plurality of microcapsules.
[0131] The microcapsules are preferably dispersed in the aqueous phase. For microcapsules according to the invention dispersed in the aqueous phase, preferably the concentration of microcapsules in the aqueous phase is greater than 5% and less than 70% by weight, preferably greater than 20% and less than 60% by weight, most preferably greater than 30% and less than 50% by weight, based on the weight of the dispersion.
[0132] The microcapsules are advantageously in the form of a dispersion, which allows for a better and more uniform distribution of the microcapsules in the final pastille. Moreover, the water in the continuous or external phase of the dispersion acts as a plasticizer, improving the above-mentioned properties of the final product and effectively adjusting the viscosity and flexibility of the polymer matrix, which results in a matrix that is less brittle, more flexible and has a better cushioning effect. This allows for better protection of the fragile microcapsules and facilitates their incorporation into solid consumer product formulations without changing the basic chemical characteristics of the plasticized material.
[0133] Therefore, in step (i) of the process according to the third aspect of the invention, the microcapsules are preferably provided in the form of an aqueous dispersion.
[0134] In the next step (ii) of the method according to the invention, at least one polymer is melted. Optionally, an adhesive can be added and the adhesive is heated and melted together with the polymer as defined herein. Alternatively, each material can be melted separately and the resulting melts combined and homogenized.
[0135] It is further preferred to use a polymer as defined herein, preferably polyethylene glycol, in order to achieve a homogeneous distribution of the microcapsules within the polymer matrix. The melting point of said at least one polymer, preferably polyethylene glycol, is in the range of 25°C to 100°C, preferably in the range of 40°C to 80°C.
[0136] According to a further preferred variant of the invention, in order to embed the microcapsules efficiently and uniformly within the polymer matrix, the melting point of the polymer, preferably with a molecular weight of about 3,000 to 20,000 Da, according to the first, second and / or third aspect of the invention, is preferably in the range of 25°C to 100°C, preferably 40°C to 80°C.
[0137] In a preferred variant of the process according to the invention, the melting step (ii) is carried out at a temperature ranging from 25° C. to 100° C., preferably from 40° C. to 80° C., even more preferably at 80° C., in order to obtain a homogeneous distribution of the microcapsules in the polymer buffer matrix.
[0138] In a next step (iii), the at least one microcapsule or microcapsule dispersion is mixed into the polymer melt of step (ii) to form a homogenous mixture in order to uniformly distribute the microcapsules within the melt.
[0139] Finally, in the next step (iv), pastilles are formed by dropping the mixture from step (iii) using modern pastillation techniques known to those skilled in the art. Pastilles are formed by forming particles, usually using a droplet former, and cooling the resulting particles to form pastilles. The manufacturing process for pastilles and granules is commercially available. Furthermore, good results are obtained when scaled up by dropletization in air or vegetable oil using a pulse generator. Figure 13 shows an example of a pastille obtained from the composition according to the invention.
[0140] If necessary, the resulting granules are solidified in an additional cooling step (v).
[0141] If necessary, at least one plasticizer and / or structurant can be added during or after steps (ii) and / or (iii).
[0142] In order to achieve a uniform distribution of the microcapsules within the protective matrix, it is advantageous to use microcapsules with particle sizes in the range of 150 μm to 5 mm, preferably 500 μm to 3 mm.
[0143] Therefore, according to a preferred variant of the invention, the particle size of the microcapsules according to the first, second and / or third aspect of the invention is preferably in the range of 150 μm to 5 mm, preferably in the range of 500 μm to 3 mm.
[0144] Yet another aspect of the invention relates to a composition produced by the method of the invention.
[0145] consumer products
[0146] In yet another aspect, the present invention relates to the use of a composition according to the invention for the manufacture of a consumer product formulation. The terms "consumer product formulation" and "consumer product" are used synonymously within the context of the present invention.
[0147] Any of the above compositions, i.e. the composition according to the first aspect of the invention, the composition according to the second aspect of the invention and / or the composition obtained according to the process according to the third aspect of the invention, are suitable for the manufacture of consumer product formulations.
[0148] Particular advantages of the inventive pastille composition have been found in terms of the manufacture of solid consumer products such as washing powders, laundry soaps, fabric softener bars, deodorant sticks, etc. Thus, the consumer product according to the invention is preferably a solid consumer product.
[0149] Thus, in another preferred variant, the present invention also relates to the use of the composition according to the invention for the manufacture of consumer products and consumer product formulations, such as solid products like fabric care products (detergent powders, laundry soaps, fabric softener bars, etc.), bar soaps, household products (toilet cleaner bars, all-purpose cleaner bars, carpet cleaner powders, detergent powders for washing dishes or cleaning various surfaces, etc.), personal care products (deodorants, soaps, etc.), scent boosters, scent enhancers, pharmaceuticals, and mixtures thereof.
[0150] Finally, in another aspect, the present invention relates to a consumer product or consumer product formulation comprising or consisting of a composition according to the present invention, i.e. a composition according to the first aspect of the invention, a composition according to the second aspect of the invention and / or a composition obtained according to the process according to the third aspect of the invention.
[0151] The compositions of the present invention allow for efficient incorporation of active ingredients into solid product formulations and efficient, targeted release of the active ingredients. EXAMPLES
[0152] The present invention will now be described in more detail with reference to specific examples, but the present invention is not limited to these examples.
[0153] Example 1: Composition containing microcapsules but no adhesive in laundry soap (Composition I) - Sensory evaluation
[0154] In Example 1, a composition containing microcapsules was prepared as follows. In a first step, core-shell microcapsules were prepared, containing a melamine-formaldehyde-based shell material and a fragrance core (microcapsule size: 10-50 μm). The microcapsules were prepared by known techniques. Next, a polymer, polyethylene glycol (molecular weight: 5400 Da-6600 Da), was melted at a temperature of 80° C., and the resulting polymer melt was mixed with the microcapsules. In a next step, this viscous mixture was dripped through a small opening using a modern pastillation method to form multiple pastilles with an average particle size of about 2 mm, in which the microcapsules were embedded in a polyethylene glycol matrix, and the pastilles were further cooled to solidify. The percentages of polyethylene glycol in the final pastilles were about 98%, 95%, and 92% by weight, respectively, based on the total weight of the pastilles.
[0155] The sensory evaluation was carried out as follows: After preparing the composition of the present invention, the resulting microcapsule composition was mixed with particulate commercial laundry soap, the resulting mixture was processed in an extruder, and the final soap was chopped into small pieces. The final content of microcapsules in 30 g of laundry soap was 0.4 wt %.
[0156] The laundry soap thus prepared was applied to damp fabric (terry cloth) by rubbing. After rinsing, the fabric was air dried at room temperature.
[0157] A laundry soap without the composition of the present invention containing fragrance microcapsules was used as a control. As a second control, a laundry soap was used that contained a melamine-formaldehyde based shell material and a fragrance core, but did not contain a surrounding polyethylene glycol matrix. In the third control, unlike the pastilles described above, the capsules were produced by coating with polyethylene glycol (coating thickness about 5-25 nm) without being mixed with the matrix.
[0158] The particle sizes of all the microcapsules were in the range of 10-50 μm.
[0159] The release of the fragrance took place in three stages. In the first stage, the odor of the untreated fabric was examined. In the second stage, the odor of the fabric was examined after it had been lightly rubbed. For this, the fabric was subjected to a slight mechanical stress by moving it back and forth between the hands several times, which broke the capsules. In the third stage, the fabric was rubbed vigorously, which broke the capsules, and the odor was examined afterwards. After each stage, the fragrance intensity was evaluated.
[0160] Eight to nine testers rated the intensity of the scent on a scale from 1 (no smell) to 9 (extremely strong smell).
[0161] The results of the sensory evaluation are shown in FIG.
[0162] Samples with compositions of the present invention containing core-shell microcapsules embedded in a polyethylene glycol matrix perform significantly better, effectively protecting the fragile microcapsules in the solid product formulation while still effectively releasing the active ingredient. The polymer matrix acts as a shock-absorbing layer during the manufacturing process of the consumer product. Samples without such a shock-absorbing layer or simply with a coating do not perform well, since most of the microcapsules are destroyed during the manufacturing of the consumer product.
[0163] Example 2: Composition containing microcapsules with adhesive in laundry soap (Composition II - Sensory Evaluation
[0164] In Example 2, a composition containing microcapsules was prepared as follows. In the first step, core-shell microcapsules containing a melamine-formaldehyde-based shell material and a fragrance core were prepared (microcapsule size: 10-50 μm). The microcapsules were prepared by known techniques. Next, the polymer polyethylene glycol (molecular weight: 5400 Da-6600 Da) and beeswax as an adhesive were melted at a temperature of 80° C., and the resulting polymer melt was mixed with the microcapsules. The ratio of polyethylene glycol to beeswax was 75% by weight to 17% by weight, based on the total weight of the pastilles. In the next step, this viscous mixture was dripped through a small opening using a modern pastille method to form multiple pastilles with an average particle size of about 2 mm, in which the microcapsules were embedded in a polyethylene glycol-beeswax matrix, and the pastilles were further cooled to solidify. The polyethylene glycol-beeswax mixture in the final pastilles was about 92% by weight, based on the total weight of the pastilles.
[0165] After preparing the composition of the present invention, the resulting microcapsule composition was mixed with particulate commercial laundry soap, the resulting mixture was processed in an extruder, and the final soap was chopped into pieces. The final content of microcapsules in 30 g of laundry soap was 0.4 wt. %.
[0166] The sensory evaluation was carried out in the same manner as in Example 1. The results of the sensory evaluation are shown in FIG.
[0167] A significant improvement in performance is observed when samples containing the prepared protected microcapsules are compared to unscented samples, samples containing unprotected microcapsules, and samples containing simply coated microcapsules. Furthermore, it has been observed that the combination of a polymer (polyethylene glycol) with an adhesive (beeswax) results in a significant improvement in performance, improved absorption and protection, compared to compositions containing only a polyethylene glycol matrix.
[0168] Example 3: Composition in tablet form containing microcapsules but no adhesive (Composition I) - Sensory evaluation
[0169] Pastilles having melamine-formaldehyde-based fragrance microcapsules embedded in a polyethylene glycol matrix were prepared according to the method described in Example 1.
[0170] Next, a powder mixture of sodium sulfate and bentonite was prepared and mixed with the prepared pastilles. After homogenizing the mixture, it was tableted at 100 kN. The final content of the microcapsules was 1 wt% in the final tablet of 10 g.
[0171] Each control sample was prepared in the same manner. A tablet without the inventive composition containing fragranced microcapsules was used as the control sample. As a second control sample, a tablet with a melamine-formaldehyde based shell material and a fragranced core, but without a surrounding polyethylene glycol matrix, was used. As a third control sample, coated microcapsules were used.
[0172] For fabric treatment, liquid detergent and the prepared tablets were added to the washing machine, the fabrics were washed at 30°C and then air dried at room temperature. The prepared tablets were used as solid fabric softeners.
[0173] The sensory evaluation was carried out in accordance with Example 1. The results of the sensory evaluation are shown in FIG.
[0174] Example 3 similarly improves the performance of a solid product formulation containing the inventive composition having an impact absorbing layer around friable microcapsules, showing that it can be effectively incorporated into the product without adversely affecting release behavior.
[0175] More surprisingly, even though the concentrations in the final product are the same, the particles with a high content (92% polyethylene glycol and 8% microcapsules by weight per pastille) have a better sensory evaluation than the particles with a low content (98% polyethylene glycol and 2% microcapsules by weight per pastille), indicating that the composition of the present invention can increase the number of microcapsules incorporated.
[0176] Example 4: Composition in tablet form containing microcapsules together with an adhesive (Composition II) - Sensory evaluation
[0177] The samples of Example 4 were prepared and evaluated in a similar manner to the samples based on Example 3. However, unlike Example 3, the polymer matrix in which the core-shell microcapsules are embedded further comprises a beeswax component, similar to Example 2.
[0178] The results of the sensory evaluation are shown in FIG.
[0179] Sensory evaluation revealed that samples with capsules containing only polyethylene glycol and samples with a mixture that also contained the adhesive beeswax performed significantly better than the control samples.
[0180] Example 5: Composition containing microcapsules but no adhesive in a powder detergent (Composition I) - Sensory evaluation
[0181] Pastilles having melamine-formaldehyde-based fragrance microcapsules embedded in a polyethylene glycol matrix were prepared according to the method described in Example 1.
[0182] The prepared pastilles were then mixed with a commercial powder detergent and homogenized, with the final content of microcapsules being 0.5% by weight in 40 g of laundry soap.
[0183] Finally, the product was placed in the washing machine and the fabric was washed at 30°C and then air dried at room temperature.
[0184] The sensory evaluation was carried out in accordance with Example 1. The results of the sensory evaluation are shown in FIG.
[0185] The performance of all samples is significantly improved due to the buffering function of the polymer matrix during the consumer product manufacturing process. Unprotected microcapsules are unsuitable for the manufacture of fragranced detergent powders, as they are destroyed during mixing and homogenization with the detergent powder.
[0186] Example 6: Composition containing microcapsules together with an adhesive in a powder detergent (Composition II) - Sensory evaluation
[0187] According to another example, a composition of the present invention comprising a plurality of pastilles was prepared, processed and analyzed as in Example 5. The polymer matrix further comprises an adhesive (beeswax).
[0188] The results of the sensory evaluation are shown in FIG.
[0189] From Figure 6 it can be seen that depending on the formulation, the addition of adhesives results in similar sensory performance: in all cases the performance of the fragranced detergent powder is increased by 5-6 times compared to the control detergent powder not containing the fragrance composition according to the invention.
[0190] Example 7: Composition containing biodegradable microcapsules but no adhesive in laundry soap (Composition I) - Sensory evaluation
[0191] Example 7 corresponds to Example 1 above. However, instead of core-shell microcapsules with a melamine-formaldehyde based shell material and a scented core, biodegradable microcapsules with a biodegradable isocyanate based shell material and a scented core were used. The shell material of the microcapsules used was based on a polymer of 1,3-bis(6-isocyanatohexyl)-1,3-diazetidine-2,4-dione and bis(isocyanatomethyl)cyclohexane, gelatin and maltodextrin.
[0192] Within the scope of the present invention, a microcapsule is considered to be biodegradable if the shell material of the microcapsule is degradable according to the criteria of OECD 310F.
[0193] The results of the sensory evaluation are shown in FIG.
[0194] The results demonstrate that the present compositions are suitable regardless of microcapsule composition and allow for the efficient incorporation of biodegradable microcapsules into solid consumer product formulations such as laundry soaps.
[0195] Example 8: Composition containing biodegradable microcapsules in a laundry soap together with an adhesive (Composition II) - Sensory evaluation
[0196] In another example, a composition of the present invention comprising a plurality of pastilles was prepared, processed and analyzed as in Example 7. The polymer matrix further comprises an adhesive (beeswax).
[0197] The results of the sensory evaluation are shown in FIG.
[0198] FIG. 8 shows that the performance of the fragranced solid laundry soap is increased by 4-5 times when using a polyethylene glycol matrix or a polyethylene glycol-beeswax matrix compared to a control laundry soap that does not contain a fragrance composition according to the present invention.
[0199] Example 9: Composition containing isocyanate-based microcapsules but no adhesive in a powder detergent (Composition I) - Sensory evaluation
[0200] Example 9 corresponds to Example 5 above. However, instead of core-shell microcapsules comprising a melamine-formaldehyde based shell material and a fragrant core, microcapsules were used comprising a polyurea based shell material, which is the reaction product of a polyisocyanate and a polyamine, encapsulating a fragrant core. The shell material of the microcapsules used is based on the reaction product of hexamethylene diisocyanate, methyldiphenyl diisocyanate and guanidine carbonate.
[0201] The results of the sensory evaluation are shown in FIG.
[0202] As is evident from FIG. 9, embedding the microcapsules in a protective polymer matrix increases the incorporation stability of the microcapsules into solid consumer product formulations and significantly improves the sensory performance.
[0203] Example 10: Composition containing isocyanate-based microcapsules with adhesive in a powder detergent (Composition II) - Sensory evaluation
[0204] In another example, a composition of the present invention comprising a plurality of pastilles was prepared, processed and analyzed as in Example 9. The polymer matrix further comprises an adhesive (beeswax).
[0205] The results of the sensory evaluation are shown in FIG.
[0206] The results indicate that the use of microcapsules embedded in a polymer-adhesive matrix can further improve the performance of consumer products.
Claims
1. A composition comprising or consisting of at least one pastille, the pastille having, based on the total weight of the pastille: (a) 0.5-10% by weight of at least one microcapsule containing an active ingredient, the active ingredient being preferably a fragrance or a mixture of fragrances; (b) 92-98% by weight of a polymer, preferably a polyethylene glycol; A composition comprising or consisting of:
2. The at least one pastille further comprises: (c) 0.5 to 10% by weight, based on the total weight of the pastille, of at least one plasticizer, preferably water or polyethylene glycol; 2. The composition of claim 1, comprising or consisting of:
3. A composition comprising or consisting of at least one pastille, the pastille having, based on the total weight of the pastille: (a) 0.5-10% by weight of at least one microcapsule containing an active ingredient, the active ingredient being preferably a fragrance or a mixture of fragrances; (b) 60-80% by weight of at least one polymer, preferably polyethylene glycol; (c) 2-32% by weight of at least one adhesive, preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; A composition comprising or consisting of:
4. The at least one pastille further comprises, based on a total weight of the pastille: (d) 0.5 to 10% by weight of at least one plasticizer, preferably water or polyethylene glycol; and / or (f) 0.1 to 10 wt. % of a structuring agent, preferably selected from the group consisting of an ester, such as isopropyl myristate, or another emulsifier; The composition of claim 3 comprising or consisting of:
5. A composition according to any one of the preceding claims, wherein the at least one polymer, preferably polyethylene glycol, has a molecular weight of about 3,000 to 20,000 Da.
6. 10. The composition of any one of the preceding claims, wherein the shell of the at least one microcapsule comprises or consists of a shell material selected from the group consisting of sol-gel polymers, polyacrylates, polyacrylamides, poly(acrylate-co-acrylamide), polyureas, polyurethanes, polypeptides, polysaccharides, polyphenolic polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), or combinations thereof.
7. 10. A composition according to any one of the preceding claims, wherein the at least one adhesive is selected from the group consisting of animal and / or vegetable waxes, preferably beeswax.
8. 1. A method for the manufacture of a composition comprising or consisting of a plurality of pastilles, comprising the steps of: (i) providing at least one microcapsule or an aqueous dispersion comprising at least one microcapsule; (ii) melting at least one polymer and, optionally, an adhesive; (iii) mixing said at least one microcapsule into the polymer melt of step (ii); (iv) forming a pastille by dropwise addition of the mixture of step (iii); (v) optionally cooling; Optionally, the process further comprises the step of adding at least one plasticizer and / or structuring agent during or after step (ii) or (iii).
9. A method for preparing a composition according to claim 8, wherein the melting point of said at least one polymer, preferably polyethylene glycol, is in the range of from 25°C to 100°C, preferably from 40°C to 80°C.
10. A process for preparing a composition according to claim 8 or 9, wherein the melting step (ii) is carried out at a temperature in the range of from 25°C to 100°C, preferably from 40°C to 80°C, even more preferably at 80°C.
11. The method for producing a composition according to any one of claims 8 to 10, wherein the particle size of the microcapsules is in the range of 150 µm to 5 mm.
12. A method for preparing a composition according to any one of claims 8 to 11, wherein the microcapsules are provided in the form of an aqueous dispersion.
13. Use of a composition according to any one of claims 1 to 7 for the manufacture of a consumer product formulation.
14. 14. The use of the composition according to claim 13, wherein the consumer product formulation is a solid product such as fabric care products (detergent powders, laundry soaps, fabric softener bars, etc.), bar soaps, household products, personal care products (deodorants, soaps, etc.), pharmaceuticals, and mixtures thereof.
15. A consumer product formulation comprising or consisting of a composition according to any one of claims 1 to 7.
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