Process for preparing powder or incense tablet

Abstract

The present invention relates in particular to the field of perfume particles for solid consumer product formulations such as, for example, fiber care products. More specifically, the present invention relates to a process for preparing powders or tablets consisting of, or comprising, a plurality of microcapsules containing one or more components. Furthermore, the present invention relates to powders or tablets obtained by that process. The present invention further relates to consumer products comprising powders or tablets according to the invention or even more tablets, and to the use of powders or tablets for scenting consumer products according to the invention.

Description

Technical Field

[0001] The present invention relates in particular to the field of perfume particles for solid consumer product formulations such as fiber care products and the like. More specifically, the present invention relates to a process for preparing powders or troches (pastilles) consisting of or containing a plurality of microcapsules containing at least one active ingredient. Furthermore, the present invention relates to powders or troches obtained by the process according to the invention. The present invention further relates to powders or troches or even more troches, i.e., consumer products comprising a plurality of troches according to the invention, and to the use of powders or troches for scenting consumer products according to the invention.

Background Art

[0002] Today, many consumer products such as detergents, fabric softeners, laundry powders, deodorants, lotions, etc. are scented with perfume substances or contain cosmetic ingredients in order to provide certain effects.

[0003] Unfortunately, for example, the perfume substances or cosmetic ingredients of such products often interact with other components of the product formulation, or the more volatile components of the fragrance formulation tend to evaporate too quickly. As a result, this leads to an undesired change and / or reduction of the desired effect, such as the olfactory impression, or to an overly early "use" of the cosmetic ingredients over time, or may cause an adverse reaction with other components of the product formulation, resulting in a reduction in the quality and / or stability of the product. In order to prevent the possibility of perfume or other active components interacting with other components of the product, for example, to prevent the evaporation of perfume, and thus not to distort or reduce the desired olfactory impression, the perfume or other active ingredients can be added to the formulation in encapsulated form. In this way, for example, a targeted release of the active components can be ensured, and thus the desired olfactory impression can be guaranteed. Furthermore, it is possible to reduce the interaction between the components of the product and to improve the quality and storage stability of the product.

[0004] Accordingly, a wide variety of consumer products contain active ingredients such as fragrances encapsulated in their formulations. For example, fabric care formulations such as liquid detergents or fabric softeners contain a plurality of such scented microcapsules. Further, the formulations require the incorporation of preservatives to enhance stability and durability, such as methylisothiazolinone (MIT) that may cause allergic reactions or skin irritation, while powder detergents generally do not require the addition of preservatives and reduce environmental pollution. However, the mixing of the components of the microcapsules with the components of other solid detergents leads to the destruction of the fragile microcapsules, resulting in, for example, the loss of olfactory performance, so the incorporation of microcapsules into powdered formulations such as powder detergents is quite troublesome.

[0005] It is particularly difficult to manufacture microcapsules having good stability and good release characteristics. The ability of the capsule to retain the active ingredient and thus prevent the loss of volatile components depends on the stability of the capsule in the main product components. However, very stable microcapsules, for example, capsules having a relatively thick capsule wall, generally have a low performance tendency because the targeted destruction of the microcapsules is hindered, thus preventing the release of the active ingredient(s). However, if the capsule is too unstable, it will be broken already during storage or production, resulting in the leakage of the active ingredient and neither will function. Therefore, the increase in the capsule wall, i.e., the shell of the multilayered microcapsules or an even thicker shell, each deteriorates the targeted release of the active ingredient, and the microcapsules generally require a complex multi-step preparation process, thus similarly resulting in a decrease in performance.

[0006] In addition, considering the increasing ecological awareness of the public (such as waste reduction, preservative reduction, etc.), there is a new increasing trend towards solid consumer products such as solid hair care products, soaps, and solid body soaps. Therefore, solid consumer products will become increasingly relevant not only in the cosmetics industry but also in other industries. However, as shown above, the incorporation of microcapsule powder formulations is quite troublesome because the mixing of microcapsule components with other common solid detergent components leads to the breakage of fragile microcapsules.

[0007] As a result, it is necessary to improve the efficient incorporation of active agents such as fragrance components into solid consumer product formulations, while at the same time enabling the efficient and targeted release of the active agents.

[0008] In particular, it is necessary to provide the formulation containing the active agent, and in this case, the active agent is provided with improved efficiency and stability.

[0009] In particular, it is necessary to provide a composition containing the active agent for use in such consumer product formulations, especially textile processing compositions having improved olfactory performance and stability.

[0010] At the same time, in order to cover high demand, the composition for solid consumer product formulations should be more easily obtainable, and the obtained composition should exhibit improved characteristics in terms of, for example, its olfactory quality. SUMMARY OF THE INVENTION

[0011] The present invention has been made in consideration of the drawbacks described above. In order to solve the above-mentioned drawbacks, the present invention provides a method for preparing a composition that enables the efficient incorporation of an active ingredient having improved olfactory performance and stability into a solid consumer product formulation and enables the preparation of such consumer products.

[0012] Accordingly, in a first aspect, the present invention relates to a process for preparing a powder or a lozenge comprising, consisting of, or including a plurality of microcapsules containing one or more active ingredients, the process comprising or consisting of the following steps: (i)(a) mixing at least one anhydrous alkaline earth salt or alkali metal salt or a mixture of at least one anhydrous alkaline earth salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, and (c) optionally at least one humectant, wherein the humectant is selected from the group consisting of propylene glycol, ethylene glycol, dipropylene glycol, glycerol, sorbitol, and maltitol; (ii) heating the mixture obtained in step (i) to produce a melt; (iii) dropping the melt produced in step (ii) onto the surface of an object; (iv) seeding and optionally cooling the melt dropped in step (iii) to at least partially crystallize the dropped melt; and (v) recovering the resulting powder or lozenge.

[0013] In a preferred embodiment, the at least one anhydrous alkaline earth salt or alkali metal salt is potassium acetate and / or potassium citrate and / or potassium phosphate and / or magnesium oxalate and / or magnesium sulfate and / or magnesium acetate and / or magnesium citrate and / or magnesium phosphate and / or magnesium oxalate and / or calcium sulfate and / or calcium acetate and / or calcium citrate and / or calcium phosphate and / or calcium oxalate. These anhydrous salts have been found to be particularly suitable for the preparation of the powders / lozenges according to the invention, and at the same time provide excellent protection for the fragile microcapsules embedded therein while providing excellent release characteristics.

[0014] More preferably, at least one anhydrous alkaline earth salt or alkali metal salt is sodium sulfate and / or sodium acetate and / or potassium citrate. When using these salts, the best crystallization behavior and protection of the fragile microcapsules were observed.

[0015] According to the most preferred embodiment, the components of the salt are sulfate, citrate or phosphate. This avoids the formation of the acetic acid odor tone in the final product formulation.

[0016] According to a second aspect, the present invention relates to a powder or a tablet (or a plurality of tablets) obtained by the process according to the present invention.

[0017] Furthermore, in a further aspect, the present invention relates to a consumer product selected from the group consisting of detergents and cleaning agents, personal care products, nutritional or recreational preparations, cosmetic or pharmaceutical preparations, perfume products or scented products, preferably scented fabric softeners, laundry perfumes, the product comprising a powder or a tablet or a plurality of tablets according to the present invention, i.e., at least one tablet.

[0018] Finally, the present invention relates to the use of a powder or a tablet according to the present invention for scenting a consumer product, preferably a consumer product according to the present invention.

[0019] That is, the inventors have found that the preparation process of the powder or incense tablet according to the present invention can provide such a powder or incense tablet for the efficient incorporation of the active ingredient in an encapsulated form that exhibits excellent release characteristics (performance) for a wide range of solid consumer product formulations and such consumer products. Thereby, a microcapsule encapsulated by a crystallized salt is obtained, which serves as a buffer to protect the fragile microcapsule from mechanical, chemical, and / or thermal effects during the preparation of the final consumer product (formulation) without adversely affecting the performance of the microcapsule in the consumer product (formulation). Based on this, the present dosage form enables the efficient incorporation of the active ingredient via microcapsules in solid consumer product formulations while simultaneously enabling the efficient and targeted release of the active ingredient, thus making it possible to overcome the drawbacks of the state of the art. The fragile microcapsules are embedded in the crystals to form a powder or incense tablet that can withstand harsh chemical and physical conditions. Based on the method as defined herein, it was possible to obtain a stable but at the same time fragile protection matrix that enables the targeted release of the active ingredient from the microcapsules embedded in the protective salt matrix.

[0020] The problems of the present invention are solved by the purpose of the independent claims of the patent. Preferred embodiments are apparent from the following description in the same way as the language of the independent claims of the patent.

[0021] Unless otherwise indicated, all ratios are by weight. Numerical examples given in the form "x to y" include the given values. When multiple preferred numerical ranges are specified in this form, all ranges created by combining the various endpoints are also included.

[0022] When the terms "at least one" or "one or more" are used herein, they refer to one or more, for example, 2, 3, 4, 5, 6, 7, 8, 9 or more.

[0023] The term "and / or" indicates that a connection exists or an alternative is provided.

Brief Description of the Drawings

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Mode for Carrying Out the Invention

[0033] Hereinafter, the present invention will be described in more detail.

[0034] Therefore, in a first aspect, the present invention relates to a process for preparing a powder or an incense tablet comprising, consisting of, or containing a plurality of microcapsules containing one or more components, comprising or consisting of the following steps: (i) (a) Mixing at least one anhydrous alkaline earth salt or alkali metal salt or a mixture of at least one anhydrous alkaline earth salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, and (c) optionally at least one humectant, wherein the humectant is selected from the group consisting of propylene glycol, ethylene glycol, dipropylene glycol, glycerol, sorbitol, and maltitol; (ii) Heating the mixture obtained in step (i) to produce a melt; (iii) Dropping the melt produced in step (ii) onto the surface of the object; (iv) Seeding and optionally cooling the melt dropped in step (iii) to at least partially crystallize the dropped melt; and (v) Recovering the obtained powder or incense tablet.

[0035] Preferably, the humectant is also included in the composition according to the present invention.

[0036] Surprisingly, microcapsules that are prone to breakage when mixed with other (solid) components of consumer product formulations tend to break and be crushed, so it has been found that such inorganic compositions enable efficient incorporation into a wide range of consumer product formulations, particularly solid consumer product formulations.

[0037] The present invention has been made in view of the drawbacks described above. In order to solve the above-mentioned drawbacks, the present invention provides a composition and a method for its preparation, enabling efficient incorporation of an active ingredient into a solid consumer product formulation having improved olfactory performance and stability, and / or enabling the preparation of such consumer products.

[0038] For the present invention, it is essential that at least one alkaline earth salt or alkali metal salt is an anhydrous alkaline earth salt or alkali metal salt due to the general entropy effect of the anhydrous salt. The use of hydrated salts did not provide the desired properties, namely high stability and improved performance. Furthermore, the products obtained using hydrated salts were not incorporated into solid consumer product formulations and showed insufficient storage stability.

[0039] According to the present invention, an anhydrous alkaline earth salt or alkali metal salt is considered to be a salt without water molecules bound to the salt molecule. Furthermore, the anhydrous alkaline earth salt or alkali metal salt is considered to have no water molecules in the salt crystal and is preferably commercially available as so-called anhydrous salts, respectively.

[0040] Therefore, within the scope of the present invention, hydrates are not used. A hydrate is a salt containing water molecules that are bound to the metal center or crystallized with the metal complex (water of crystallization or water of hydration) and are bound in a certain ratio as an essential part of the crystal.

[0041] Due to the entropy effect, a mixture containing (a) at least one anhydrous alkaline earth salt or alkali metal salt or a mixture of at least one anhydrous alkaline earth salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry containing at least one microcapsule containing at least one active ingredient or at least one capsule containing at least one active ingredient, and (c) optionally at least one humectant crystallizes after heating to form a melt (step (i)) and after dropping the melt onto the surface of the object (step (iii)).

[0042] According to a preferred embodiment, microcapsules are added to the composition according to the present invention by themselves. Thereby, each microcapsule contains at least one active ingredient.

[0043] The microcapsules of the composition according to the present invention can be any of those known to those skilled in the art.

[0044] Preferably, the microcapsules used within the scope of the present invention are such microcapsules, wherein the shell of at least one microcapsule is selected from the group consisting of a sol-gel polymer (e.g., silica), polysiloxane, polyacrylate, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polyamide, polypeptide, polysulfonate, polysaccharide, polyphenol polymer, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), poly(melamine-urea), or combinations thereof, and preferably, a shell material selected from the group consisting of a sol-gel polymer, polyacrylate, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polypeptide, polysaccharide, polyphenol polymer, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), or combinations thereof, or consists of them.

[0045] The composition according to the invention comprises at least one of said microcapsules, i.e. one of the abovementioned types of microcapsules is embedded in the polymer matrix of the invention, or a maximum of a plurality of microcapsules from two or more different microcapsules are embedded in the polymer matrix. Thereby, all of the microcapsules can be of the same type, i.e. all of the microcapsules are, for example, of the poly(melamine-formaldehyde) type, or a part of the microcapsules of component a) is, for example, of the poly(melamine-formaldehyde) type and the others are of the polyurea type, i.e. component a) can comprise, or consist of, a mixture of different types of microcapsules based on different encapsulating / shell materials.

[0046] Furthermore, the microcapsules used in the composition according to the invention can be loaded with different substances such as different active ingredients, i.e. the composition according to the invention comprises microcapsules with different core materials. However, according to a further preferred variant, all of the microcapsules comprise the same active ingredient(s).

[0047] According to a further preferred variant, the composition according to the invention comprises microcapsules that are different in both the core material and the shell material, similar to the core material.

[0048] However, preferably, the microcapsules according to component a) of the invention are selected from the group of capsule types consisting of poly(melamine-formaldehyde)-based microcapsules and isocyanate-based microcapsules such as, for example, polyurea-based and / or polyurethane-based microcapsules and mixtures thereof, and are preferably biodegradable.

[0049] According to another preferred embodiment, the microcapsules are added to the composition according to the invention in the form of an aqueous dispersion (microcapsule slurry). The capsule slurry is a dispersion of the capsules in water, and the capsule content is usually between 25% and 40% by weight based on the total slurry.

[0050] Preferably, the capsule slurry is used in the preparation of the composition according to the invention. This enables the preparation of a more stable and more flexible composition while at the same time enabling an efficient and targeted release of the active ingredient.

[0051] Advantageously, due to the entropy effect, the mixture crystallizes disorderly. This can also be expressed as a spontaneously occurring crystallization, and a powder or tablet with improved stability can be obtained.

[0052] In the context of the present invention, the powder or tablet can be represented as microcapsules or can at least contain microcapsules. In particular, the present invention can be understood in such a way that the preparation process of the powder or tablet can be understood as the preparation process of microcapsules in the form of the powder or tablet.

[0053] As a result, the present invention relates to a process for the preparation of a powder or tablet according to the invention which makes it possible to provide microcapsules with increased stability starting from at least one capsule slurry or one capsule. Their stability is justified by the presence of the disorderly crystallized alkaline earth salt and / or alkali metal salt used. At the same time, the resulting composition is not brittle, but rather shows a certain degree of flexibility, thereby enabling an efficient and stable incorporation into solid consumer product formulations during storage as well as during production.

[0054] Generally, microcapsules are particles that contain a core and a wall material surrounding the core. The core can be a solid, liquid or gaseous substance or a mixture of substances, which is surrounded by a polymer dense, permeable or semi-permeable wall material. The wall is usually formed by emulsification and coacervation of the core or precipitation of the polymer during interfacial polymerization. The core is also called the internal phase. Other names used for the wall include the external phase, shell or coating. The shell wall can contain one or more layers and can include additional coatings with coating substances. The diameter of the microcapsules usually varies within the range of 1 μm to 1,000 μm. The wall thickness is usually 0.5 μm to 150 μm, but can vary in the range of 5×10 -9 m to 5×10 -6 m. Usually, a loading of 25% to 95% by weight with respect to the core material is possible, but a loading of 1% to 99% by weight is also possible.

[0055] For example, hydrophobic active ingredients, such as a single fragrance (also called an aroma / odor substance or a perfume substance), a fragrance mixture (also called a mixture of aroma / odor substances or a mixture of perfume substances or essential oils), an aroma substance or a mixture of aroma substances, can be easily incorporated into a number of diverse application formulations through encapsulation.

[0056] Based on their properties, microcapsules are used in the printing industry, food industry (vitamins, fragrances, plant extracts, enzymes, microorganisms), agrochemicals (fertilizers, pesticides), feed industry (minerals, vitamins, enzymes, drugs, microorganisms), pharmaceutical industry, detergent industry, cosmetics industry, etc.

[0057] Various capsule walls or coating materials are known in the manufacture of microcapsules. The capsule wall can be made of natural, semi-synthetic or synthetic materials. Natural shell materials include gum arabic, agar, agarose, maltodextrin, alginic acid or its salts, such as sodium alginate and calcium alginate, fats and fatty acids, cetyl alcohol, collagen, chitosan, lecithin, gelatin, albumin, shellac, polysaccharides such as starch or dextran, polypeptides, protein hydrolysates, sucrose, 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, for example, polymers such as polyacrylate, polyamide, polyvinyl alcohol, polyvinyl pyrrolidone.

[0058] Depending on the type of capsule wall material and the manufacturing process, microcapsules with different properties in terms of diameter, size distribution and physical and / or chemical properties are formed in each case.

[0059] Preferably, the microcapsules used within the scope of the present invention are such microcapsules, wherein the shell of 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, polyphenol polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), poly(melamine-urea), or combinations thereof.

[0060] Preferably, the microcapsules according to the present invention are selected from the group consisting of the following capsule types: preferably biodegradable poly(melamine-formaldehyde) - based microcapsules and isocyanate - based microcapsules such as, for example, polyurea - based and / or polyurethane - based microcapsules.

[0061] In the context of the present invention, microcapsules are understood to be microparticles that contain at least one or more active ingredients (plural possible) as the core material within the capsule and are surrounded by a capsule shell or capsule wall as defined above. As active ingredients to be encapsulated according to the present invention, basically any material suitable for inclusion in microcapsules can be considered in the process according to the present invention. Preferably, hydrophobic or lipophilic, that is, water - insoluble or water - immiscible liquids or solids, as well as suspensions, can be regarded as active ingredients to be encapsulated. They are mainly non - polar substances. Such hydrophobic substances are almost always lipophilic, that is, they dissolve well in fats and oils.

[0062] The terms "microcapsules" and "capsules" or "hydrophobic" and "lipophilic" are used synonymously within the context of the present invention.

[0063] As indicated above, the microcapsules can be included as such in the composition according to the present invention, or alternatively, the microcapsules can be included in the form of a microcapsule slurry, that is, an aqueous dispersion of microcapsules.

[0064] The microcapsules according to the present invention contain at least one active ingredient as the core material (regardless of whether added as such or as a microcapsule slurry).

[0065] In the context of this specification, the core material is preferably a hydrophobic active substance, i.e., a substance having a specific effect or causing a specific reaction, such as a drug, an insecticide, a cosmetic active ingredient, a food active ingredient, etc. In particular, the hydrophobic active substance is a lipophilic or hydrophobic fragrance or aroma substance, or a lipophilic or hydrophobic essential oil or aroma (i.e., a mixture of a fragrance substance or an aroma substance, respectively), a cooling agent, a TRPV1 or TRPV3 modulator, a pungent taste or a substance that produces a warm or hot sensation on the skin or mucous membrane, or a substance that produces a tingling sensation in the mouth or throat, or an active ingredient having astringent effect, a substance derived from the group of insecticides, biocides, insecticides, repellents, food additives, cosmetic active ingredients, pharmaceutical active ingredients, dyes, dye precursors; pesticides, dyes, luminous paints, fluorescent brighteners, solvents, waxes, silicone oils, lubricants, printing coating agents for paper, or a mixture of two or more of the aforementioned active ingredients.

[0066] The microcapsules in the context of the present invention may have a core material in the form of a hydrophobic single aromatic substance or a single odorant substance, wherein the core material contains at least one single aromatic substance or a single odorant substance or a mixture thereof selected from one or more of the following groups: Extracts of natural raw materials, and their fractions, or components isolated therefrom; single fragrance substances from the hydrocarbon group; aliphatic alcohols; aliphatic aldehydes and acetals; aliphatic ketones and oximes; aliphatic sulfur-containing compounds; aliphatic nitriles; esters of aliphatic carboxylic acids; formate, acetate, propionate, isobutyrate, butyrate, isovalerate, pentanoate, hexanoate, crotonate, tiglate, 3-methyl-2-butenoate esters of acyclic terpene alcohols; acyclic terpene aldehydes and ketones and their dimethyl and diethyl acetals; formate, acetate, propionate, isobutyrate, butyrate, isovalerate, pentanoate, hexanoate, crotonate, tiglate and 3-methyl-2-butenoate esters of cyclic terpene alcohols, cyclic terpene aldehydes and ketones; cyclic alcohols; cyclic and cycloaliphatic ethers; cyclic and macrocyclic ketones; cycloaliphatic aldehydes; cycloaliphatic ketones; esters of cyclic alcohols; esters of cycloaliphatic carboxylic acids; aromatic hydrocarbons; araliphatic alcohols; esters of araliphatic alcohols and aliphatic carboxylic acids, araliphatic ethers; aromatic and araliphatic aldehydes; aromatic 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.

[0067] Specific examples of the above substances are known to those skilled in the art. A fragrance or odorant substance and a mixture of two or more of the above substances are chemical substances or compositions that impart, convey and / or modulate a specific odor or odor impression. Preferably, the said odor (impression) is regarded as pleasant.

[0068] The term "perfume" refers to encapsulated perfume. The terms "perfume", "encapsulated perfume" and "fragrance" can be used interchangeably.

[0069] In an alternative embodiment according to the present invention, the microcapsules according to the present invention use a flavor substance or essential oil, or an aroma substance or aroma, respectively, as an active ingredient to be encapsulated or as a core material. These are compositions containing at least one flavor substance or one aroma substance. Such compositions, especially mixtures of flavor substances or essential oils, preferably contain 2, 3, 4, 5, 6, 7, 8, 9, 10 or more flavor substances.

[0070] The perfume mixture or essential oil preferably includes, for example, ambergris oil; amyrrh oil; angelica seed oil; angelica root oil; anise oil; valerian oil; basil oil; oakmoss absolute; bay oil; mugwort oil; benzoin resin; bergamot oil; beeswax absolute; birch tar oil; bitter almond oil; savory oil; buckthorn leaf oil; cubeb oil; cade oil; calamus oil; camphor oil; cananga oil; cardamom oil; cascarilla oil; cassia oil; cassie absolute; castoreum absolute; cedar leaf oil; cedarwood oil; cistus 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; orris absolute; oakmoss absolute; elemi oil; tarragon oil; eucalyptus citriodora oil; eucalyptus oil; fennel oil; pine needle oil; galbanum oil; galbanum resin; geranium oil; grapefruit oil; guaiacwood 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; spearmint oil; caraway seed oil; labdanum oil; labdanum absolute; labdanum resin; lavandin absolute; lavandin oil; lavender absolute; lavender oil; lemongrass oil; rosemary oil; distilled lime oil; pressed lime oil; linalool oil; yomogi oil; bay leaf oil; mace oil; marjoram oil; mandarin oil; massoia bark oil; mimosa absolute; musk grain oil; musk tincture; muscat sage oil; nutmeg oil; myrrh absolute; myrrh oil; myrtle oil; clove leaf oil; clove flower oil; neroli oil; olibanum absolute; olibanum oil; opopanax oil; orange blossom absolute; orange oil; oregano oil; palmarosa oil; patchouli oil; perilla oil; peruvian balsam oil; parsley leaf oil; parsley seed oil; petitgrain oil; peppermint oil; pepper oil; pimento oil; pine oil; poly oil; rose absolute; rosewood oil; rose oil; rosemary oil; sage oil dalmatian; sage oil spanish;Sandalwood oil; celery seed oil; spike lavender oil; star anise oil; storax oil; taget oil; fir needle oil; tea tree oil; turpentine oil; 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-ylang oil; hyssop oil; civet absolute; cinnamon leaf oil; cinnamon bark oil and fractions thereof, or essential oils, concretes, absolutes, resins, resinoids, balsams, tinctures such as components isolated therefrom, are selected from the group of extracts from natural raw materials such as these.;

[0071] In a further variant of the invention, the aroma substance can also be encapsulated as the core material in the form of a single aroma, wherein the core material contains at least one single aroma or a mixture thereof as the active ingredient.;

[0072] However, preferably a single aromatic substance or odorant (i.e., a compound having an odor or smell, and thus all natural and synthetic substances that impart an olfactorily perceptible smell), or alternatively a mixture of aromatic substances or odorants (so-called perfume oils) is used as the active ingredient encapsulated by the shell of the microcapsules. More preferably, the said substances and mixtures of substances impart a pleasant smell to the consumer product.;

[0073] In a preferred variant of the invention, all of the microcapsules contained in the powder or incense tablet according to the invention are loaded with the same active ingredient(s). For example, all of the microcapsules contain a fragrance substance, and even more preferably the same fragrance substance.;

[0074] According to an alternative embodiment, the microcapsules contained in the powder or incense tablet according to the invention encapsulate different classes of active ingredients or different substances within the same class of active ingredients. For example, some of the microcapsules contain a specific fragrance substance while other microcapsules encapsulate another fragrance substance.;

[0075] Thereby, preferably, the core material is selected regardless of the shell material.

[0076] Thus, according to a further preferred variation of the present invention, the incense tablet of the present invention can contain one type of microcapsule or a mixture of two or more different types of microcapsules. Thereby, the microcapsules can vary in terms of the active ingredient composition (i.e., the core of the microcapsule) and / or the wall composition (i.e., the material of the capsule shell).

[0077] The single incense tablet composition or powder composition of the present invention may contain microcapsules (s) as defined above between 0.5 wt% and 10 wt% based on the total weight of the incense tablet composition or powder composition.

[0078] Thus, 0.5 wt% to 10 wt% of microcapsules can be incorporated into the final composition based on the total weight of the incense tablet, i.e., a single incense tablet of the composition according to the present invention contains 0.5 wt% to 10 wt% of microcapsules (s) as defined above. If the amount of the microcapsule components is kept within these ranges, a homogeneous distribution of the microcapsules within the incense tablet (s) can be achieved. Further, if the amount of component (b) is within the above range, the active ingredient can be efficiently incorporated into the final solid consumer product formulation by efficient protection by the surrounding salt matrix, i.e., the microcapsules do not break during the preparation process of the solid consumer product, and thus, the encapsulated active ingredient (s) can be effectively retained without loss, and as a result, as shown in the experimental section, the performance of the microcapsules is significantly improved.

[0079] According to a preferred embodiment, the amount of the microcapsules (s) is in the range of 0.5 wt% to 10 wt% based on the total weight of the powder or incense tablet, and more preferably in the range of 3 wt% to 8 wt% based on the total weight of the powder or incense tablet.

[0080] The microcapsules can be incorporated directly into the composition of the present invention or, alternatively, can be added in the form of a capsule slurry.

[0081] The composition of the present invention containing microcapsules encapsulating the active ingredient(s) can be efficiently incorporated into various solid consumer product formulations to enable efficient and targeted release of the active ingredient(s). Thus, the presence of the crystallized inorganic salt acts as a kind of shock-absorbing layer that protects the microcapsules from damage due to mechanical, chemical, and / or thermal effects, and thereby prevents premature release and decomposition of the active ingredient(s) during the preparation process of the consumer product.

[0082] To achieve an ideal distribution of the incense tablets and, by extension, an ideal distribution of the microcapsules embedded therein within the final solid consumer product formulation, it is further advantageous if the powder or powder particles of the incense tablets each have a diameter in the range of 100 μm to 1 cm, preferably 500 μm to 3 mm. Incense tablets that are too large result in a non-uniform distribution.

[0083] The said incense tablets or granules are preferably present in the form of tablets, pills, spheres, etc. having shapes such as spherical, hemispherical, compressed hemispherical, lentil-shaped, and oblong, and can be prepared by any method known to those skilled in the art.

[0084] Furthermore, the powder or incense tablets and microcapsules of the present invention may each further contain one or more components that improve the visual aesthetics of the final consumer product, such as a colorant. Additionally, additives and / or active ingredients such as optical brighteners, detergents, laundry activators, etc. may be included by the powder or incense tablets.

[0085] Process for preparation

[0086] In the first step of the process according to the invention, (a) at least one anhydrous alkaline earth salt or alkali metal salt or a mixture of at least one anhydrous alkaline earth salt and at least one anhydrous alkali metal salt is mixed with (b) at least one capsule slurry or at least one capsule (wherein the capsule contains at least one active ingredient) and (c) optionally at least one humectant.

[0087] In the context of the present invention, the components defined above apply equally here, that is, terms such as "microcapsule", "anhydrous salt", "humectant", "tablet", etc., as well as the corresponding amounts and properties defined above apply.

[0088] Preferably, the composition according to the invention contains a humectant. Thus, in a further preferred variant of the invention in step (i) of the process according to the invention, (a) at least one anhydrous alkaline earth salt or alkali metal salt or a mixture of at least one anhydrous alkaline earth salt and at least one anhydrous alkali metal salt is mixed with (b) at least one capsule slurry or at least one capsule (wherein the capsule contains at least one active ingredient) and (c) optionally at least one humectant.

[0089] Preferably, the humectant is selected from the group consisting of propylene glycol, ethylene glycol, dipropylene glycol, glycerol, sorbitol, and maltitol. These humectants have been found to be particularly suitable for the preparation of the powders or tablets according to the invention. The use of such polyols enables the preparation of highly stable products that can be incorporated into various consumer product formulations. Other substances such as microfibrillated cellulose did not achieve the desired properties.

[0090] Preferably, as the alkaline earth salt or alkali metal salt, anhydrous lithium sulfate and / or lithium acetate and / or lithium citrate and / or lithium phosphate and / or lithium oxalate and / or sodium sulfate and / or sodium acetate and / or sodium citrate and / or sodium phosphate and / or sodium oxalate and / or potassium sulfate and / or potassium acetate and / or potassium citrate and / or potassium phosphate and / or magnesium oxalate and / or magnesium sulfate and / or magnesium acetate and / or magnesium citrate and / or magnesium phosphate and / or magnesium oxalate and / or calcium sulfate and / or calcium acetate and / or calcium citrate and / or calcium phosphate and / or calcium oxalate. These are preferred salts as component (a).

[0091] In particular, sodium sulfate and / or sodium acetate and / or potassium citrate are used to obtain a powder or a tablet with significantly improved stability characteristics while at the same time enabling an efficient and targeted release of the active ingredient.

[0092] The crystalline salt matrix enables high release performance while protecting the microcapsules from chemical and mechanical influences. By virtue of this protection, it becomes possible to efficiently incorporate the loaded microcapsules into a wide range of consumer product formulations, particularly solid consumer product formulations. In the production of such compositions, the fragile microcapsules are subject to high shear, resulting in the breakage of the microcapsules and, as a result, an accelerated release of the active ingredient. Surprisingly, the compositions according to the invention can be advantageously incorporated into such formulations, thereby showing improved performance and chemical and mechanical stability within these formulations, during their production, and towards other components.

[0093] Suitable component (b) is defined above.

[0094] According to the present invention, the humectant is a hygroscopic substance used to keep the moisture of the mixture produced in step (i).

[0095] Preferably, a polyol, more preferably an aliphatic polyol, even more preferably propylene glycol or ethylene glycol or dipropylene glycol or glycerol or sorbitol or maltitol or a mixture thereof is used as the humectant.

[0096] Preferably, at least one encapsulated active ingredient is selected from the group consisting of odoriferous substances, fragrances, perfumes, essential oils, flavoring agents, cosmetic ingredients, pharmaceutical active ingredients, insect repellents, ingredients of oral care products and dental care products, latent heat storage media and adsorbents. More preferably, the ingredient is an odoriferous substance or a fragrance or an essential oil, and is added in a ratio of 0 wt% to 10 wt%, preferably 0 wt% to 6 wt% based on the total weight of the incense composition or powder composition.

[0097] According to the present invention, a capsule slurry or capsules can be used.

[0098] Preferably, the capsule slurry is a dispersion of capsules in water. More preferably, in order to obtain a powder or incense tablet with improved stability and improved sensory properties, the capsule content is between 25 wt% and 65 wt% (and preferably 25 wt% and 40 wt%) based on the total weight of the incense composition or powder composition. Alternatively, if there is no capsule slurry but at least one capsule is used, the capsule content is between 1 wt% and 80 wt% based on the total weight of the incense composition or powder composition.

[0099] According to another further preferred variation, the ratio of the capsules is 10 wt% to 70 wt% based on the total weight of the incense composition or powder composition, or the ratio of the capsule slurry contained in the composition according to the present invention is 1 wt% to 80 wt% (and even more preferably 10 wt% to 40 wt%).

[0100] If the amount of component (b) of the microcapsules is maintained within these ranges, a homogeneous distribution of the microcapsules within the incense tablet(s) can be achieved. Furthermore, if the amount of component (b) is within the above ranges, the active ingredient can be efficiently incorporated into the final solid consumer product formulation by the efficient protection provided by the surrounding salt matrix, i.e., the microcapsules do not break during the preparation process of the solid consumer product, and thus the encapsulated active ingredient can be effectively retained without loss. As a result, as shown in the experimental section, the performance of the microcapsules is significantly improved.

[0101] Preferably, the ratio of the alkaline earth salt and / or alkali metal salt is 20% to 99% by weight.

[0102] According to a further preferred modification, the ratio of the alkaline earth salt and / or alkali metal salt is 40% to 80% by weight based on the total weight of the incense tablet composition or powder composition.

[0103] If the salt component defined above is included within the above range in the composition according to the present invention, efficient protection of the fragile microcapsules within the crystalline salt matrix can be achieved while at the same time enabling efficient and targeted release of the active ingredient.

[0104] According to another further preferred modification, the composition according to the present invention contains a humectant. Preferably, the humectant is included in an amount of 0% to 5% by weight based on the total weight of the incense tablet composition or powder composition.

[0105] Preferably, the ratio of the humectant is 0% to 2.5% by weight, and even more preferably 0.1% to 2.5% by weight, based on the total weight of the incense tablet composition or powder composition.

[0106] Surprisingly, the presence of a humectant has been found to significantly improve the stability and performance of the compositions according to the present invention. In addition, when comparing samples with and without the addition of a humectant, the addition of the humectant not only improves the manufacture and preparation of more homogeneous incense tablets, but also more efficiently protects fragile microcapsules, and thus, by enabling a more targeted release of the fragrance, has been found to result in an improvement in the sensory experience. Surprisingly, the humectant component contained further enables the improvement of the properties of the final product and efficiently adjusts the viscosity and flexibility of the crystalline matrix, so that the matrix is not more brittle, but rather more flexible, the buffering effect is improved, and thus the protection of fragile microcapsules is enhanced, and the incorporation into solid consumer product formulations is facilitated without changing the basic chemical properties of the composition. Furthermore, surprisingly, the humectant component has been found to promote incense tablet formation and significantly improve the miscibility of the microcapsule component with the salt component and further optional components or additives, thereby enabling the achievement of a more homogeneous distribution of the microcapsules (and thus the active ingredients) within the crystalline matrix. By adding a humectant within the ranges defined above, it is possible to efficiently adjust the properties of the matrix, so that without changing the basic chemical properties of the plasticizing material, the buffering effect is improved, fragile microcapsules are better protected, and the incorporation into solid consumer product formulations is facilitated, and a matrix that is not more brittle but rather more flexible can be obtained.

[0107] Preferably, based on the total weight of the incense tablet composition or the powder composition, the ratio of the alkaline earth salt and / or the alkali metal salt is 20% to 99% by weight, the ratio of the capsules is 10% to 70% by weight or the ratio of the capsule slurry is 1% to 80% by weight, and optionally the ratio of the humectant is 0% to 2.5% by weight.

[0108] In order to obtain a powder or a tablet with improved stability and improved sensory properties, based on the total weight of the tablet composition or the powder composition, the ratio of the alkaline earth salt and / or the alkali metal salt is 40% to 80% by weight, the ratio of the capsule is 1% to 70% by weight, or the ratio of the capsule slurry is 1% to 80% by weight, and the ratio of the humectant is 0% to 5% by weight.

[0109] In the next step (ii) of the process according to the present invention, the mixture obtained in step (i) is heated to obtain a melt.

[0110] Preferably, the melting step (ii) is carried out at a temperature in the range of 40°C to 80°C in order to achieve a homogeneous distribution of the individual microcapsules in the crystalline buffer matrix. Preferably, the temperature is in the range of 40°C to 60°C, and even more preferably in the range of 40°C to 50°C.

[0111] In this step, additional additives such as adhesives, surfactants, plasticizers and / or structuring agents can be added and mixed to obtain a homogeneous mixture.

[0112] In the next step, tablets are formed by dropping the mixture / melt of step (ii) using state-of-the-art granulation processes known to those skilled in the art.

[0113] Granulation is a particle formation process, in which usually tablets are formed using a droplet forming device and then cooling the individual particles as obtained. The process for preparing tablets or granules is a commercially used method, and the tablets may be formed into various shapes including tablets, pills, spheres, etc. Furthermore, upscaling by dropping using a pulsator in air or in vegetable oil also showed good results.

[0114] Usually, the melt is dropped onto the surface, resulting in the formation of individual tablets.

[0115] In an embodiment of the present invention, the surface is cooled before and / or during dropping in order to improve the crystallization process of the melt.

[0116] Thus, in a further process step (iii) of the present invention, the melt produced in step (ii) is dropped onto the surface of the object, and the dropped melt is at least partially crystallized, followed by step (iv), i.e., seeding the dropped melt and optionally cooling it.

[0117] Seeding is crystallization using seed crystals. A seed crystal is a small piece of single crystal material or polycrystalline material, from which usually a large crystal of the same material is grown, i.e., crystal seeding is a technique widely adopted to provide a pre-formed mold (seed) to which new molecules can converge to form a crystal. Usually, the seed crystal has the same composition as the final crystal. Such a process is known to those skilled in the art.

[0118] Thus, within the scope of the present invention, the seed crystal has the same composition as the anhydrous salt used in step (i) of the present invention.

[0119] Seeding enables the formation of a homogeneous and stable crystal salt matrix embedding fragile microcapsules while at the same time enabling an efficient and targeted release of the active ingredient encapsulated in said microcapsules.

[0120] Seeding also has a significant effect on the reaction rate. During slow precipitation, i.e., while the salt matrix is formed slowly, the fragile capsules are pushed outwards. This results in a non-uniform capsule distribution. Therefore, the thin and fragile capsules are not well protected against external influences such as pressure.

[0121] Surprisingly, it has been found that seeding with seed crystals significantly promotes the formation of the salt matrix and contributes to a uniform distribution of the fragile capsules within this protective matrix. Thus, the microcapsules are better protected without adversely affecting the release characteristics.

[0122] Seeding affects the crystallization behavior and thus the final crystal structure, and therefore also affects the overall structure of the composition obtained according to the present invention. The crystals obtained via seeding exhibit different properties compared to crystals that do not contain any seed crystals.

[0123] Other components such as the presence of a humectant also affect the crystallization behavior and thus the final structure and properties.

[0124] Finally, the powder or tablets obtained as step (v) are recovered.

[0125] Generally, tablets are formed by dropping the mixture of step (iii) using state-of-the-art granulation processes known to those skilled in the art. Granulation is a particle formation process, and usually, tablets are formed using a droplet forming device.

[0126] In order to achieve a homogeneous distribution of the microcapsules, the powder particles of the powder or tablets each have a diameter of 100 μm to 1 cm, preferably 500 μm to 3 mm.

[0127] Furthermore, in a further aspect, the present invention relates to a composition prepared according to the process of the present invention.

[0128] In one embodiment of the present invention, the powder particles of the powder or tablets each have a weight in the range of 0.5 mg to 25 mg, preferably 1 mg to 5 mg.

[0129] The composition according to the present invention comprises or consists of at least one tablet having the composition defined above. Preferably, the composition is present as a plurality of tablets. Alternatively, the composition is present as a single tablet of the composition defined above.

[0130] Consumer product

[0131] Furthermore, in another aspect, the present invention relates to the use of the powder or tablets according to the present invention for the preparation of consumer product formulations. The terms "consumer product formulation" and "consumer product" are used synonymously within the context of the present invention.

[0132] Outstanding advantages of the powder or tablets according to the present invention obtained by the preparation process according to the present invention have been found in view of the preparation of solid consumer products such as powder detergents, laundry soaps, solid fabric softeners, deodorants, etc. Therefore, preferably, the consumer product according to the present invention is a solid consumer product.

[0133] When incorporated into a consumer product formulation, the microcapsules must be chemically stable in a rather active environment, but at the same time must also be mechanically stable when subjected to mechanical stresses such as during mixing and optionally under pressure of a solid consumer product formulation. However, generally, as the shell thickness increases, capsule breakage during processing by shear increases, resulting in deterioration of the release characteristics (release of the active ingredient). Surprisingly, it has been found that the composition according to the present invention based on microcapsules embedded in a crystalline salt matrix is particularly suitable for incorporation into solid consumer product formulations. The crystalline salt matrix protects the microcapsules while enabling high release performance.

[0134] Accordingly, in another preferred variant, the present invention also relates to the use of the powder or tablets according to the present invention for the preparation of consumer product formulations, wherein the consumer product or consumer product formulation is a solid product such as a fabric care product (e.g., powder detergent, laundry soap, solid fabric softener), solid soap, household product (e.g., solid WC cleaner, solid all-purpose cleaner, powder carpet cleaner, powder detergent for dishwashing or for cleaning various surfaces), personal care product (e.g., deodorant, soap), fragrance booster, aroma enhancer, pharmaceutical, and mixtures thereof.

[0135] Finally, in another aspect, the present invention relates to such consumer products or consumer product formulations that include or consist of the composition according to the present invention, i.e., the composition according to the first aspect of the present invention, the composition according to the second aspect of the present invention, and / or the composition obtained based on the process according to the third aspect of the present invention.

[0136] The powder or tablet of the present invention enables efficient incorporation of the active ingredient into a solid product formulation and enables efficient and targeted release of the active ingredient.

Examples

[0137] Hereinafter, the present invention will be described in more detail and specifically with reference to examples, which are not intended to limit the present invention.

[0138] Example 1: Microcapsules Crystallized with Sodium Sulfate and Incorporated into a Powder Detergent - Functional Evaluation

[0139] According to the first example, a composition comprising or consisting of at least one tablet containing microcapsules was prepared as follows: Anhydrous sodium sulfate was mixed with a microcapsule slurry (40% pure microcapsules; ratio of capsules to water 2:3) at a weight ratio of 1:1. The mixture was heated to 45 °C until a viscous mass was obtained. The mixture was then dropped and seeded using seed crystals (anhydrous sodium sulfate) to obtain the tablets according to the present invention. The microcapsules are based on a melamine formaldehyde capsule wall encapsulating a fragrance mixture. All the microcapsules have a particle size in the range of 10 - 70 μm.

[0140] In the context of the present invention, the powder or tablet according to the present invention can be shown as microcapsules crystallized with an anhydrous salt as mentioned in the present disclosure.

[0141] The sensory evaluation was conducted as follows: After preparing the incense tablets according to the present invention as described above, the incense tablets were mixed with a commercially available powder detergent and homogenized. The final dosage of the microcapsules in 40 g of the powder detergent was 0.2% by weight (corresponding to 0.8% by weight of the incense tablets in 40 g of the powder detergent).

[0142] Finally, the product was placed in a washing machine and the fabric (terry cloth) was washed at 30°C.

[0143] After rinsing, the fabric was air-dried at room temperature (hanging).

[0144] The corresponding powder detergent was used as a reference, and in this case, the microcapsules were added directly to the powder detergent.

[0145] Fragrance release was carried out in three steps. In the first step, the odor of the untreated dry cloth was smelled ("before rubbing"). In the second step, the odor of the lightly kneaded dry cloth was smelled; for this purpose, slight mechanical stress was applied by moving the cloth back and forth between both hands several times to break the capsules. In the third step, the dry cloth was rubbed strongly and the odor after the capsules were broken was smelled. After each step, the aroma intensity was evaluated.

[0146] To evaluate the sensory performance, 8 - 9 testers evaluated the aroma intensity on a scale of 1 (odorless) to 9 (very strong odor).

[0147] The results of the sensory evaluation are shown in Figure 1.

[0148] Samples containing the incense tablets according to the present invention, which contain microcapsules embedded in a protective crystal matrix, such as sodium sulfate crystals (see Figures 1 and 2), show efficient protection of the fragile microcapsules within the crystals while at the same time showing a considerably improved performance that enables efficient release of the active ingredient. The sodium sulfate crystals serve as a shock-absorbing layer in the manufacturing process of consumer products. Samples that do not contain such a shock-absorbing layer or samples that contain only a simple coating do not exhibit performance because most of the microcapsules have already been destroyed during the preparation of the consumer product.

[0149] Surprisingly, the best sensory performance was obtained using sodium acetate anhydrous. Furthermore, very good sensory performance is obtainable using potassium citrate anhydrous (see Figure 3).

[0150] However, it was important to use only salts without water such as sodium acetate without water (not present as a hydrate).

[0151] Example 2: Microcapsules Crystallized with Sodium Sulfate and Incorporated into Laundry Soap - Sensory Evaluation

[0152] According to the process described in Example 1, a plurality of incense tablets embedded with microcapsules were prepared.

[0153] Sensory evaluation was carried out as follows: When the composition according to the present invention was prepared, the obtained incense tablets as they were were combined with a commercially available laundry soap in the form of soap particles, the obtained mixture was passed through an extruder, and the final soap was cut into pieces.

[0154] Subsequently, the prepared laundry soap was applied by rubbing it on a wet cloth (toweling). After rinsing, the cloth was air-dried at room temperature.

[0155] A corresponding laundry soap not containing the composition of the present invention containing scented microcapsules was used as a reference.

[0156] Thereafter, commercially available powder detergent was mixed with the prepared incense tablets and homogenized.

[0157] Finally, the product was put into a washing machine, the cloth was washed at 30 °C, and then air-dried at room temperature.

[0158] Sensory evaluation was carried out according to Example 1. The results of the sensory evaluation are shown in Figure 2.

[0159] All samples showed significant improvements in performance based on the buffering function of sodium sulfate crystals in the preparation process of consumer products. Unprotected microcapsules are not suitable for the preparation of scented laundry soap because they are destroyed when mixed and homogenized with the powder detergent.

[0160] Example 3: Influence of various humectants

[0161] A plurality of incense tablets according to the present invention were prepared according to the process described in Example 1. The composition contained 75% by weight of salt (sodium sulfate) and 25% by weight of microcapsule slurry (containing 40% by weight of microcapsules based on the total weight of the slurry, i.e., 40% by weight of capsule loading) based on the total weight of the composition. These samples contained 0% by weight of humectant (moisturizing cream).

[0162] To show the influence of the humectant (sorbitol) component on the final product, the amount of the corresponding salt was reduced simultaneously while the amount of the humectant was increased stepwise (see Table 1).

[0163] [Table 1]

[0164] The results are shown in Figures 4a (0% humectant) and 4b (1%, 2.5% and 5%). Samples 2 and 3 showed excellent results. Good results were also achieved for Sample 1. No crystallization was observed for the sample containing 5% by weight of the humectant sorbitol.

[0165] Furthermore, it was found that the addition of a small amount of humectant contributed to the improvement of long-term stability, that is, the incense tablets maintained their structure over a long period of time and did not "collapse" or fall apart.

[0166] Therefore, it can be concluded that in order to achieve an excellent product with improved stability and performance over time, the ratio of the humectant should be in the range of 0 wt% to 2.5 wt% based on the total weight of the incense tablet or powder. Particularly good long-term results were achieved when the humectant was present in an amount of 1 wt% to 2.5 wt% based on the total weight of the incense tablet or powder.

[0167] The same experiment was also carried out with glycerol instead of sorbitol. The results are shown in Figure 5 (1%, 2.5%, 5%). Only Samples 2 and 3 showed sufficient results. Crystallization was not observed in the sample containing 5 wt% of the humectant glycerol.

[0168] The same experiment was also carried out with propylene glycol instead of sorbitol. The results are shown in Figure 6 (1%, 2.5%, 5%). Only Samples 2 and 3 showed sufficient results. Crystallization was not observed in the sample containing 5 wt% of the humectant propylene glycol.

[0169] The presence of the humectant was found to have a decisive influence on the crystallization behavior of the composition.

[0170] Example 4: Influence of Salt

[0171] According to the process described in Example 1, a plurality of incense tablets according to the present invention were prepared.

[0172] The composition contained 72.5 wt% of salt (sodium sulfate), 25 wt% of microcapsule slurry (containing 40 wt% of microcapsules based on the total weight of the slurry, i.e., 40 wt% of capsule loading), and 2.5 wt% of humectant (propylene glycol) based on the total weight of the composition.

[0173] In one example, the salt was anhydrous sodium sulfate (see Figure 7a), and in another example, it was hydrated sodium sulfate (sodium sulfate decahydrate) (see Figure 7b).

[0174] This result indicates that the anhydrous salt yields better crystallization results. The production was more difficult to handle. On the one hand, the desired crystal structure was hardly formed, and on the other hand, the resulting product was overall significantly moist and sticky. Powders or tablets could not be obtained. Such products could not be incorporated into powder formulations such as powder detergents. The final consumer product formulation would clump together immediately upon mixing. Therefore, within the scope of the present invention, the anhydrous salt is preferred.

[0175] The crystallization process of sodium sulfate was utilized. For this purpose, anhydrous sodium sulfate was mixed with a capsule slurry. The water in the capsule slurry formed a viscous but pluggable substance. By seeding the crystals, solids could be developed. However, sodium sulfate decahydrate dissolves in its own crystallization water at 32 °C. As a result, stable tablets could not be obtained even when using the hydrated salt.

[0176] Thus, it was found that it is disadvantageous for a salt, for example, sodium sulfate, to dissolve in its own crystallization water. As described above, the desired product cannot be obtained in this way, and not only the formation of tablets but also the incorporation into a powdered consumer product formulation is impossible.

[0177] On the other hand, by using anhydrous salts, it becomes possible to prepare a kind of paste that is easy to handle and can be easily processed into tablets that can be stably incorporated into powdered consumer product formulations.

[0178] Example 5: Influence of Seeding

[0179] Furthermore, in further examples, the crystallization behavior was analyzed depending on seeding.

[0180] For this purpose, two different compositions were prepared based on the following composition: 75 wt% salt (sodium sulfate), 25% microcapsules.

[0181] The composition contained 75 wt% salt (sodium sulfate) and 25 wt% microcapsule slurry (containing 40 wt% microcapsules based on the total weight of the slurry, i.e., 40 wt% capsule loading) based on the total weight of the composition. These samples contained 0 wt% humectant (moisturizing cream).

[0182] On the one hand, seed crystals (anhydrous sodium sulfate) were used to prepare incense tablets according to the process described in Example 1. The results are shown in Figure 8b (with seeding).

[0183] On the other hand, incense tablets were prepared according to the same process but without seeding, i.e., no seed crystals were added. The results are shown in Figure 8a (without seeding).

[0184] As can be seen from the figure, crystallization was not observed in the samples prepared without seeding. Incense tablets were not obtained; rather, wet, uncrystallized droplets were obtained. The product was further difficult to handle. On the one hand, the desired crystal structure was hardly formed, and on the other hand, the resulting product was overall significantly moist and sticky. Powders or incense tablets were not obtained. Such a product could not be incorporated into powder formulations such as powder detergents. As soon as it was mixed, the final consumer product formulation would clump together.

[0185] However, the addition of seed crystals resulted in complete crystallization, which in turn led to the formation of stable incense tablets. Therefore, it can be concluded that seeding is necessary for sufficient crystallization and thus the formation of the incense tablets according to the present invention. These incense tablets are easy to handle and can be stably incorporated into powder consumer product formulations.

[0186] Furthermore, it has been found that seeding can form a homogeneous and stable crystal salt matrix embedding fragile microcapsules while at the same time enabling an efficient and targeted release of the active ingredient encapsulated in the microcapsules.

[0187] Furthermore, seeding was found to have a significant impact on the reaction rate. During slow precipitation, i.e., the slow formation of the salt matrix, fragile capsules are pushed outwards. As a result, the distribution of the capsules becomes inhomogeneous. Therefore, fine and fragile capsules are not well protected from external influences such as pressure.

[0188] Surprisingly, seeding with seed crystals was found to significantly accelerate the formation of the salt matrix and contribute to the homogeneous distribution of fragile capsules within this protective matrix. Therefore, the microcapsules are much better protected without adversely affecting the release characteristics.

[0189] Since seeding affects the crystallization behavior, it also affects the final crystal structure and thus the overall structure of the composition obtained according to the present invention. The crystals obtained by seeding exhibit different properties, particularly in terms of stability, compared to crystals that do not contain seed crystals.

[0190] Example 6:

[0191] In another example, the incense tablets according to the present invention were prepared as follows: 1) Providing 25 g of sodium sulfate (anhydrous) - component (a) 2) Adding 16 g of capsule slurry (containing melamine - formaldehyde - based microcapsules at a concentration of 40 wt%; the ratio of capsules to water is 2:3) - component (b); 3) Adding 0.2 g of C18 - C22 hydroxyalkyl hydroxypropyl guar (stabilizer); 4) Heating the mixture at 45 °C in a warm bath; 5) Adding a very thin layer of sodium sulfate (anhydrous) for seeding; 6) Forming small droplets of the mixture; and 7) Adding the as - obtained incense tablets to the final product formulation (detergent).

[0192] C18-C22 hydroxyalkyl hydroxypropyl guar was added as a stabilizer.

[0193] Furthermore, a scented tablet containing microcapsules without a protective salt layer was prepared for comparison.

[0194] The results of the sensory evaluation are shown in Fig. 9 (left: without the protective salt matrix, right: with the protective salt matrix according to the present invention).

[0195] The results indicate that the protection of the fragile microcapsules according to the present invention considerably improves the olfactory properties of the final product formulation. By adding a stabilizer, this effect could be further improved.

Claims

1. A process for preparing a powder or a tablet consisting of or containing a plurality of microcapsules containing components of 1 or more, comprising the following steps: (i) (a) At least one anhydrous alkaline earth salt or alkali metal salt or a mixture of at least one anhydrous alkaline earth salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, and (c) optionally at least one humectant are mixed, wherein the humectant is selected from the group consisting of propylene glycol, ethylene glycol, dipropylene glycol, glycerol, sorbitol, and maltitol; (ii) Heating the mixture obtained in step (i) to produce a melt; (iii) Dropping the melt produced in step (ii) onto the surface of the object; (iv) Seeding and optionally cooling the melt dropped in step (iii) to at least partially crystallize the dropped melt; (v) A process for preparing the powder or the tablet, comprising or including recovering the obtained powder or the tablet.

2. Based on the total weight of the tablet or powder, the ratio of the alkaline earth salt and / or alkali metal salt is 20% to 99% by weight, the ratio of the capsules is 10% to 70% by weight or the ratio of the capsule slurry is 1% to 80% by weight, and optionally the ratio of the humectant is 0% to 2.5% by weight. The process for preparing the powder or tablet according to claim 1.

3. The process for preparing the powder or tablet according to claim 1 or 2, wherein the melting step (ii) is carried out at a temperature in the range of 40°C to 80°C.

4. The process for preparing the powder or tablet according to any one of claims 1 to 3, wherein the surface is cooled before and / or during dropping.

5. As the alkaline earth salt or alkali metal salt, anhydrous lithium sulfate and / or lithium acetate and / or lithium citrate and / or lithium phosphate and / or lithium oxalate and / or sodium sulfate and / or sodium acetate and / or sodium citrate and / or sodium phosphate and / or sodium oxalate and / or potassium sulfate and / or potassium acetate and / or potassium citrate and / or potassium phosphate and / or magnesium oxalate and / or magnesium sulfate and / or magnesium acetate and / or magnesium citrate and / or magnesium phosphate and / or magnesium oxalate and / or calcium sulfate and / or calcium acetate and / or calcium citrate and / or calcium phosphate and / or calcium oxalate, particularly sodium sulfate and / or sodium acetate and / or potassium citrate are used, the preparation process of the powder or incense tablet according to any one of claims 1 to 4.

6. The preparation process of the powder or incense tablet according to any one of claims 1 to 5, wherein a polyol, preferably an aliphatic polyol, more preferably propylene glycol or ethylene glycol or dipropylene glycol or glycerol or sorbitol or maltitol or a mixture thereof is used as a humectant.

7. The preparation process of the powder or incense tablet according to any one of claims 1 to 6, wherein at least one component is selected from the group consisting of odor substances, fragrances, perfumes, essential oils, flavoring agents, cosmetic ingredients, pharmaceutically active ingredients, insect repellents, components of oral care products and dental care products, latent heat storage media and adsorbents.

8. The preparation process of the powder or incense tablet according to any one of claims 1 to 7, wherein the at least one component is an odor substance or a fragrance or an essential oil, and is added in a ratio of 0 wt% to 10 wt%, preferably 0 wt% to 6 wt% based on the total weight of the incense tablet or powder.

9. The process for preparing the powder or the incense tablet according to any one of claims 1 to 8, wherein the at least one capsule has a wall material comprising one or more substances selected from the group consisting of natural, semi-synthetic and fully synthetic shell materials, preferably melamine formaldehyde resin, gelatin, alginate, polyurethane, polyamine and polyurea, or one or more such substances comprise one or more such substances, or are based on one or more such substances.

10. A powder or an incense tablet obtained by the process according to any one of claims 1 to 9.

11. The powder or the incense tablet according to claim 10, wherein the powder particles of the powder or the incense tablet each have a diameter in the range of 100 μm to 1 cm, preferably 500 μm to 3 mm.

12. The powder or the incense tablet according to claim 10 and / or 11, wherein the powder particles of the powder or the incense tablet each have a weight in the weight range of 0.5 mg to 25 mg, preferably 1 mg to 5 mg.

13. A consumer product, selected from the group consisting of detergents and cleaning agents, personal care products, nutritional or recreational preparations, cosmetic or pharmaceutical preparations, perfume products or scented products, preferably fragrant rinses, laundry perfumes, the consumer product comprising the powder or the incense tablet according to claims 10 to 12 or more incense tablets.

14. Use of the powder or the incense tablet according to claims 10 to 12 for scenting a consumer product, preferably the consumer product according to claim 13.

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