Method for preparing powder or lozenge

Abstract

The present invention relates to the field of perfuming particles, in particular perfuming particles for use in solid consumer product formulations, such as textile care products or the like. More specifically, the present invention relates to a method of preparing a powder or lozenge consisting of or comprising a plurality of microcapsules, the microcapsules containing one or more ingredients. In addition, the invention also relates to a powder or lozenge obtained by said method. The invention further relates to a consumer product comprising a powder or a lozenge or a plurality of lozenges according to the invention, and to the use of a powder or a lozenge for perfuming a consumer product according to the invention.

Description

Technical Field

[0001] The present invention relates to the field of perfumed particles, in particular perfumed particles for solid consumer product formulations, such as textile care products or the like. More specifically, the present invention relates to a method for preparing a powder or a pastille consisting of or comprising a plurality of microcapsules, said microcapsules containing at least one active ingredient. In addition, the present invention also relates to a powder or a pastille obtained by the method according to the present invention. The present invention further relates to a consumer product comprising a powder or a pastille or a plurality of pastilles (i.e. a plurality of pastilles) according to the present invention, and to the use of a powder or a pastille according to the present invention for perfumery of a consumer product according to the present invention. Background Art

[0002] Nowadays, many consumer products such as detergents, fabric softeners, washing powders, deodorants, lotions, etc. are scented with fragrance materials or contain cosmetic ingredients to achieve specific effects.

[0003] Unfortunately, often, for example, the aromatic substances or cosmetic ingredients of such products interact with other components of the product formulation, or the components of the perfume formulation with greater volatility tend to evaporate prematurely. Therefore, this leads to undesirable changes and / or reductions in the desired effects such as the fragrance impression, or causes the cosmetic ingredients to be "used" prematurely over time, or may even cause adverse reactions with other components of the product formulation, resulting in a decrease in product quality and / or stability. In order to prevent possible interactions between fragrances or other active ingredients and other ingredients of the product, or, for example, to prevent the volatilization of fragrances and therefore not distort or reduce the desired olfactory impression, the fragrances or other active ingredients can be added to the formulation in an encapsulated form. In this way, for example, the desired olfactory impression can be guaranteed based on the targeted release of the active ingredients. In addition, the interactions between the product components can be reduced, thereby allowing improved product quality and storage stability.

[0004] Therefore, a wide variety of consumer products contain encapsulated active ingredients, such as fragrances, in their formulations. For example, textile care formulations such as liquid detergents or fabric softeners contain a large number of such fragranced microcapsules. In addition, the formulations need to incorporate preservatives to increase their stability and durability, such as methylisothiazolinone (MIT), which may cause allergic reactions or skin irritation, while powdered detergents generally do not require the addition of preservatives and reduce environmental pollution. However, the incorporation of microcapsules in powdered formulations (such as powdered detergents) is even more difficult, because the mixing of microcapsule components and other solid detergent components can lead to the rupture of fragile microcapsules, resulting in, for example, a loss of olfactory properties.

[0005] It is particularly difficult to prepare microcapsules with both good stability and good release characteristics. The ability of the capsule to retain the active ingredient and therefore prevent the loss of volatile components depends in particular on the stability of the capsule in the product matrix. However, very stable microcapsules, such as capsules with relatively thick capsule walls, generally tend to show low performance because the targeted rupture of the microcapsules and therefore the release of the one or more active ingredients is hindered. However, if they are too unstable, they are already damaged or cause leakage of the active ingredient during storage or manufacturing, and cannot function. Therefore, the enhancement of the capsule wall, i.e., a multilayer microcapsule shell or a thicker shell, respectively, also leads to performance degradation, because the targeted release of the active ingredient is difficult, and the microcapsules generally require a complex multi-step preparation process.

[0006] Furthermore, solid consumer products (e.g., solid hair care products, soaps, and solid shower gels) are showing a new growth trend in view of the increasing public ecological awareness (reduced waste, reduced preservatives, etc.), making solid consumer products increasingly valuable, not only in the cosmetics industry, but also in other industries. However, as noted above, the incorporation of microcapsules in powdered formulations is rather difficult, since mixing of the microcapsule components with other, usually solid, detergent components can lead to the rupture of the fragile microcapsules.

[0007] There is therefore a need for improved efficient incorporation of active ingredients, such as perfuming ingredients, into solid consumer product formulations which, however, at the same time allows for an effective and targeted release of said active ingredients.

[0008] In particular, there is a need to provide such formulations comprising such active ingredients, wherein the active ingredients have improved efficacy and stability.

[0009] In particular, there is a need to provide compositions comprising such active ingredients for use in such consumer product formulations, in particular textile treatment compositions, which have improved olfactory properties and stability.

[0010] At the same time, in order to meet the high demands, compositions for solid consumer product formulations should be more accessible and the resulting compositions should exhibit improved properties, for example in terms of their olfactory qualities. Summary of the invention

[0011] The present invention is made in view of the disadvantages described above. In order to solve the above disadvantages, the present invention provides a method for preparing a composition, which allows active ingredients with improved olfactory properties and stability to be effectively incorporated into solid consumer product formulations, as well as for preparing the consumer product itself.

[0012] Thus, in a first aspect, the present invention relates to a method for preparing a powder or a lozenge consisting of or comprising a plurality of microcapsules containing one or more active ingredients, the method consisting of or comprising the following steps:

[0013] (i) mixing the following components (a), (b) and (c): (a) at least one anhydrous alkaline earth or alkali metal salt, or a mixture of at least one anhydrous alkaline earth metal salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, (c) optionally at least one humectant, wherein the humectant is selected from propylene glycol or ethylene glycol or dipropylene glycol or glycerol or sorbitol or maltitol;

[0014] (ii) heating the mixture obtained in step (i) to produce a melt;

[0015] (iii) dropping the melt produced in step (ii) onto a surface of an object;

[0016] (iv) seeding and optionally cooling the melt dripping in step (iii) to at least partially crystallize the dripping melt; and

[0017] (v) collecting the powder or tablets obtained.

[0018] In a preferred embodiment, the at least one anhydrous alkaline earth 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. It has been found that these anhydrous salts are particularly suitable for preparing the powder / lozenge composition according to the invention and provide excellent protection for the fragile microcapsules embedded therein while providing excellent release properties.

[0019] More preferably, the at least one anhydrous alkaline earth or alkali metal salt is sodium sulfate and / or sodium acetate and / or potassium citrate. When these salts are used, optimal crystallization behavior and protection of fragile microcapsules are observed.

[0020] According to a most preferred embodiment, the salt component is a sulfate, a citrate or a phosphate. This avoids the formation of acetic acid odor in the final product formulation.

[0021] According to a second aspect, the present invention relates to a powder or a pastille (or pastilles) obtained by a process according to the present invention.

[0022] Furthermore, in another aspect, the present invention relates to a consumer product selected from detergents and cleaners, personal care products, nutritional or conditioning preparations, cosmetic or pharmaceutical preparations, perfumed products or products to be perfumed, preferably fragrance rinses, laundry fragrances, said product comprising a powder or a pastille or a plurality of pastilles, i.e. at least one pastille, according to the invention.

[0023] Finally, the invention relates to the use of a powder or a pastille according to the invention for perfuming a consumer product, preferably a consumer product according to the invention.

[0024] That is, the inventors have found that the method for preparing powder or lozenge according to the present invention allows to provide such a powder or lozenge, which is used to effectively incorporate active ingredients into a wide range of solid consumer product formulations and consumer products themselves in an encapsulated form showing excellent release characteristics (performance). Thus, microcapsules encapsulated by crystalline salts can be obtained, which act as buffers, protecting fragile microcapsules from mechanical, chemical and / or thermal influences in the process of preparing final consumer products (preparations), without negatively affecting the performance of the microcapsules in the consumer products (preparations). Based on this, the dosage form of the present invention allows active ingredients to be effectively incorporated into solid consumer product formulations via microcapsules, while allowing the effective and targeted release of the active ingredients, thereby overcoming the shortcomings of the prior art. The fragile microcapsules are embedded in the crystals forming the powder or lozenge, which can even withstand harsh chemical and physical conditions. Based on the method as clearly described herein, a stable but flexible protective matrix can be obtained, which allows the active ingredient to be released in a targeted manner from the microcapsules embedded in the protective salt matrix.

[0025] The problem of the invention is solved by the subject-matter of the independent claims. Preferred embodiments are evident from the wording of the dependent claims and the following description.

[0026] Unless otherwise indicated, all percentages are by weight. Numerical examples given in the form of "x to y" include the values ​​given. When multiple preferred numerical ranges are explicitly stated in this format, all ranges resulting from combining the various endpoints are also included.

[0027] As used herein, the term "at least one" or "one or more" means 1 or more, for example 2, 3, 4, 5, 6, 7, 8, 9 or more.

[0028] The term "and / or" indicates that there is a combination or that alternatives are provided. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 : Figure 1 The results of a sensory evaluation of the performance (ie release performance) of the pastilles according to the invention incorporated into detergents are shown.

[0030] Figure 2 : Figure 2 The results of a sensory evaluation of the performance (ie release performance) of a pastille according to the invention incorporated into a laundry soap are shown.

[0031] Figure 3 : Figure 3 Shown is a comparison of the results of a sensory evaluation of the performance (ie release performance) of different pastilles according to the invention, each incorporated into a detergent.

[0032] Figure 4: Figure 4a and 4b The effect of the humectant sorbitol is shown.

[0033] Figure 5 : Figure 5 The effect of the humectant glycerin is shown.

[0034] Figure 6 : Figure 6 The effect of the humectant polypropylene glycol is shown.

[0035] Figure 7: Figure 7a and 7b The effect of hydrated salt is shown.

[0036] FIG8 : FIG8 shows the effect of seeding during the process ( Figure 8a : No seeding was performed; Figure 8b : Seeding crystal).

[0037] Fig. 9 : Fig. 9 The results of a sensory evaluation of the performance (ie release performance) of the pastilles according to the invention incorporated into detergents are shown. DETAILED DESCRIPTION OF THE INVENTION

[0039] Hereinafter, the present invention is described in more detail.

[0040] Thus, in a first aspect, the present invention relates to a method for preparing a powder or a tablet consisting of or comprising a plurality of microcapsules containing one or more ingredients, the method consisting of or comprising the following steps:

[0041] (i) mixing the following components (a), (b) and (c): (a) at least one anhydrous alkaline earth or alkali metal salt, or a mixture of at least one anhydrous alkaline earth metal salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, (c) optionally at least one humectant, wherein the humectant is selected from propylene glycol or ethylene glycol or dipropylene glycol or glycerol or sorbitol or maltitol;

[0042] (ii) heating the mixture obtained in step (i) to produce a melt;

[0043] (iii) dropping the melt produced in step (ii) onto a surface of an object;

[0044] (iv) seeding and optionally cooling the melt dripping in step (iii) to at least partially crystallize the dripping melt; and

[0045] (v) collecting the powder or tablets obtained.

[0046] Preferably, a humectant is also included in the composition according to the invention.

[0047] It has surprisingly been found that such inorganic compositions allow efficient incorporation in a wide variety of consumer product formulations, in particular solid consumer product formulations, since the fragile microcapsules tend to break or be crushed when mixing them with other (solid) components in the consumer product formulation.

[0048] The present invention is made in view of the disadvantages described above. In order to solve the above disadvantages, the present invention provides a composition and a method for preparing the same, which allows active ingredients with improved olfactory performance and stability to be effectively incorporated into solid consumer product formulations, and / or used to prepare the consumer product itself.

[0049] It is essential to the present invention that the at least one alkaline earth or alkali metal salt is an anhydrous alkaline earth or alkali metal salt due to the general entropic effects of such anhydrous salts. The use of aqueous salts does not provide the desired properties, i.e. increased stability and improved performance. Furthermore, the products obtained using aqueous salts cannot be incorporated into solid consumer product formulations and exhibit insufficient storage stability.

[0050] According to the present invention, anhydrous alkaline earth or alkali metal salts can be considered as salts without water molecules attached to the salt molecules. In addition, the anhydrous alkaline earth or alkali metal salts can be considered as containing no water molecules in the salt crystals, preferably because they are each commercially available as their so-called anhydrous salts.

[0051] Hydrates are therefore not used within the scope of the present invention. Hydrates are salts which contain water molecules which are bound in certain proportions to form a component of the crystal, either to the metal center or to the metal complex crystallization (water of crystallization or water of hydration).

[0052] Due to the entropic effect, a mixture comprising the following components (a), (b) and (c) crystallizes after heating and producing a melt (step (i)) and after dripping the melt onto a surface of an object (step (iii)): (a) at least one anhydrous alkaline earth or alkali metal salt, or a mixture of at least one anhydrous alkaline earth metal salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry, the capsule slurry comprising at least one microcapsule containing at least one active ingredient, or at least one capsule containing at least one active ingredient, (c) optionally at least one humectant.

[0053] According to a preferred embodiment, the microcapsules are added as such to the composition according to the invention. Thus, each microcapsule contains at least one active ingredient.

[0054] The microcapsules of the composition according to the invention may be any microcapsules known to a person skilled in the art.

[0055] Preferably, the microcapsules used within the scope of the present invention are such microcapsules, wherein the shell of the at least one microcapsule comprises a shell material or consists of a shell material selected from the group consisting of sol-gel polymers (e.g. silica gel), polysiloxanes, polyacrylates, polyacrylamides, poly(acrylate-co-acrylamides), polyureas, polyurethanes, polyamides, polypeptides, polysulfonates, polysaccharides, polyphenol polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), poly(melamine-urea) or combinations thereof, and preferably selected from the group consisting of sol-gel polymers, polyacrylates, polyacrylamides, poly(acrylate-co-acrylamides), polyureas, polyurethanes, polypeptides, polysaccharides, polyphenol polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde) or combinations thereof.

[0056] The composition according to the invention comprises at least one of said microcapsules, i.e. either a single microcapsule of the above-mentioned type is embedded in the polymer matrix according to the invention, or two or more different microcapsules, up to a large number of microcapsules, can be embedded in said polymer matrix. Thus, all microcapsules can be of the same type, i.e. all microcapsules are, for example, based on poly(melamine-formaldehyde), or some of the microcapsules of component a) are, for example, based on poly(melamine-formaldehyde) and other microcapsules are based on polyurea, i.e. component a) can comprise or consist of a mixture of different types of microcapsules based on different encapsulation materials / shell materials.

[0057] In addition, the microcapsules used in the composition according to the invention can be loaded with different materials, for example loaded with different active ingredients, i.e. the composition according to the invention comprises different microcapsules which differ in their core material. However, according to a further preferred variant, all microcapsules contain the same active ingredient.

[0058] According to a further preferred variant, the composition according to the invention comprises different microcapsules which differ in their core material and in their shell material.

[0059] Preferably, however, the microcapsules of component a) according to the invention are chosen from the group of capsule types consisting of poly(melamine-formaldehyde)-based microcapsules and isocyanate-based microcapsules, such as polyurea-based and / or polyurethane-based microcapsules, and mixtures thereof, and they are preferably biodegradable.

[0060] 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). Capsule slurry is a dispersion of capsules in water and the capsule content is generally 25 to 40% by weight, based on the total slurry.

[0061] Preferably, a capsule slurry is used to prepare the composition according to the invention. This allows a more stable and flexible composition to be easily prepared, while allowing an effective and targeted release of the active ingredient.

[0062] Advantageously, due to the entropic effect, the mixture crystallizes in a disordered manner. This can be further described as a spontaneously occurring crystallization, and this spontaneous crystallization enables powders or tablets with increased stability to be obtained.

[0063] In the context of the present invention, a powder or a tablet may be denoted as a microcapsule or may at least contain a microcapsule. In particular, the present invention may be understood as follows: a method for preparing a powder or tablet may be understood as a method for preparing microcapsules in the form of a powder or tablet.

[0064] The present invention therefore relates to a method for preparing a powder or a tablet according to the invention, which allows, starting from said at least one capsule slurry or one capsule, to provide microcapsules with improved stability. These stabilities are due to the presence of the disordered crystallized alkaline earth and / or alkali metal salts used. At the same time, the composition obtained is not brittle, but exhibits a certain degree of flexibility, thereby allowing efficient and stable incorporation into solid consumer product formulations both during manufacture and storage.

[0065] Typically, microcapsules are particles comprising a core and a wall material (which surrounds the core), wherein the core can be a solid, liquid or gaseous substance or a mixture of substances, which is surrounded by a dense, permeable or semi-permeable wall material of the polymer type. The wall is usually formed by precipitation of polymers during emulsification and coagulation or interfacial polymerization. The core is also called the inner phase. Other names for the wall include the outer phase, shell or coating. The shell wall may contain one or more layers and may contain an additional coating with a coating material. The diameter of the microcapsule typically varies in the range of 1 μm to 1000 μm. The wall thickness is typically 0.5 μm to 150 μm, but may also be 5×10 -9 m to 5×10 -6 Typically, the loading of the core material may be from 25 wt % to 95 wt %, but loadings of from 1 wt % to 99 wt % are also possible.

[0066] For example, hydrophobic active ingredients, such as single fragrances (also called fragrance / odorous substances or fragrance substances), fragrance mixtures (also called mixtures of fragrance / odorous substances or mixtures of fragrance substances or perfume oils), fragrance substances or mixtures of fragrance substances, can be easily incorporated into a large number of different application formulations by encapsulation.

[0067] Based on the properties of microcapsules, they are used in the printing industry, food industry (vitamins, condiments, plant extracts, enzymes, microorganisms), agricultural chemistry (fertilizers, pesticides), feed industry (minerals, vitamins, enzymes, drugs, microorganisms), pharmaceutical industry, detergent industry and cosmetics industry, etc.

[0068] A wide variety of capsule walls or coating materials are known for making microcapsules. The capsule wall can be made of natural, semisynthetic or synthetic materials. Natural shell materials include gum arabic, agar, agarose, maltodextrin, alginic acid or its salts, such as sodium alginate or calcium alginate, fats and fatty acids, cetyl alcohol, collagen, chitosan, lecithin, gelatin, albumin, shellac, polysaccharides, such as starch or dextran, polypeptides, protein hydrolysates, sucrose and waxes. Semisynthetic capsule wall materials include chemically modified cellulose, especially cellulose esters and cellulose ethers, such as cellulose acetate, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose and carboxymethyl cellulose, and starch derivatives, especially starch ethers and starch esters. Synthetic shell materials are, for example, polymers, such as polyacrylates, polyamides, polyvinyl alcohol or polyvinyl pyrrolidone.

[0069] Depending on the type of capsule wall material and the manufacturing process, the microcapsules formed have different properties in each case with regard to diameter, size distribution and physical and / or chemical properties.

[0070] Preferably, the microcapsules used within the scope of the present invention are such microcapsules, wherein the shell of the at least one microcapsule comprises or consists of a shell material selected from sol-gel polymers (e.g. silica gel), polysiloxanes, polyacrylates, polyacrylamides, poly(acrylate-co-acrylamides), polyureas, polyurethanes, polyamides, polypeptides, polysulfonates, polysaccharides, polyphenol polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), poly(melamine-urea) or combinations thereof.

[0071] Preferably, the microcapsules according to the invention are selected from the group of capsule types consisting of poly(melamine-formaldehyde)-based microcapsules and isocyanate-based microcapsules, such as polyurea-based and / or polyurethane-based microcapsules, which are preferably biodegradable.

[0072] In the context of the present invention, microcapsules are understood to be particles which contain at least one or more active ingredients as core material in the interior of the capsule and which are surrounded by a capsule shell or capsule wall as explicitly indicated above. As active ingredient to be encapsulated according to the invention, in the method according to the invention, basically any material suitable for inclusion in a microcapsule can be considered. Preferably, hydrophobic or lipophilic, i.e. water-insoluble or water-immiscible liquids or solids and suspensions can be considered as active ingredients to be encapsulated. These are primarily non-polar substances. Such hydrophobic substances are almost always lipophilic, i.e. they dissolve well in fats and oils.

[0073] In the context of the present invention, the terms "microcapsule" and "capsule" or "hydrophobic" and "lipophilic" are used synonymously.

[0074] As indicated above, the microcapsules may be included in the composition according to the invention directly or, alternatively, in the form of a microcapsule slurry, ie an aqueous dispersion of microcapsules.

[0075] The microcapsules according to the invention comprise at least one active ingredient as the core material (whether added directly or as a microcapsule slurry).

[0076] In the context of the present 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, pesticide, cosmetic active ingredient, food active ingredient, etc. In particular, the hydrophobic active substance is a lipophilic or hydrophobic aromatic or fragrance substance or a lipophilic or hydrophobic perfume oil or fragrance (i.e., a fragrance substance or a mixture of fragrance substances, respectively), a cooling agent, a TRPV1 or TRPV3 modulator, a substance that produces a spicy taste or a warm or hot sensation on the skin or mucous membranes, or a substance that produces a tingling sensation in the mouth or throat, or an active ingredient with an astringent effect, a pesticide, a biocide, an insecticide, a substance from the group of insect repellents, a food additive, a cosmetic active ingredient, a pharmaceutical active ingredient, a dye, a dye precursor, an agrochemical, a dye, a luminescent pigment, an optical brightener, a solvent, a wax, a silicone oil, a lubricant, a paper printing coating, or a mixture of two or more of the above active ingredients.

[0077] The microcapsules in the context of the present invention may have a core material in the form of a hydrophobic individual fragrance substance or individual odorant substance, wherein the core material comprises at least one individual fragrance substance or individual odorant substance or a mixture thereof, which is selected from one or more of the following groups:

[0078] Extracts of natural raw materials and also fractions thereof or components isolated therefrom; individual aromatic substances from the group of hydrocarbons; aliphatic alcohols; aliphatic aldehydes and acetals; aliphatic ketones and oximes; aliphatic sulfur compounds; aliphatic nitriles; esters of aliphatic carboxylic acids; formates, acetates, propionates, isobutyrates, butyrates, isovalerates, valerates, hexanoates, crotonates, tiglates and 3-methyl-2-butenoates of acyclic terpene alcohols; acyclic terpene aldehydes and ketones and their dimethyl and diethyl acetals; formates, acetates, propionates, isobutyrates, butyrates, isovalerates, valerates, hexanoates, crotonates, tiglates and 3-methyl-2-butenoates of cyclic terpene alcohols Esters, isovalerates, valerates, caproates, crotonates, tiglates and 3-methyl-2-butenoates; cyclic terpene aldehydes and ketones; cyclic alcohols; cyclic and alicyclic ethers; cyclic ketones and macrocyclic ketones; alicyclic aldehydes; alicyclic ketones; esters of cyclic alcohols; esters of alicyclic carboxylic acids; aromatic hydrocarbons; aromatic aliphatic alcohols; esters formed from aromatic aliphatic alcohols and aliphatic carboxylic acids; aromatic aliphatic ethers; aromatic and aromatic aliphatic aldehydes; aromatic and aromatic aliphatic ketones; aromatic and aromatic aliphatic carboxylic acids and their esters; nitrogen-containing aromatic compounds; phenyl ethers and phenyl esters; heterocyclic compounds; lactones; and mixtures of the above active ingredients.

[0079] Specific examples of the above substances are known to those skilled in the art. Fragrance substances or odorant substances and mixtures of two or more of said substances are chemical substances or compositions for imparting, conferring and / or regulating a specific smell or smell impression. Preferably, the smell (impression) is considered to be pleasant.

[0080] The term "fragrance" refers to an encapsulated fragrance. The terms "fragrance", "encapsulated fragrance" and "perfume" can be used interchangeably.

[0081] In an alternative embodiment according to the invention, the microcapsules according to the invention use fragrance substances or fragrance oils, or fragrance substances or fragrances as the active ingredient to be encapsulated or as the core material, respectively. These are compositions containing at least one fragrance substance or one fragrance substance. Such compositions, in particular mixtures of fragrance substances or fragrance oils, preferably contain two, three, four, five, six, seven, eight, nine, ten or more fragrance substances.

[0082] The fragrance mixture or fragrance oil, respectively, is preferably selected from extracts of natural raw materials, such as essential oils, extracts, absolutes, resins, balms, tinctures, such as ambergris oil; fragrant tree oil; angelica seed oil; angelica root oil; anise oil; valerian oil; basil oil; tree moss absolute; laurel oil; mugwort oil; benzoin resin; bergamot oil; beeswax absolute; birch tar; bitter almond oil; savory oil; buco leaf oil; cabrera wood oil; juniper oil; sweet calamus oil; camphor oil; cananga oil; cardamom oil; quinoa oil; cinnamon oil; acacia absolute; castoreum absolute; cedar leaf oil; cedar oil; labdanum oil; citronella oil; lemon oil; copaiba balm; copaiba balm oil; coriander oil; costus root oil; cumin oil; cypress oil; davana oil; dill weed oil; dill seed oil; Eau debrouts absolute; oakmoss absolute; elemi oil; tarragon oil; lemon eucalyptus oil; eucalyptus oil; fennel oil; spruce needle oil; gabion oil; gabion resin; geranium oil; grapefruit oil; guaiac wood oil; guyun balm; guyun balm oil; helichrysum absolute; helichrysum oil; ginger oil; orris root absolute; orris root oil; jasmine absolute; calamus oil; blue chamomile oil; Roman chamomile oil; carrot seed oil; quinoa oil; pine needle oil; curly mint oil; caraway oil; labdanum oil; labdanum absolute; labdanum resin; lavender absolute; lavender oil; lavender absolute; lavender oil; lemongrass oil; angelica oil; distilled lime oil; pressed lime oil; linalool oil oil); Litsea cubeba oil; Bay leaf oil; Macis oil; Marjoram oil; Mandarin oil; Cinnamon bark oil; Mimosa absolute; Musk grain oil; Musk tincture; Musk sage oil; Musk grape oil; Myrrh absolute; Myrrh oil; Myrtle oil; Clove leaf oil; Clove flower oil; Neroli oil; Frankincense absolute; Frankincense oil; Red myrrh oil; Neroli absolute; Orange oil; Oregano oil; Palmarosa oil; Patchouli oil; Perilla seed oil; Peru balm oil; Parsley leaf oil; Parsley seed oil; Orange leaf oil; Mint oil; Chili oil; Allspice oil; Pine oil; Poley Oil; rose absolute; rosewood oil; rose oil; rosemary oil; dalmatine sage oil; Spanish sage oil; sandalwood oil; celery seed oil; spike lavender oil; anise oil; styrax oil; marigold oil; fir oil; tea tree oil; turpentine oil; thyme oil; tolu balsam; tonka bean absolute; tuberose absolute; vanilla essence; violet absolute; verbena oil; vetiver oil; juniper berry oil; wine yeast oil; wormwood oil; wintergreen oil; ylang-ylang oil; hyssop oil; civet absolute; laurel leaf oil; cassia bark oil; and fractions thereof or components isolated therefrom.

[0083] In another variant of the invention, the fragrance substances can also be encapsulated in the form of individual fragrances as core materials, wherein the core material comprises at least one individual fragrance substance or a mixture thereof as active ingredient.

[0084] However, preferably, individual aromatic or odorous substances (i.e. compounds having a taste or smell, and therefore all natural and synthetic substances which impart an olfactory perceptible smell) or, alternatively, mixtures of aromatic or odorous substances (so-called perfume oils) are used as active ingredients surrounded by the microcapsule shell. More preferably, said substances and mixtures of substances impart a pleasant smell to the consumer product.

[0085] In a preferred variant of the invention, all microcapsules contained in the powder or lozenge according to the invention are loaded with the same active ingredient or ingredients, for example all microcapsules contain a fragrance substance, even more preferably, all contain the same fragrance substance.

[0086] According to an alternative embodiment, the microcapsules contained in the powder or lozenge according to the invention encapsulate different classes of active ingredients or different substances in the same class of active ingredients. For example, some of the microcapsules contain a specific fragrance substance, while other microcapsules surround another fragrance substance.

[0087] Thus, preferably, the core material is chosen independently of the shell material.

[0088] Therefore, according to another preferred variant of the invention, the lozenge according to the invention may contain one type of microcapsules or a mixture of two or more different types of microcapsules. Thus, the microcapsules may differ in the active ingredient composition (i.e. the microcapsule core) and / or the wall composition (i.e. the material of the capsule shell).

[0089] A single tablet or powdered composition of the present invention may contain 0.5% to 10% by weight of one or more microcapsules as specifically described above, based on the total weight of the tablet or powdered composition.

[0090] Therefore, 0.5% to 10% by weight of microcapsules based on the total weight of the tablet can be incorporated into the final composition, that is, a single tablet of the composition according to the present invention contains 0.5% to 10% by weight of one or more microcapsules as clearly described above. If the amount of the microcapsule component is kept within these ranges, a uniform distribution of the microcapsules in the one or more tablets can be achieved. In addition, if the amount of component (b) is within the above range, the active ingredient can be effectively incorporated into the final solid consumer product formulation due to the effective protection of the surrounding salt matrix, that is, the microcapsules will not break during the preparation of the solid consumer product, and therefore the encapsulated one or more active ingredients can be effectively retained without loss, thereby resulting in significantly improved microcapsule performance, as shown in the experimental section.

[0091] According to a preferred embodiment, the amount of the one or more microcapsules ranges from 0.5 to 10 wt. % based on the total weight of the powder or the tablet, and even more preferably from 3 to 8 wt. % based on the total weight of the tablet or powder.

[0092] The microcapsules may be incorporated directly into the composition of the present invention, or may be added in the form of a capsule slurry.

[0093] The composition of the present invention comprising microcapsules encapsulating the one or more active ingredients is effectively incorporated into a wide variety of solid consumer product formulations, thereby allowing effective and targeted release of the one or more active ingredients. Thus, the presence of the crystalline inorganic salt acts as a kind of shock-absorbing layer, which protects the microcapsules from damage caused by mechanical, chemical and / or thermal influences and thus prevents premature release and degradation of the one or more active ingredients during the preparation of the consumer product.

[0094] It is also advantageous that the powder or the powder particles of the tablets each have a diameter in the range of 100 μm to 1 cm, preferably 500 μm to 3 mm, in order to achieve an ideal distribution of the tablets in the final solid consumer product formulation and thus an ideal distribution of the microcapsules embedded therein. Tablets that are too large will result in uneven distribution.

[0095] The lozenge or granule is preferably in the shape of a tablet, a pill, a sphere, etc., having a spherical, hemispherical, compressed hemispherical, lenticular and elliptical shape, and can be prepared by a person skilled in the art by any method known in the art.

[0096] In addition, the powder or pastille of the present invention and the microcapsule can further comprise one or more components that improve the visual aesthetics of the final consumer product, such as a colorant. In addition, the powder or pastille can comprise additives and / or active ingredients, such as optical brighteners, detergents, laundry active agents, etc.

[0097] Preparation method:

[0098] In the first step (i) of the process according to the invention, the following components (a) are mixed with components (b) and (c): (a) at least one anhydrous alkaline earth or alkali metal salt or a mixture of at least one anhydrous alkaline earth metal salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, wherein the capsules contain at least one active ingredient, and (c) optionally at least one humectant.

[0099] In the context of the present invention, the components explicitly stated above apply equally here, ie the terms "microcapsules", "anhydrous salts", "humectants", "pastilles" etc., and the corresponding amounts and properties as explicitly stated above.

[0100] Preferably, the composition according to the invention comprises a humectant. Thus, in a further preferred variant of the invention, in the first step (i) of the process according to the invention, the following components (a) are mixed with components (b) and (c): (a) at least one anhydrous alkaline earth or alkali metal salt or a mixture of at least one anhydrous alkaline earth metal salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, wherein the capsules contain at least one active ingredient, (c) at least one humectant.

[0101] Preferably, the humectant is selected from propylene glycol or ethylene glycol or dipropylene glycol or glycerol or sorbitol or maltitol. It has been found that these humectants are particularly suitable for preparing powders or lozenges according to the present invention. The use of such polyols allows the preparation of highly stable products that can be incorporated into various consumer product formulations. Other substances, such as microfibrillated cellulose, etc., do not achieve the desired performance.

[0102] Preferably, as alkaline earth or alkali metal salts, 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 are used. These are preferred salts as component (a).

[0103] In particular, sodium sulfate and / or sodium acetate and / or potassium citrate are used to obtain powders or lozenges having significantly improved stability properties while allowing an effective and targeted release of the active ingredient.

[0104] The crystalline salt matrix protects the microcapsules from chemical and mechanical influences, while achieving high release performance. The protection allows the microcapsules of the load to be effectively incorporated into a wide range of consumer product formulations, particularly solid consumer product formulations. In the process of manufacturing such compositions, fragile microcapsules can be subject to high shear, which can cause the rupture of the microcapsules, and therefore cause the premature release of the active ingredient. It has been surprisingly found that the composition according to the present invention can be advantageously incorporated into such formulations, thereby in these formulations, in their manufacturing process and relative to other ingredients, showing improved performance and chemical and mechanical stability.

[0105] Suitable components (b) are as specified above.

[0106] According to the present invention, the humectant is a hygroscopic substance used to keep the mixture to be prepared in step (i) moist.

[0107] 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.

[0108] Preferably, the at least one encapsulated active ingredient is selected from odorants, fragrances, flavoring agents, perfume oils, flavoring agents, cosmetic ingredients, pharmaceutical active ingredients, insect repellents, ingredients for oral and dental care products, latent heat storage media and adsorbents. More preferably, the ingredient is a odorant or fragrance or perfume oil, and its addition ratio is 0% to 10% by weight, preferably 0% to 6% by weight, based on the total weight of the lozenge or powdered composition.

[0109] According to the present invention, capsule slurries or capsules may be used.

[0110] Preferably, the capsule slurry is a dispersion of capsules in water. More preferably, in order to obtain a powder or lozenge with improved stability and improved organoleptic properties, the capsule content is 25% to 65% by weight (and preferably 25% to 40% by weight) based on the total weight of the lozenge or powdered composition. Alternatively, in the case where no capsule slurry is used but at least one capsule is used, the capsule content is 1% to 80% by weight based on the total weight of the lozenge or powdered composition.

[0111] According to another further preferred variant, the proportion of capsules is from 10% to 70% by weight, or the proportion of capsule slurry contained in the composition according to the invention is from 1% to 80% by weight (and even more preferably from 10% to 40% by weight), based on the total weight of the tablet or powdered composition.

[0112] If the amount of the microcapsule component (b) is maintained within these ranges, a uniform distribution of the microcapsules within the one or more tablets can be achieved. In addition, if the amount of component (b) is within the above ranges, the active ingredient can be effectively incorporated into the final solid consumer product formulation due to the effective protection of the surrounding salt matrix, i.e., the microcapsules will not break during the preparation of the solid consumer product, and thus the encapsulated one or more active ingredients can be effectively retained without loss, resulting in significantly improved microcapsule performance, as shown in the experimental section.

[0113] Preferably, the proportion of alkaline earth and / or alkali metal salts is from 20 to 99% by weight.

[0114] According to a further preferred variant, the proportion of alkaline earth and / or alkali metal salts is 40% to 80% by weight, based on the total weight of the pastille or powdered composition.

[0115] If the amount of the salt component specified above is contained in the composition according to the invention within the range, effective protection of the breakable microcapsules within the crystalline salt matrix can be achieved while allowing effective and targeted release of the active ingredient.

[0116] According to another further preferred variant, a humectant is included in the composition according to the invention. Preferably, the amount of humectant is from 0% to 5% by weight, based on the total weight of the pastille or powdered composition.

[0117] Preferably, the proportion of the humectant is from 0% to 2.5% by weight, even more preferably from 0.1% to 2.5% by weight, based on the total weight of the lozenge or powdered composition.

[0118] It has been surprisingly found that the presence of a humectant significantly improves the stability and performance of the composition according to the present invention. In addition, it has been found that the comparison of samples with and without the addition of a humectant shows that the addition of a humectant not only improves the manufacture and preparation of more uniform lozenges, but also improves the sensory experience by allowing more effective protection of fragile microcapsules and therefore allowing more targeted release of fragrances. Surprisingly, the humectant component included further improves the performance of the final product, which allows effective regulation of the viscosity and flexibility of the crystalline matrix, thereby producing a matrix with less brittleness and greater flexibility, which has an improved buffering effect, and therefore better protects the fragile microcapsules and promotes incorporation into solid consumer product formulations, without changing the basic chemical properties of the composition. In addition, it has been surprisingly found that the humectant component is conducive to forming the lozenge, and significantly improves the miscibility of the microcapsule component and the salt component and other optional components or additives, so that the microcapsules (and therefore the active ingredient) can be more evenly distributed in the crystalline matrix. The addition of the humectant within the range explicitly stated above enables the properties of the matrix to be effectively adjusted, thereby producing a less brittle and more flexible matrix which has an improved cushioning effect and therefore better protects the fragile microcapsules and facilitates incorporation into solid consumer product formulations without changing the basic chemical characteristics of the plasticized material.

[0119] Preferably, based on the total weight of the tablet or powdered composition, the proportion of alkaline earth and / or alkali metal salt is 20% to 99% by weight, the proportion of capsule is 10% to 70% by weight, or the proportion of capsule slurry is 1% to 80% by weight, and optionally, the proportion of humectant is 0% to 2.5% by weight. Surprisingly, this results in improved stability and improved organoleptic properties of the powder or tablet.

[0120] In order to obtain a powder or lozenge with improved stability and improved organoleptic properties, the proportion of alkaline earth and / or alkali metal salt is 40% to 80% by weight, the proportion of capsules is 1% to 70% by weight, or the proportion of capsule slurry is 1% to 80% by weight, and the proportion of moisturizer is 0% to 5% by weight, based on the total weight of the lozenge or powdered composition.

[0121] In the subsequent step (ii) of the process according to the invention, the mixture obtained in step (i) is heated to obtain a melt.

[0122] Preferably, the melting step (ii) is carried out at a temperature in the range of 40°C to 80°C to achieve a uniform distribution of the discrete microcapsules in the crystalline buffer matrix. Preferably, the temperature range is 40°C to 60°C, even more preferably 40°C to 50°C.

[0123] During this step, additional additives such as binders, surfactants, plasticizers and / or structurants may be added and mixed to obtain a homogeneous mixture.

[0124] In a subsequent step, the mixture / melt of step (ii) is formed into tablets by dropping using prior art tableting methods known to those skilled in the art.

[0125] Pastillation is a particle formation process in which pastilles are usually formed using a droplet former and then cooling the discrete particles obtained. The method of preparing pastilles or granules is the commercially used method, and the pastilles can be formed into different shapes, including tablets, pills, spheres, etc. In addition, scale-up by dropping in air or vegetable oil using a pulse generator has also shown good results.

[0126] Typically, dripping the melt onto a surface results in the formation of discrete ingots.

[0127] In one embodiment of the invention, the surface is cooled before and / or during dripping in order to improve the crystallization process of the melt.

[0128] Therefore, in another method step (iii) of the present invention, the melt prepared in step (ii) is dripped onto the surface of an object to at least partially crystallize the dripped melt, and then step (iv) is carried out, i.e. seeding and optionally cooling the dripped melt.

[0129] Seeding describes crystallization using seed crystals. A seed crystal is a small piece of single or polycrystalline material from which a large crystal of generally the same material can be grown, i.e. crystal seeding is a technique widely used to provide a preformed template (seed) on which new molecules can aggregate to form crystals. Typically, the seed crystal has the same composition as the final crystal. Such methods are known to those skilled in the art.

[0130] Therefore, within the scope of the present invention, the seed crystals have the same composition as the anhydrous salt used in step (i) of the present invention.

[0131] Seeding allows the formation of a homogeneous and stable crystalline salt matrix which embeds the breakable microcapsules while allowing an efficient and targeted release of the active ingredient encapsulated in the microcapsules.

[0132] Seeding also has a significant effect on the reaction rate. During slow precipitation (i.e. slow formation of the salt matrix), the fragile capsules are pushed outwards. This results in an uneven distribution of the capsules. Therefore, the delicate and fragile capsules are not well protected against external influences, such as pressure.

[0133] Surprisingly, it has been found that seeding with seed crystals significantly accelerates the formation of the salt matrix and facilitates the uniform distribution of the breakable capsules within this protective matrix. As a result, the microcapsules are better protected and the release properties are not negatively affected.

[0134] Seeding affects the crystallization behavior and therefore also the final crystal structure and thus also the overall structure of the resulting composition according to the invention. The crystals obtained by seeding exhibit different properties than crystals without any seeds.

[0135] Other components, such as the presence of humectants, can also influence the crystallization behavior and thus the final structure and properties.

[0136] Finally, as step (v), the resulting powder or tablet is collected.

[0137] Typically, the tablets are formed by dropping the mixture of step (iii) using prior art tableting methods known to those skilled in the art. Tabletting is a particle forming process in which a drop former is typically used to form tablets.

[0138] In order to achieve a uniform distribution of the microcapsules, the powder particles of the powder or the tablet each have a diameter ranging from 100 μm to 1 cm, preferably from 500 μm to 3 mm.

[0139] Furthermore, in another aspect, the present invention relates to a composition prepared by the method according to the present invention.

[0140] In one embodiment of the present invention, the powder or the powder particles of the tablet each have a weight ranging from 0.5 mg to 25 mg, preferably from 1 mg to 5 mg.

[0141] The composition according to the invention comprises or consists of at least one lozenge having a composition as specified above. Preferably, the composition is present as a plurality of lozenges. Alternatively, the composition is present as a single lozenge having a composition as specified above.

[0142] consumer goods:

[0143] Furthermore, in another aspect, the present invention relates to the use of a powder or a lozenge according to the present invention for the preparation of a consumer product formulation.The terms "consumer product formulation" and "consumer product" are used synonymously in the context of the present invention.

[0144] Considering the preparation of solid consumer products (such as powder detergents, laundry soaps, solid fabric softeners, deodorant sticks, etc.), it has been found that the powder or lozenges of the present invention obtained by the preparation method according to the present invention are particularly advantageous. Therefore, preferably, the consumer product according to the present invention is a solid consumer product.

[0145] When incorporated into a consumer product formulation, the microcapsules must remain chemically stable in a rather harsh environment, but at the same time mechanically stable when subjected to mechanical stress, for example during mixing and optionally pressing of a solid consumer product formulation. However, an increase in shell thickness generally leads to a poorer release performance (release of the active ingredient) because shearing during processing can cause a high rate of capsule breakage. It has been surprisingly found that the composition according to the invention based on microcapsules embedded in a crystalline salt matrix is ​​particularly suitable for incorporation into a solid consumer product formulation. The crystalline salt matrix protects the microcapsules while achieving a high release performance.

[0146] Therefore, in another preferred variant, the present invention also relates to the use of the powder or pastilles according to the invention for the preparation of consumer products and formulations thereof, wherein the consumer products or consumer product formulations are solid products, such as textile care products (e.g. powder detergents, laundry soaps, solid fabric softeners), solid soaps, household products (e.g. solid toilet cleaners, solid all-purpose cleaners, powdered carpet cleaners, powder detergents for washing dishes or cleaning various surfaces), personal care products (e.g. deodorants, soaps), fragrance enhancers, perfumers, pharmaceutical products and mixtures thereof.

[0147] Finally, in another aspect, the present invention relates to a consumer product or a consumer product formulation itself comprising or consisting of a composition according to the present invention, i.e. a composition according to the first aspect of the present invention, a composition according to the second aspect of the present invention and / or a composition obtained based on a process according to the third aspect of the present invention.

[0148] The powders or lozenges of the present invention allow for efficient incorporation of active ingredients into solid product formulations, thereby allowing for efficient and targeted release of said active ingredients. DETAILED DESCRIPTION

[0149] Example

[0150] Hereinafter, the present invention is described in more detail and specifically with reference to Examples, however, these Examples are not intended to limit the present invention.

[0151] Example 1: Microcapsules crystallized in sodium sulfate and incorporated into powder detergent - sensory evaluation.

[0152] According to a first embodiment, a composition comprising or consisting of at least one pastille containing microcapsules is prepared as follows: anhydrous sodium sulfate is mixed with a microcapsule slurry (40% pure microcapsules; a capsule to water ratio of 2:3) in a weight ratio of 1:1. The mixture is heated to 45°C until a viscous mass is obtained. The mixture is then dripped and seeded with seed crystals (anhydrous sodium sulfate) to obtain pastilles according to the invention. The microcapsules are based on melamine formaldehyde capsule walls encapsulating a fragrance mixture. The particle size of all microcapsules is in the range of 10 to 70 μm.

[0153] In the context of the present invention, the powder or lozenge according to the invention may be represented as microcapsules crystallized in anhydrous salt as mentioned in the present disclosure.

[0154] The sensory evaluation was performed as follows: Once the pastilles according to the invention were prepared as described above, they were combined with a commercial powder detergent and homogenized. The final dosage of the microcapsules in 40 g of powder detergent was 0.2% by weight (equivalent to 0.8% by weight of pastilles in 40 g of the powder detergent).

[0155] Finally, the product was added to the washing machine and the fabric (terry cloth) was washed at 30°C.

[0156] After rinsing, the fabrics were air dried (line dried) at room temperature.

[0157] As reference a corresponding powder detergent was used, into which the microcapsules were added directly.

[0158] The fragrance release was carried out in three steps. The first step describes the odor of an untreated dry cloth ("before rubbing"). The second step describes the odor of a lightly kneaded dry cloth; for this purpose, the cloth was subjected to a slight mechanical stress by moving it back and forth several times between the hands, causing the capsules to rupture. The third step describes the odor after the dry cloth was rubbed vigorously, thus causing the capsules to rupture. After each step, the fragrance intensity was evaluated.

[0159] To evaluate the sensory performance, 8 to 9 testers rated the fragrance intensity on a scale of 1 (no odor) to 9 (very strong odor).

[0160] exist Figure 1 The results of the sensory evaluation are shown in FIG.

[0161] Samples comprising lozenges according to the invention comprising microcapsules embedded in a protective crystalline matrix, for example sodium sulfate crystals (see Figure 1 and 2 ) showed significantly increased performance, indicating that the fragile microcapsules were effectively protected within the crystals while allowing for effective release of the active ingredient. The sodium sulfate crystals acted as a shock absorbing layer during the preparation of the consumer product. Samples without such a shock absorbing layer and samples containing only the coating did not function because most of the microcapsules were destroyed during the preparation of the consumer product.

[0162] Surprisingly, it has been found that the best organoleptic results are obtained with anhydrous sodium acetate. In addition, very good organoleptic results can be obtained with anhydrous potassium citrate (see Figure 3 ).

[0163] However, it is very important to use only anhydrous salts such as anhydrous sodium acetate (not in hydrate form).

[0164] Example 2: Microcapsules crystallized in sodium sulfate and incorporated into laundry soap - sensory evaluation

[0165] A plurality of tablets were prepared according to the method described in Example 1, wherein the microcapsules were embedded in the tablets.

[0166] The sensory evaluation was carried out as follows: Once the composition according to the invention was prepared, the pastilles obtained were combined with a commercial laundry soap in the form of soap granules, and the resulting mixture was passed through an extruder and the final soap was cut into pieces.

[0167] The prepared laundry soap was then applied to damp fabrics (terry cloth) by rubbing. After rinsing, the fabrics were air-dried at room temperature.

[0168] A corresponding laundry soap (which comprises perfumed microcapsules) not comprising the composition of the invention was used as reference.

[0169] Subsequently, a commercially available powdered detergent was mixed with the prepared tablets and homogenized.

[0170] Finally, add the product to your washing machine and wash your clothes at 30°C, then air dry at room temperature.

[0171] The sensory evaluation was performed according to Example 1. Figure 2 The results of the sensory evaluation are shown in FIG.

[0172] All samples showed a significant improvement in performance, based on the buffering function of the crystalline sodium sulfate during the preparation of the consumer product. Unprotected microcapsules were destroyed during mixing and homogenization with the powdered detergent and are therefore not suitable for the preparation of perfumed laundry soaps.

[0173] Example 3: Effect of different moisturizers.

[0174] A plurality of lozenges according to the invention were prepared according to the method described in Example 1. The composition contained 75 wt% salt (sodium sulfate) based on the total weight of the composition and 25 wt% microcapsule slurry (containing 40 wt% microcapsules based on the total weight of the slurry, i.e., a capsule loading of 40 wt%). These samples contained 0 wt% humectant (humectant).

[0175] The amount of humectant was gradually increased by simultaneously decreasing the corresponding amount of salt to illustrate the effect of the humectant (sorbitol) component on the final product (see Table 1).

[0176] Table 1.

[0177] sample Salt [wt%] Slurry [wt%] Humectant [wt%] observe 1 75 25 0 Good results 2 74 25 1 The results were excellent 3 72.5 25 2.5 The results were excellent 4 70 25 5 No crystallization

[0178] The results are Figure 4a (0% humectant) and 4b (1%, 2.5% and 5%). Samples 2 and 3 indeed showed excellent results. Good results were also achieved for sample 1. For the sample containing 5 wt% of the humectant sorbitol, no crystallization was observed.

[0179] Furthermore, it has been found that the addition of small amounts of humectants helps improve long term stability, ie, the lozenges retain their structure over time and do not "collapse" or fall apart.

[0180] Therefore, it can be concluded that in order to obtain an excellent product with improved stability and performance over time, the proportion of the humectant should be from 0% to 2.5% by weight based on the total weight of the tablet or powder. Particularly good long-term results are achieved when the humectant is present in an amount of from 1% to 2.5% by weight based on the total weight of the tablet or powder.

[0181] The same experiment was also carried out using glycerol instead of sorbitol. Figure 5 (1%, 2.5% and 5%). Only samples 2 and 3 showed truly excellent results. For the sample containing 5 wt% of the humectant glycerol, no crystallization was observed.

[0182] The same experiment was also performed using propylene glycol instead of sorbitol. Figure 6 (0%, 1%, 2.5% and 5%). Only samples 2 and 3 did show adequate results. For the sample containing 5 wt% of the humectant propylene glycol, no crystallization was observed.

[0183] It has been found that the presence of a humectant has a critical influence on the crystallization behavior of the composition.

[0184] Example 4: Effect of salt.

[0185] A plurality of lozenges according to the invention were prepared according to the method described in Example 1.

[0186] The composition comprises 72.5 wt% salt (sodium sulfate) based on the total weight of the composition, 25 wt% microcapsule slurry (comprising 40 wt% microcapsules based on the total weight of the slurry, i.e., a capsule loading of 40 wt%) and 2.5% humectant (propylene glycol).

[0187] In one embodiment, the salt is non-hydrated sodium sulfate (see Figure 7a ), and in another embodiment is sodium sulfate hydrate (sodium sulfate decahydrate) (see Figure 7b ).

[0188] The results show that non-hydrated salts provide better crystallization results. The products are more difficult to handle. On the one hand, the desired crystal structure is hardly formed, and on the other hand, the resulting product is therefore also significantly more moist and stickier overall. Powders or pastilles cannot be obtained. Such products cannot be incorporated into powder formulations, such as powder detergents. Mixing will immediately lead to agglomeration of the final consumer product formulation. Therefore, non-hydrated salts are preferred within the scope of the present invention.

[0189] A crystallization process for sodium sulfate was developed. For this purpose, anhydrous sodium sulfate and the capsule slurry were mixed. The water in the capsule slurry formed a viscous but pluggable mass. By seeding the crystals, a solid product could be developed. However, sodium sulfate decahydrate dissolves in its own water of crystallization at 32°C. Therefore, stable tablets could not be obtained when the salt was used in hydrated form.

[0190] It was therefore found that the dissolution of the salt (e.g. sodium sulfate) in its own water of crystallization was disadvantageous. As mentioned above, this would not lead to the desired product and would not be possible to form a lozenge, let alone to incorporate into a powdered consumer product formulation.

[0191] On the other hand, the use of anhydrous salts allows the preparation of an easily handleable paste which can be easily processed into lozenges which can be stably incorporated into powdered consumer product formulations.

[0192] Example 5: Effect of seeding.

[0193] Furthermore, in another embodiment, the dependence of the crystallization behavior on seeding was analyzed.

[0194] For this purpose, two different compositions were prepared based on the following composition: 75% by weight salt (sodium sulfate), 25% microcapsules.

[0195] The composition contained 75 wt% salt (sodium sulfate) based on the total weight of the composition and 25 wt% microcapsule slurry (containing 40 wt% microcapsules based on the total weight of the slurry, i.e., a capsule loading of 40 wt%). These samples contained 0 wt% humectant (moisturizer).

[0196] In one aspect, tablets were prepared using seed crystals (anhydrous sodium sulfate) according to the method described in Example 1. The results are shown in Figure 8b (for seeding).

[0197] On the other hand, tablets were prepared according to the same method, but without seeding, i.e. without adding seed crystals. The results are shown in Figure 8a In (no seeding).

[0198] As can be seen from the figure, for the sample without seed crystal preparation, no crystallization is observed. Cannot obtain lozenges, but obtain wet and uncrystallized droplets. The product is more difficult to handle. On the one hand, there is almost no required crystal structure formed, and on the other hand, the product formed is therefore also obviously more moist and stickier on the whole. Powders or lozenges cannot be obtained. Such products cannot be incorporated into powder formulations, such as powder detergents. Mixing can immediately cause the final consumer product formulation to agglomerate.

[0199] However, adding seed crystals provides complete crystallization and thus results in the formation of stable lozenges. Therefore, it can be concluded that seeding is required to achieve sufficient crystallization and thus form lozenges according to the present invention. The lozenges are easy to handle and can be stably incorporated into powdered consumer product formulations.

[0200] It has further been found that seeding also allows the formation of a homogeneous and stable crystalline salt matrix which embeds the breakable microcapsules and at the same time allows an effective and targeted release of the active ingredient encapsulated in the microcapsules.

[0201] It has also been found that seeding has a significant effect on the reaction rate. During slow precipitation (i.e. slow formation of the salt matrix), the fragile capsules are pushed outwards. This results in an uneven distribution of the capsules. As a result, the delicate and fragile capsules are not well protected against external influences, such as pressure.

[0202] Surprisingly, it has been found that seeding with seed crystals significantly accelerates the formation of the salt matrix and facilitates the uniform distribution of the breakable capsules within this protective matrix. As a result, the microcapsules are better protected and the release properties are not negatively affected.

[0203] Seeding affects the crystallization behavior and therefore also the final crystal structure and thus also the overall structure of the resulting composition according to the invention. The crystals obtained by seeding exhibit different properties than crystals without any seeds, especially in terms of stability.

[0204] Embodiment 6:

[0205] In another embodiment, the lozenge according to the present invention is prepared as follows:

[0206] 1) providing 25 g of sodium sulfate (anhydrous) - component (a);

[0207] 2) adding 16 g of capsule slurry (comprising melamine-formaldehyde based microcapsules at a concentration of 40 wt.%; the ratio of capsules to water is 2:3) - component (b);

[0208] 3) adding 0.2 g C18-C22 hydroxyalkyl hydroxypropyl guar gum (stabilizer);

[0209] 4) heating the mixture to 45° C. in a water bath;

[0210] 5) Add a very thin layer of sodium sulfate (anhydrous) for seeding;

[0211] 6) forming droplets of the mixture; and

[0212] 7) Add the obtained pastilles to the final product formulation (detergent).

[0213] C18-C22 hydroxyalkyl hydroxypropyl guar gum was added as a stabilizer.

[0214] In addition, tablets containing microcapsules without a protective salt layer were also prepared for comparison.

[0215] The results of sensory evaluation were Fig. 9 (left: unprotected salt matrix, right: protected salt matrix according to the present invention).

[0216] The results show that the protection of the breakable microcapsules according to the invention significantly improves the olfactory properties of the final product formulation. This effect can be further improved by adding stabilizers.

Claims

1. A method for preparing a powder or tablet consisting of or comprising a plurality of microcapsules containing one or more ingredients, the method consisting of or comprising the following steps: (i) mixing the following components (a), (b) and (c): (a) at least one anhydrous alkaline earth or alkali metal salt, or a mixture of at least one anhydrous alkaline earth metal salt and at least one anhydrous alkali metal salt, (b) at least one capsule slurry or at least one capsule, (c) optionally at least one humectant, wherein the humectant is selected from propylene glycol or ethylene glycol or dipropylene glycol or glycerol or sorbitol or maltitol; (ii) heating the mixture obtained in step (i) to produce a melt; (iii) dropping the melt produced in step (ii) onto a surface of an object; (iv) seeding and optionally cooling the melt dripping in step (iii) to at least partially crystallize the dripping melt; and (v) collecting the powder or tablets obtained.

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

3. A process for preparing a powder or a tablet according to any one of the preceding claims, wherein the melting step (ii) is carried out at a temperature in the range of 40°C to 80°C.

4. A method for preparing a powder or a lozenge according to any one of claims 1 to 3, wherein the surface is cooled before and / or during dripping.

5. The method for preparing a powder or lozenge according to any one of claims 1 to 4, wherein as alkaline earth 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, in particular sodium sulfate and / or sodium acetate and / or potassium citrate.

6. The method for preparing a powder or lozenge 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 the humectant.

7. A process for preparing a powder or lozenge according to any one of claims 1 to 6, wherein the at least one ingredient is selected from odorants, fragrances, flavoring agents, perfume oils, flavoring agents, cosmetic ingredients, pharmaceutical active ingredients, insect repellents, ingredients for oral and dental care products, latent heat storage media and adsorbents.

8. A method for preparing a powder or lozenge according to any one of claims 1 to 7, wherein the at least one ingredient is a scent or fragrance or fragrance oil, and is added in a proportion of 0 to 10% by weight, preferably 0 to 6% by weight, based on the total weight of the lozenge or powder.

9. A method for preparing a powder or tablet according to any one of claims 1 to 8, wherein the at least one capsule has a wall material consisting of one or more of the following substances, the substances being selected from natural, semi-synthetic and fully synthetic shell materials, preferably melamine-formaldehyde resins, gelatin, alginates, polyurethanes, polyamides and polyureas, or one or more of such substances comprises or is based on one or more of such substances.

10. A powder or lozenge obtainable by the process of any one of claims 1 to 9.

11. The powder or pastille according to claim 10, wherein the powder particles of the powder or pastille each have a diameter ranging from 100 μm to 1 cm, preferably from 500 μm to 3 mm.

12. The powder or lozenge according to claim 10 and / or claim 11, wherein the powder particles of the powder or lozenge each have a weight ranging from 0.5 mg to 25 mg, preferably from 1 mg to 5 mg.

13. A consumer product selected from detergents and cleaners, personal care products, nutritional or conditioning preparations, cosmetic or pharmaceutical preparations, perfumed products or products to be perfumed, preferably fragrance rinses, laundry fragrances, comprising a powder or a pastille or pastilles according to one or more of claims 10 to 12.

14. Use of a powder or lozenge according to claims 10 to 12 for perfuming a consumer product, preferably a consumer product according to claim 13.

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