Fragrance oil capsules for aroma-enhanced solid formulations
By using a composition of microcapsules, polymer matrix, and free fragrance in solid consumer product formulations, the olfactory performance and stability issues caused by the fragility of microcapsules are resolved, and the effective incorporation and targeted release of fragrance are achieved, thereby improving the olfactory performance and stability of consumer products.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-18
- Publication Date
- 2026-03-27
AI Technical Summary
Existing technologies make it difficult to effectively incorporate and stably release fragrances into solid consumer product formulations, resulting in poor olfactory performance and product stability issues. In particular, microcapsules are fragile in powder detergents, affecting olfactory impression and storage stability.
A composition comprising microcapsules, a polymer matrix, and free fragrances is used to form tablets by melting polymers and mixing microcapsules, combined with plasticizers and structuring agents, to prepare flavored granules with excellent release properties, protecting the microcapsules from mechanical, chemical, and thermal effects.
It enables the effective incorporation and targeted release of fragrances in solid consumer products, enhancing olfactory performance and stability. It is suitable for a variety of consumer products such as textile care products, simplifying the processing and improving homogeneity.
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Figure CN121752236A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of fragranced granules, particularly to fragranced granules for use in solid consumer product formulations such as textile care products. More specifically, this invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of at least one microcapsule and a polymer matrix encapsulating the at least one microcapsule, wherein the composition further comprises a free fragrance agent, and this invention relates to a composition additionally comprising or consisting of at least one binder in the matrix. Furthermore, this invention relates to a method for preparing a corresponding composition and its use in the preparation of consumer products, as well as consumer products themselves comprising or consisting of compositions according to the invention. Background Technology
[0002] Currently, many consumer products such as detergents, fabric softeners, laundry powders, deodorants, and cleaning agents are scented with fragrance materials or contain cosmetic ingredients to deliver specific effects.
[0003] Unfortunately, often, for example, the fragrance substances or cosmetic ingredients in such products interact with other components of the product formulation, or the volatile components of the fragrance formulation tend to evaporate prematurely. This results in undesirable changes and / or reductions in the fragrance impression, or premature "use" of the cosmetic ingredient over time, or even adverse reactions with other components of the product formulation, leading to reduced product quality and / or stability. To prevent potential interactions between fragrances or other active ingredients and other components of the product, or, for example, to prevent the evaporation of fragrances and thus not distort or reduce the desired olfactory impression, fragrances or other active ingredients can be added to the formulation in an encapsulated form. In this way, the desired olfactory impression can be guaranteed, for example, based on the targeted release of the active ingredient. Furthermore, interactions between product components can be reduced, thereby allowing for improved product quality and storage stability.
[0004] Therefore, a wide variety of consumer products include encapsulated active ingredients, such as fragrances, in their formulations. For example, textile care formulations such as liquid detergents or fabric softeners include various such scented microcapsules. Additionally, these formulations require the incorporation of preservatives to increase their stability and durability, such as methylisothiazolinone (MIT), which can cause allergic reactions or skin irritation, while powdered detergents generally do not require the addition of preservatives and reduce environmental pollution. However, incorporating microcapsules into powdered formulations (such as powdered detergents) significantly exacerbates the problem because the mixing of microcapsule components with other detergent components leads to the rupture of fragile microcapsules, causing, for example, a loss of olfactory properties.
[0005] Microcapsules that simultaneously possess good stability and good release performance are particularly challenging to prepare. The ability of a capsule to retain the active ingredient and thus prevent the loss of volatile components depends heavily on its stability within the product base. However, very stable microcapsules, such as capsules with fairly thick walls, generally tend to exhibit low performance because microcapsule rupture and therefore the release of the active ingredient are hindered. Conversely, if they are too unstable, they may have already deteriorated during storage or resulted in leakage of the active ingredient and thus become ineffective. Therefore, increasing the capsule wall, i.e., multi-layered microcapsule shells or even thicker shells, similarly leads to reduced performance because the targeted release of the active ingredient is deteriorated, and these microcapsules typically require complex, multi-step preparation methods.
[0006] Furthermore, given the public's increasing ecological awareness (less waste, fewer preservatives, etc.), there is a new and growing trend towards solid consumer products such as solid hair care products, soaps, and solid bath products, making them increasingly relevant not only in the cosmetics industry but also in other industries. However, as noted above, incorporating microcapsules into powder formulations significantly exacerbates the problem, as the mixing of microcapsule components with other typically solid detergent components leads to the breakage of fragile microcapsules.
[0007] Therefore, there is a need to improve the effective incorporation of active substances, such as flavoring ingredients, into solid consumer product formulations, while simultaneously allowing for the effective and targeted release of said active substances.
[0008] Specifically, there is a need to provide compositions containing the active substance for such consumer product formulations, particularly textile treatment compositions, that have improved olfactory properties and stability.
[0009] At the same time, in order to meet high demand, the compositions used in solid consumer product formulations should be more readily available, and the resulting compositions should exhibit improved properties, such as in terms of their olfactory quality. Summary of the Invention
[0010] The present invention was made in view of the above-mentioned disadvantages. In order to overcome the above disadvantages, the present invention provides a composition and a method for preparing the same, which allows for the effective incorporation of an active ingredient having improved olfactory properties and stability into a solid consumer product formulation and / or allows for the preparation of the consumer product itself.
[0011] More specifically, the present invention provides a method that allows for the facilitating processing of the corresponding composition while demonstrating improved olfactory properties.
[0012] Therefore, in a first aspect, the present invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet (based on the total weight of the tablets) comprises or consists of the following: (a) 0.5% to 10% by weight of at least one microcapsule encapsulating the active ingredient. The active ingredient is preferably a single fragrance or a mixture of fragrances; (b) 92% to 98% by weight of polymer, The polymer is preferably polyethylene glycol; and (c) 0.1% to 10% by weight of free fragrance or mixture of free fragrance, and preferably hydrophobic fragrance or mixture of fragrance (i.e., hydrophobic free fragrance component). The above items are based on the total weight of the tablets.
[0013] Preferably, the composition is used in the preparation of fragranced consumer product formulations, particularly fragranced textile treatment compositions.
[0014] In a preferred embodiment of the composition, the polymer is preferably polyethylene glycol.
[0015] According to a second aspect, the present invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet (based on the total weight of the tablets) comprises or consists of the following: (a) 0.5% to 10% by weight of at least one microcapsule encapsulating the active ingredient. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) at least one polymer, ranging from 60% to 80% by weight. The polymer is preferably polyethylene glycol; (c) at least one adhesive, ranging from 2% to 32% by weight. The adhesive is preferably selected from the group consisting of: fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; and (d) 0.1% to 10% by weight of free fragrance or mixture of free fragrance, preferably hydrophobic fragrance or mixture of fragrance (i.e., hydrophobic free fragrance component).
[0016] In a preferred embodiment of the composition, the polymer is preferably polyethylene glycol, and / or the binder is preferably selected from the group consisting of animal waxes and / or plant waxes, and preferably beeswax.
[0017] According to a third aspect, the present invention relates to a method for preparing a composition comprising a plurality of tablets or of a plurality of tablets, the method comprising the following steps: (i) Providing at least one microcapsule or an aqueous dispersion containing at least one microcapsule; (ii) Melting at least one polymer and optionally an adhesive; (iii) Incorporate at least one microcapsule into the polymer melt of step (ii); (iv) Mixing free fragrances or mixtures of free fragrances; (v) Forming an ingot from the mixture of step (iv) by dripping; and (vi) Optional cooling; Optionally, it may also include the step of adding at least one plasticizer and / or at least one structuring agent in or after steps (ii), (iii) and / or (iv).
[0018] Furthermore, the present invention relates to a composition comprising or consisting of at least one tablet obtained by the method according to the invention, wherein the tablet comprises or consists of the following: (a) At least one microcapsule encapsulating an active ingredient, The active ingredient is preferably a fragrance or a mixture of fragrances; (b) at least one polymer, preferably polyethylene glycol; (c) Optionally at least one adhesive, The adhesive is preferably selected from the group consisting of: fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; and (d) Free fragrance or mixture of free fragrances, and preferably hydrophobic fragrance or mixture of fragrances (i.e., hydrophobic free fragrance components). The composition has a viscosity η of less than 900 mPa·s at 80°C.
[0019] In another aspect, the present invention relates to compositions prepared according to the method of the present invention.
[0020] Finally, the present invention relates to the use of the compositions according to the invention in the preparation of consumer products and their formulations, as well as consumer products and their formulations comprising or composed of the compositions according to the invention.
[0021] Specifically, the inventors have discovered that the compositions according to the invention allow for the efficient and further improved incorporation of active ingredients in an encapsulated form exhibiting excellent release characteristics (performance) into a wide range of solid consumer product formulations and the consumer products themselves, which simultaneously exhibit excellent olfactory properties, particularly pre-friction properties. Therefore, the polymer matrix acts as a buffer, protecting fragile microcapsules from mechanical, chemical, and / or thermal influences during the preparation of the final consumer product (formulation) without negatively impacting the performance of the microcapsules within the consumer product (formulation). Based on this, the dosage form of the present invention allows for the efficient incorporation of active ingredients into solid consumer product formulations via microcapsules, while simultaneously allowing for the efficient and targeted release of said active ingredients, thus overcoming the disadvantages of the prior art. The fragile microcapsules are encapsulated in a protective matrix that can withstand even harsh chemical and physical conditions, such as elevated temperatures or acidic or alkaline conditions. The addition of free aromatic substances or aromatic mixtures dispersed in the polymer matrix further improves the initial olfactory properties of the solid consumer product (formulation) and allows for facilitated processing and improved homogeneity by having a favorable effect on the viscosity of the composition according to the invention.
[0022] This problem is addressed by the purpose of the independent patent claims. The preferred embodiments are apparent from the wording of the dependent patent claims and the following description.
[0023] Unless otherwise stated, all percentages are by weight. Examples of numerical values given in the form of "x to y" include the given values. When multiple preferred numerical ranges are specified in this form, all ranges resulting from combining different endpoints are also included.
[0024] As used herein, the terms “at least one” or “one or more” refer to one or more, such as 2, 3, 4, 5, 6, 7, 8, 9 or more.
[0025] The term "and / or" indicates a connection or provides an alternative. Attached Figure Description
[0026] Figure 1 : Figure 1 The results of a sensory evaluation of the performance (i.e. release characteristics) of different samples of powdered detergents, depending on the presence of fragrance emulsifiers (i.e., free fragrance components), are shown.
[0027] Figure 2 : Figure 2 The viscosity of different samples is shown as dependent on the presence of fragrance emulsifiers (i.e., free fragrance components).
[0028] Figure 3 : Figure 3The viscosity of different samples is shown depending on the type of fragrance emulsifier (polymer matrix: PEG 6,000 g / mol).
[0029] Figure 4 : Figure 4 The viscosity of different samples is shown in terms of molecular weight (PEG 6,000 g / mol; PEG 8,000 g / mol; PEG 10,000 g / mol).
[0030] Figure 5 : Figure 5 The results of sensory evaluation of the performance (i.e. release characteristics) of different samples in powder detergents for different adhesives are shown.
[0031] Figure 6 : Figure 6 Different samples of compositions comprising at least one tablet prepared according to the present invention or of at least one tablet prepared according to the present invention are shown, illustrating the effect of microcapsule slurry content.
[0032] Figure 7 : Figure 7 Different samples comprising at least one tablet prepared based on the present invention or a composition consisting of at least one tablet prepared based on the present invention are shown, and these samples demonstrate the effect of water content / plasticizer content (without microcapsules).
[0033] Figure 8 : Figure 8 Different samples of compositions comprising at least one tablet prepared according to the present invention or of at least one tablet prepared according to the present invention are shown, illustrating the effect of water content / plasticizer content (with microcapsules).
[0034] Figure 9 : Figure 9 A photograph shows microcapsules and free fragrance oils in laundry soap.
[0035] Figure 10 : Figure 10 Photographs of microcapsules and free aromatic oils in PEG are shown.
[0036] Figure 11 : Figure 11 The results of a sensory evaluation of the performance (i.e., release characteristics) of the laundry soap according to the invention are shown. Detailed Implementation
[0037] The invention will now be described in more detail.
[0038] The compositions of the present invention comprise or consist of at least one tablet, the at least one tablet comprising an encapsulated active ingredient (preferably a fragrance (or a mixture of fragrances)), a polymer forming a polymer matrix (preferably polyethylene glycol), a free fragrance (or a mixture of free fragrances), and optionally at least one binder.
[0039] In a first aspect, the present invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of the following: (a) At least one microcapsule containing an active ingredient, based on 0.5% to 10% by weight of the total weight of the tablets. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) Based on 92% to 98% by weight of the polymer in the total weight of the tablets, The polymer is preferably polyethylene glycol (PEG); and (c) 0.1% to 10% by weight of free fragrance or mixture of free fragrance (i.e., free fragrance component), and preferably hydrophobic fragrance or mixture of fragrance (i.e., hydrophobic free fragrance component). The above items are based on the total weight of the tablets.
[0040] Optionally, in another preferred embodiment, the tablets of the composition according to the first aspect further comprise or consist of the following: (d) 0.5% to 10% by weight (based on the total weight of the tablets) of at least one plasticizer, wherein the plasticizer is preferably water or polyethylene glycol; The above items are based on the total weight of the tablets.
[0041] In a second aspect, the present invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of the following: (a) At least one microcapsule containing an active ingredient, based on 0.5% to 10% by weight of the total weight of the tablets. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) at least one polymer, preferably polyethylene glycol, comprising 60% to 80% by weight of the total weight of the tablets; (c) At least one adhesive, comprising 2% to 32% by weight of the total weight of the tablets. The adhesive is preferably selected from the group consisting of: fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; and (d) 0.1% to 10% by weight of free fragrance or mixtures of free fragrance; The above items are based on the total weight of the tablets.
[0042] According to another preferred embodiment, the tablets of the composition according to the second aspect optionally also comprise or consist of the following: (e) at least one plasticizer, comprising 0.5% to 10% by weight of the total weight of the tablets. The plasticizer is preferably water or polyethylene glycol; and / or (f) 0.1% to 10% by weight of the structuring agent based on the total weight of the tablets. The structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; The above items are based on the total weight of the tablets.
[0043] Based on the above composition, an effective buffer or buffer system has been developed that effectively combines short-term and long-term release properties, especially fragrance properties, based on a combination of free fragrance and encapsulated fragrance for various products, particularly (solid) textile care products.
[0044] Preferably, the composition does not contain any inorganic or organic salts. These can negatively affect viscosity and thus the processability and stability of the resulting tablets.
[0045] Microcapsules and active ingredients, component (a) : The compositions according to the present invention comprise at least one microcapsule encapsulating an active ingredient, wherein the at least one microcapsule is dispersed in a polymer matrix.
[0046] Typically, microcapsules are particles comprising a core and a wall material surrounding the core, wherein the core can be a solid, liquid, or gaseous substance or mixture of substances (and preferably at least one active substance) surrounded by a polymer-dense, permeable, or semi-permeable wall material. The wall is typically formed by the precipitation of the polymer during emulsification and coagulation or interfacial polymerization. The core is also referred to as the inner phase. Other names for the wall include outer phase, shell, or coating. The shell wall may comprise one or more (different) layers and may include an additional coating with a coating substance. The diameter of microcapsules typically varies from 1 µm to 1,000 µm. The wall thickness is typically from 0.5 µm to 150 µm, but can be 5.10 µm. -9 m to 5.10 -6 The loading of nuclear material varies within the range of m. Typically, the loading is between 25% and 95% by weight, but loadings between 1% and 99% by weight are also possible.
[0047] For example, hydrophobic active ingredients (such as single fragrances (also known as aromatic / odorous substances or fragrance substances), fragrance mixtures (also known as mixtures of aromatic / odorous substances or mixtures of fragrance substances or fragrance oils), flavor substances or mixtures of flavor substances) can be easily incorporated into a wide variety of application formulations through encapsulation.
[0048] Based on their properties, microcapsules are particularly used in the printing industry, food industry (vitamins, seasonings, plant extracts, enzymes, microorganisms), agrochemicals (fertilizers, pesticides), feed industry (minerals, vitamins, enzymes, drugs, microorganisms), pharmaceutical industry, detergent industry, and cosmetics industry.
[0049] Various capsule wall or coating materials are known for use in the manufacture of microcapsules. Capsule walls can be made from natural, semi-synthetic, or synthetic materials. Natural shell materials include gum arabic, agar, agarose, maltodextrin, alginate or its salts (e.g., 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. Semi-synthetic capsule wall materials include chemically modified cellulose, particularly cellulose esters, and cellulose ethers, such as cellulose acetate, ethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and carboxymethyl cellulose, as well as starch derivatives, particularly starch ethers and starch esters. Synthetic shell materials are polymers such as polyacrylates, polyamides, polyvinyl alcohol, or polyvinylpyrrolidone.
[0050] Depending on the type of capsule wall material and its manufacturing method, microcapsules with different properties in terms of diameter, size distribution, and physical and / or chemical properties are formed in each case.
[0051] The microcapsules of component (a) of the composition according to the invention can be any microcapsule known to those skilled in the art.
[0052] Preferably, the microcapsules used within the scope of the invention are microcapsules in which the shell of at least one microcapsule comprises or is composed of a shell material selected from the group consisting of: sol-gel polymers (e.g., silica), polysiloxanes, polyacrylates, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polyamide, 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, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, polypeptides, polysaccharides, polyphenol polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), or combinations thereof.
[0053] The compositions according to the invention comprise at least one of the microcapsules, i.e., a single microcapsule of the above-described type is embedded in the polymer matrix of the invention, or two or more different microcapsules, or even multiple microcapsules, are embedded in the polymer matrix. Therefore, all microcapsules can be of the same type, i.e., all microcapsules are, for example, poly(melamine-formaldehyde) based, or some microcapsules of component (a) are, for example, poly(melamine-formaldehyde) based, while others are polyurea based, i.e., component (a) can comprise a mixture of different types of microcapsules based on different encapsulation / shell materials or consist of a mixture of different types of microcapsules based on different encapsulation / shell materials.
[0054] Furthermore, the microcapsules used in the compositions according to the invention can be loaded with different materials, such as different active ingredients, i.e., the compositions according to the invention contain different microcapsules on their core materials.
[0055] According to another preferred variant, the compositions according to the invention comprise different microcapsules, each with a different core material and a different shell material.
[0056] However, preferably, the microcapsules of component (a) according to the invention are selected from the group consisting of: poly(melamine-formaldehyde) microcapsules and isocyanate-based microcapsules, such as polyurea-based and / or polyurethane-based microcapsules and mixtures thereof, and these microcapsules are preferably biodegradable.
[0057] Biodegradable microencapsulation technology is known to those skilled in the art and is particularly suitable in the context of this invention in terms of environmental sustainability. Examples of such biodegradable microcapsules are isocyanate-based or polysaccharide-based microcapsules.
[0058] The biodegradation of microencapsulated slurries in the environment involves the biodegradation of the polymer shell according to the present invention. Measurements of the bioactivity or decomposition of the shell material can be determined under various conditions, including soil, seawater, or sludge, particularly under OECD guidelines. OECD tests that can be used to determine the biodegradability of organic chemicals include the six test methods described in OECD Test Guidelines 301A-F: DOC Die-Away test (TG 301 A), CO2 evolution test (TG 301 B), modified MITI test(I) (TG 301 C), closed bottle test (TG 301 D), modified OECD screening test (TG 301 E), and respiration rate test (TG 301 F). Further details can be found in the official OECD Chemicals Test Guidelines: OECD (2006). Revised Introduction to the OECD Guidelines for Testing of Chemicals , No. 3 Chapter, OECD Guidelines for the Testing of Chemicals, Chapter 3, OECD Publishing, Paris.
[0059] In the context of this invention, microcapsules are considered biodegradable if they meet the requirements of the OECD 301 F biodegradability standard (standardized OECD 301 F testing procedure: breathalyzer test). According to OECD 301 F, microcapsules are considered readily biodegradable if more than 60% of the wall material has degraded after 28 days.
[0060] Therefore, in the compositions according to the invention, at least one microcapsule is preferably biodegradable, according to OECD 301 F.
[0061] In the context of this invention, microcapsules are understood to be microparticles that include at least one or more active ingredients as core material within a capsule and are encapsulated by a capsule shell or capsule wall as specified above. As the active ingredient to be encapsulated according to the invention, substantially any material contained within the microcapsules may be considered suitable in the method according to the invention. Preferably, hydrophobic or lipophilic, i.e., water-insoluble or water-immiscible liquids or solids and suspensions, may be considered as the active ingredient to be encapsulated. These are primarily nonpolar substances. Such hydrophobic substances are almost always lipophilic, i.e., they dissolve well in fats and oils.
[0062] The terms “microcapsule” and “capsule” or “hydrophobic” and “lipophilic” are used synonymously in the context of this invention.
[0063] In the context of this description, the nuclear material is preferably a hydrophobic active substance, that is, a substance that has a specific function or causes a specific reaction, such as a drug, pesticide, cosmetic active ingredient, food active ingredient, etc.
[0064] Preferably, at least one lipophilic or hydrophobic active ingredient or substance is a single lipophilic or hydrophobic aromatic substance or fragrance substance or lipophilic or hydrophobic fragrance oil or fragrance agent (i.e., a mixture of two or more aromatic substances or two or more fragrance substances), a coolant, TRPV1 or TRPV3 regulator, a substance that produces a spicy or warm or hot sensation on the skin or mucous membranes or a stinging sensation in the mouth or throat, or an active ingredient with astringent properties, pesticide, biocide, insecticide, substance selected from the group including insect repellents, food additive, cosmetic active ingredient, pharmaceutical active ingredient, dye, dye precursor; agrochemical, dye, luminescent paint, optical brightener, solvent, wax, silicone oil, lubricant, paper printing coating, or a mixture of two or more of the above active ingredients.
[0065] In a preferred embodiment of the invention, the microcapsule has a core material comprising or consisting of: a hydrophobic single aromatic substance or a single odorant or a mixture of two or more such substances, wherein the core material comprises at least one single aromatic substance or a single odorant or a mixture thereof (i.e., fragrance oil), selected from one or more of the following groups: Extracts of natural raw materials and their fractions or components separated from them; single aromatic substances derived from a group of hydrocarbons; aliphatic alcohols; aliphatic aldehydes and acetals; aliphatic ketones and oximes; aliphatic sulfur compounds; aliphatic nitriles; esters of aliphatic carboxylic acids; formate, acetate, propionate, isobutyrate, butyrate, isovalerate, valerate, hexanoate, crotonate, thiocyanate and 3-methyl-2-butenoate of acyclic terpene alcohols; noncyclic terpene aldehydes and ketones and their dimethyl and diethyl acetals; formate, acetate, propionate, isobutyrate, butyrate, cycloterpene alcohols. Acid esters, isovalerates, valerates, hexanoates, crotonates, terpenoids, and 3-methyl-2-butenoates; cyclic terpenoid aldehydes and ketones; cyclic alcohols; cyclic and cyclic aliphatic ethers; cyclic and macrocyclic ketones; cyclic aliphatic aldehydes; cyclic aliphatic ketones; esters of cyclic alcohols; esters of cyclic aliphatic carboxylic acids; aromatic hydrocarbons; aryl aliphatic alcohols; esters of aryl aliphatic alcohols and aliphatic carboxylic acids; aryl aliphatic ethers; aromatic and aryl aliphatic aldehydes; aromatic and aryl aliphatic ketones; aromatic and aryl 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.
[0066] The terms “fragrant agent” and “fragrant substance” or “fragrant substance” or “odor (substance)” or “odorous substance” are used synonymously in the context of this invention.
[0067] Specific examples of the substances described above are known to those skilled in the art. Aromatic or odorous substances, as well as mixtures of two or more of these substances, are chemical substances or compositions used to impart, give, and / or modulate a particular odor or odor impression. Preferably, the odor (impression) is considered pleasant.
[0068] In an alternative embodiment of the invention, the microcapsules according to the invention use aromatic substances or fragrance oils, or flavoring substances or fragrances, as the active ingredient to be encapsulated or as the core material. These are compositions containing at least one aromatic substance or at least one fragrance substance. Such compositions, particularly mixtures of aromatic substances or fragrance oils, preferably include two, three, four, five, six, seven, eight, nine, ten or more aromatic substances.The aromatic mixtures or fragrance oils are preferably selected from the group consisting of: extracts of natural raw materials, such as essential oils, gels, absolutes, resins, aromatic resins, balsams, tinctures such as ambergris oil; sandalwood oil; angelica seed oil; angelica root oil; fennel oil; valerian oil; basil oil; tree moss absolute; laurel oil; artemisia oil; benzoin resin; bergamot oil; beeswax absolute; birch tar; bitter almond oil; peppermint oil; buchu leaf oil; Brazilian sandalwood oil; juniper oil; calamus oil; camphor oil; cananga oil; cardamom oil; calamus oil; cinnamon oil; acacia absolute; castoreum absolute; North American cedar leaf oil; cypress oil; rock rose oil; lemongrass oil; citronella oil; lemon oil; taffy balsam; taffy balsam oil; coriander oil; costus root oil; cumin oil; cypress oil; artemisia oil; dill oil; dill seed oil; Eau de Brouts absolute; Oakmoss absolute; Elemi oil; Tarragon oil; Lemon eucalyptus oil; Eucalyptus oil; Fennel oil; Spruce needle oil; White pine resin oil; White pine resin; Bay leaf oil; Grapefruit oil; Guaiac oil; Guvin balsam; Guvin balsam oil; Immortelle absolute; Immortelle oil; Ginger oil; Iris root absolute; Iris root oil; Jasmine absolute; Sweet flag oil; Blue chamomile oil; Roman chamomile oil; Carrot seed oil; Carrageenan oil; Pine needle oil; Peppermint oil; Coriander oil Seed oil; rockrose oil; rockrose absolute; rockrose resin; mixed lavender absolute; mixed lavender oil; lavender absolute; lavender oil; lemongrass oil; angelica pubescens oil; distilled white lemon oil; pressed white lemon oil; agarwood oil; litsea cubeba oil; bay leaf oil; nutmeg oil; marjoram oil; citrus oil; masala bark oil; mimosa absolute; musk seed oil; musk tincture; muskrat oil; musk sage oil; musk oil; myrrh absolute; myrrh oil; myrtle oil; cloves Bay leaf oil; clove flower oil; neroli oil; frankincense absolute; frankincense oil; myrrh oil; neroli absolute; orange oil; oregano oil; palmarosa oil; patchouli oil; perilla oil; Peruvian balsam oil; parsley leaf oil; parsley seed oil; orange leaf oil; pepper oil; allspice oil; pine oil; peppermint eucalyptus oil; rose absolute; rosewood oil; rose oil; rosemary oil; Dalmatian sage oil; Spanish sage oil; sandalwood oil; celery seed oil; spicy lavender oil Star anise oil; styrax oil; marigold oil; fir oil; tea tree oil; turpentine oil; thyme oil; turmeric balsam; tonka bean oil; tuberose oil; vanilla extract; violet leaf oil; verbena oil; vetiver oil; juniper berry oil; wine yeast oil; artemisia oil; wintergreen oil; ylang-ylang oil; hyssop oil; civet oil; cinnamon leaf oil; cinnamon bark oil; and their fractions or components separated from them, as well as mixtures of the foregoing substances.
[0069] In another variant of the invention, the fragrance substance may also be encapsulated as a core material, wherein the core material comprises at least one single fragrance substance or a mixture of two or more different fragrance substances as an active ingredient.
[0070] However, preferably, a single aromatic or odorous substance (i.e., chemical compounds having an odor or smell, and all natural and synthetic substances that thus impart a perceptible odor to the sense of smell) or alternatively a mixture of aromatic or odorous substances (so-called fragrance oils) is used as the active ingredient encapsulated in a microcapsule shell. More preferably, said substance and mixtures of substances impart a pleasant odor to the consumer product.
[0071] In a preferred variant of the invention, all microcapsules of component (a) are loaded with the same active ingredient, for example, all microcapsules of the microcapsules contain a fragrance substance and even more preferably contain the same fragrance substance.
[0072] According to an alternative embodiment, microcapsules of component (a) according to the invention encapsulate different kinds of active ingredients or different substances of the same kind of active ingredients. For example, some microcapsules contain a specific fragrance substance, while other microcapsules encapsulate another fragrance substance.
[0073] Therefore, it is preferable to select a core material without considering the shell material.
[0074] Therefore, according to another preferred variant of the invention, the tablets of the invention may comprise one type of microcapsule or a mixture of two or more different types of microcapsules. Thus, the microcapsules may vary in terms of their active ingredient composition (i.e., the microcapsule core) and / or wall composition (i.e., the material of the capsule shell).
[0075] According to the present invention, the composition comprises at least one microcapsule dispersed within a polymer component (b), which is preferably a water-soluble polymer matrix.
[0076] Based on the total weight of the tablets, microcapsules can be incorporated into the final composition at a rate between 0.5% and 10% by weight, i.e., a single tablet of the composition according to the invention contains between 0.5% and 10% by weight of the microcapsules specified above. If the amount of microcapsule component (a) is maintained within these ranges, uniform distribution of the microcapsules within the tablets can be achieved. Furthermore, if the amount of component (a) is within the aforementioned range, the active ingredient can be effectively incorporated into the final solid consumer product formulation due to the effective protection of the surrounding polymer matrix; i.e., the microcapsules do not rupture during the preparation of the solid consumer product, and thus the encapsulated active ingredient can be effectively retained without loss, resulting in significantly improved microcapsule performance, as shown in the experimental section.
[0077] Therefore, according to a preferred embodiment, the amount of microcapsules ranges from 0.5% to 10% by weight based on the total weight of the tablets, and even more preferably from 3% to 8% by weight based on the total weight of the tablets.
[0078] According to the present invention, at least one microcapsule encapsulating an active ingredient is dispersed in a polymer matrix (or polymer matrix).
[0079] Therefore, the compositions of the present invention comprising microcapsules encapsulating active ingredients can be effectively incorporated into a variety of solid consumer product formulations, thereby allowing for the effective and targeted release of the active ingredients. The surrounding polymer matrix thus acts as a shock-absorbing layer, protecting the microcapsules from damage due to mechanical, chemical, and / or thermal effects, and thus preventing premature release and degradation of the active ingredients during the preparation of the consumer product.
[0080] Polymer or polymer matrix, component (b): As specified above, the compositions / tablets according to the invention comprise or consist of at least one polymer in 92% to 98% by weight or 60% to 80% by weight (based on the total weight of the tablets).
[0081] Suitable polymers according to the invention are meltable polymers, such as polyethylene glycol (“PEG”) with a molecular weight of, for example, from about 3,000 Da to 20,000 Da, preferably from about 4,000 Da to 12,000 Da, and even more preferably from about 5,000 Da to 8,000 Da.
[0082] Component (b) may comprise a specific polymer having a molecular weight within the range specified above, or two or more different polymers. The different polymers may be the same substance differing in molecular weight within the specified range (such as PEG 3,000 and PEG 4,000), or they may be different chemical substances having the same or different molecular weights.
[0083] If the molecular weight of the polymer used as component (b) is within the range specified above, effective protection of fragile microcapsules can be achieved, thereby allowing effective incorporation into solid consumer product formulations while allowing effective targeted release of the active ingredient.
[0084] The polymer matrix protects the microcapsules from chemical and mechanical effects while allowing for high release performance. This protection allows for the efficient incorporation of the loaded microcapsules into a wide range of consumer product formulations, and particularly solid consumer product formulations. In the manufacture of such compositions, fragile microcapsules are subjected to high shear, which causes the microcapsules to rupture and thus premature release of the active ingredient. Surprisingly, the compositions according to the invention have been found to be advantageously incorporable into such formulations, thereby exhibiting improved performance and chemical and mechanical stability in these formulations, during their manufacture, and with respect to other components.
[0085] In the context of this invention, a “meltable” polymer is a plastic polymer material that becomes flexible or moldable at a specific elevated temperature and solidifies upon cooling.
[0086] The polymers used in the context of this invention may be water-soluble or water-insoluble polymers. According to an alternative embodiment, component (b) comprises a mixture of one or more water-soluble polymers, a mixture of one or more water-insoluble polymers, or a mixture of one or more water-soluble polymers and one or more water-insoluble polymers.
[0087] In a preferred variant of the invention, the polymer according to the invention (preferably having a molecular weight of about 3,000 Da to 20,000 Da) preferably has a melting point in the range of 25°C to 100°C, and more preferably in the range of 40°C to 80°C.
[0088] However, preferably, the polymer used as component (b) in the context of this invention is water-soluble. For example, when incorporated into textile care formulations such as powdered detergents, the polymeric protective matrix dissolves, thereby releasing the microcapsules and thus effectively applying the microcapsules to the textiles. This has the added advantage that the microcapsules are not damaged during storage, processing, product preparation, etc., thus preventing premature release of the active ingredients. The water-soluble polymeric matrix dissolves during the washing process and effectively releases both the encapsulated fragrance components and the free (i.e., unencapsulated) fragrance components without leaving unacceptable residues on the treated fabric.
[0089] Examples of suitable water-soluble polymers include, for example, polyvinyl alcohol, polyvinyl alcohol derivatives (such as quaternary ammonium derivatives), polyethylene glycol (with different molecular weights), polyvinylpyrrolidone, (poly)acrylates, polyacrylic acid, acrylamide, polyamino acids and amine functional polymers, sugars and polysaccharides (such as starch, modified starch, maltodextrin, carbohydrates, chitosan and gum arabic), maleic anhydride copolymers, vinyl acids and ethers, styrene, polystyrene sulfonate, ethylene glycol-propylene glycol block copolymers and mixtures thereof. Examples of suitable water-insoluble polymers include classic coated capsules, waxes such as beeswax, sunflower seed wax, rice bran wax, carnauba wax, pinova wax, rapeseed wax, soybean wax, candelilla wax, jojoba oil, cork wax, guarana wax, cotton wax, linseed wax, peat wax, rose wax, jasmine wax, winter melon pita wax, myrtle wax (waxed peach wood ( Myrica cerifera ( ), fig wax, berry wax, and mixtures of different waxes.
[0090] In a preferred embodiment of the invention, the polymer is preferably polyethylene glycol (PEG, also known as polyethylene oxide (PEO) or polyethylene oxide (POE)) with a molecular weight of about 3,000 Da to 20,000 Da, preferably about 3,000 Da to 12,000 Da, and even more preferably about 4,000 Da to 9,000 Da.
[0091] According to an alternative preferred embodiment, component (b) comprises a mixture of two or more polyethylene glycols that differ in molecular weight.
[0092] Polyethylene glycol (PEG) is an inexpensive, synthetic, hydrophilic, and biocompatible polymer widely used in biomedical and other applications, such as as an excipient or laxative in pharmaceutical compositions, as a lubricating coating in the chemical industry, and as a cream base or dispersant in cosmetic formulations. PEG is a flexible, water-soluble polymer with low toxicity that can be incorporated into a variety of formulations and has the general formula: C 2n H 4n+2 O n+1 .
[0093] The composition of the invention according to the first aspect may comprise 91% to 98% by weight of a polymer (component (b)) based on the total weight of the tablets, preferably 92% to 98% by weight of the tablets, and even more preferably 92% to 96% by weight.
[0094] A lower amount of polymer component implicitly implies a higher amount of microencapsulated component. Because the microencapsulated component is preferably added in the form of an aqueous slurry, the increased water content will result in a softer and more viscous composition, making the preparation of the tablets more challenging (see [link to product]). Figure 6 and Figure 7 ).
[0095] The composition of the invention according to the second aspect may comprise 60% to 80% by weight of polymer (component (b)) based on the total weight of the tablets, preferably 65% to 75% by weight of the tablets, and even more preferably 70% to 75% by weight.
[0096] Further investigation revealed that lower polymer content (i.e., less than 60% by weight based on the total weight of the tablets) resulted in reduced water solubility of the tablets in solid detergent formulations, for example. In this case, the desired effect was no longer achieved, and the composition according to the invention did not exhibit the expected release performance. On the other hand, if the polymer content was too high, i.e., more than 80% by weight based on the total weight of the tablets, the composition became stiff, making the tablet manufacturing process more difficult.
[0097] If the polymer specified above is included in the composition according to the invention within the range specified above, effective protection of the fragile microcapsules within the polymer matrix can be achieved while allowing effective targeted release of the active ingredient.
[0098] According to another preferred variant of the invention, the polymer exhibits specific freezing points: the lowest freezing point of the water-soluble polymer-like particles (i.e., the final tablets) is preferably above 0°C, preferably above 20°C, and particularly preferably above 35°C, while the lowest freezing point of the non-water-soluble polymer-like particles is above 0°C, preferably above 20°C, and particularly preferably above 35°C. Freezing points within these ranges allow for the facilitated formation of tablets according to the invention without requiring low temperatures for the tablet preparation process and its subsequent processing.
[0099] According to the present invention and a preferred embodiment, no additional solid carrier is required to incorporate the composition according to the invention into the product formulation. Therefore, the total amount of ingredients and waste can be further reduced without negatively impacting the intended efficacy.
[0100] adhesives : Interestingly, it was further discovered that the combination of the polymers specified above with the additional binders specified herein also resulted in effective protection of the microcapsules when incorporated into solid consumer product formulations.
[0101] Therefore, in a second aspect, the present invention relates to a composition comprising or consisting of: a microcapsule component (component (a)), a polymer component (component (b)); a binder component (component (c)) and a free fragrance component (component (d)) in a specific ratio. Thus, components (b) and (c) form a protective matrix surrounding (i.e., encapsulating) fragile microcapsules.
[0102] The adhesive according to the invention is defined as a substance (adhesion promoter or deposition aid) that allows microcapsules to have increased adhesive force on external materials and their surfaces (such as textiles). Adhesion is based on mechanical bonding, hydrogen bonding, chemical or covalent bonding, thermodynamic bonding, etc.
[0103] Preferably, the binder used as component (c) according to the second aspect of the invention is a substance selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as natural waxes and synthetic waxes. Therefore, a composition according to the second aspect of the invention may contain one such binder or a mixture of two or more such binders as component (c).
[0104] Other suitable adhesives include: Long-chain, aliphatic, straight-chain or branched, saturated or unsaturated carboxylic acids (fatty acids) with 12 to 30 carbon atoms, especially lauric acid (12:0), tridecanoic acid (13:0), myristic acid (14:0), pentadecanoic acid (15:0), palmitic acid (16:0), heptadecanoic acid (17:0), stearic acid (18:0), nonadecanoic acid (19:0), arachidic acid (20:0), icosanoic acid (21:0), benzanoic acid (22:0), tetracosanoic acid (24:0), ceric acid (26:0), linalic acid (28:0), and beeswax acid (30:0); myristenoic acid (14:1), palmitic acid (16:1), cis-9-heptadecenoic acid (17:1), phellandrene (18:1), oleic acid (18:1), trans... Oleic acid (18:1), isoleic acid (18:1), codoleic acid (20:1), stigmocarboxylic acid (20:1), cetylene acid (22:1), erucic acid (22:1), nervonic acid (24:1), linoleic acid (18:2), α-linolenic acid (18:3), γ-linolenic acid (18:3), calendula acid (18:3), pomegranate acid (18:3), α-tungsten acid (18:3), β-tungsten acid (18:3), octadecanoic acid (18:4), arachidonic acid (20:4), eicosapentaenoic acid (20:5), docosahexaenoic acid (ADA) (22:4), docosapentaenoic acid (DPA-3) (22:5), docosahexaenoic acid (22:6) and docosahexaenoic acid (24:6), phytic acid; Long-chain, aliphatic, straight-chain or branched, saturated or unsaturated primary alcohols (fatty alcohols) having 12 to 30 carbon atoms, especially lauryl alcohol (12:0), myristyl alcohol (14:0), palmitol (16:0), heptadecanol (17:0), stearyl alcohol (18:0), arachidyl alcohol (20:0), betaine alcohol (22:0), tetracosyl alcohol (24:0), hexacosyl alcohol (26:0), octacosyl alcohol (28:0) and beeswax alcohol (30:0); palmitole alcohol (16:1), oleyl alcohol (18:1), transoleyl alcohol (18:1), linoleyl alcohol (18:2), γ-linolenic acid alcohol (18:3); Esters of long-chain aliphatic saturated carboxylic acids containing 12 to 30 carbon atoms and long-chain aliphatic primary alcohols containing 12 to 30 carbon atoms, particularly lauryl palmitate, beeswax palmitate, cetyl arachidate and stearyl behenate. Animal waxes and plant waxes, especially beeswax, wool wax, Chinese wax, rice bran wax, sunflower seed wax, carnauba wax, sugarcane wax, Pinova wax, rapeseed wax, soybean wax, candelilla wax, jojoba oil, cork wax, guarana wax, small crown coconut wax (Syagrus coronata), Cuban carnauba wax (Copernicia hospita), spartum wax (Lygeum spartum, Stipatenacissima), cotton wax, linseed wax, peat wax, rose wax, jasmine wax, wash gourd pita wax, as well as myrtle wax (Myrica cerifera), wax fig wax, and berry wax.
[0105] And mixtures of two or more of the above adhesives.
[0106] Of the carboxylic acids listed above, saturated fatty acids are particularly preferred. In the context of this invention, the use of animal and vegetable waxes as specified above is most preferred because of their low melting points, which facilitates their incorporation into the composition.
[0107] According to another preferred embodiment, at least one adhesive is selected from the group consisting of animal waxes and / or plant waxes, and preferably (natural) beeswax.
[0108] In another preferred variant, at least one agent is selected from animal waxes and / or plant waxes, and is preferably selected from the group consisting of: beeswax, wool wax, Chinese wax, rice bran wax, sunflower seed wax, rice bran wax, carnauba wax, sugarcane wax, Pinova wax, rapeseed wax, soybean wax, candelilla wax, jojoba oil, cork wax, guarana wax, crown palm wax (crown carnauba), Cuban carnauba wax (dense vein wax palm), papyrus wax (paspalum), cotton wax, linseed wax, peat wax, rose wax, jasmine wax, wash melon rind wax, and myrtle wax (waxed fruit wax), waxed fig wax, berry wax, and mixtures thereof.
[0109] Furthermore, it was surprisingly found that binders such as those specified herein (e.g., animal waxes and / or plant waxes) have a positive effect on the performance of the tablets. Specifically, tablets containing animal waxes and / or plant waxes exhibit improved protective properties and improved release properties, taking into account the microcapsules embedded therein, thereby allowing for more effective protection and targeted release of the active ingredients.
[0110] Furthermore, it has been found that binders, as specified herein, and in particular animal and / or plant waxes, have a positive effect on the initial odor impression of formulations containing aromatic active ingredients.
[0111] Surprisingly, it has been found that such natural or synthetic animal waxes and / or plant waxes can be effectively incorporated into compositions according to the second aspect. Furthermore, these substances allow for improved adhesion of microcapsules to surfaces of other materials, such as textile fibers, while simultaneously supporting the protective effect of the polymer matrix, thus demonstrating several advantages. In other words, the adhesives specified herein not only improve the adhesion of the active ingredients to the corresponding surfaces but also simultaneously improve the protection of fragile microcapsules and even allow for improved performance.
[0112] According to another preferred embodiment, at least one adhesive is a plant wax, i.e., a plant-derived wax.
[0113] Alternatively, according to another preferred embodiment, at least one adhesive is an animal wax, such as beeswax or lanolin (a wax obtained from wool).
[0114] Furthermore, it was observed that the combination of polymers (e.g., polyethylene glycol) with binders (e.g., beeswax) specified herein resulted in significant performance improvements compared to compositions containing a pure polyethylene glycol matrix, indicating improved shock absorption and protection. The use of microcapsules embedded in a polymer-binder-matrix resulted in even more improved performance in consumer products.
[0115] Furthermore, a comparison of samples with and without the added binder revealed that the addition of the binder not only improved the manufacture and preparation of more uniform tablets, but also led to an improved sensory experience by allowing for more effective protection of fragile microcapsules and thus more targeted release of fragrances. Therefore, based on their sensory-enhancing properties, the binder was found to additionally act as a "fragrance enhancer."
[0116] The addition of binders as specified in this paper was found to improve release performance / sensory performance and thus improve the sensory experience by one unit, i.e., an increase in strength / efficacy of more than 10%. Therefore, the binders used in this paper are also considered "sensory enhancers" or "fragrance enhancers".
[0117] Further investigation revealed that different types of waxes can be appropriately used as such adhesives.
[0118] Therefore, considering health and environmental aspects, bio-based or bio-derived reagents are preferred. Bio-based materials (bio-derived materials) refer to compounds containing organic carbon from renewable sources, such as agricultural, plant, animal, fungal, microbial, marine, or forestry materials living in a natural environment in balance with the atmosphere, or non-fossil sources such as petroleum, as defined by testing according to ASTM D6866 standard. Furthermore, by definition, such bio-based compounds are carbon-containing compounds (organic and inorganic) from renewable sources, such as agricultural, plant, animal, fungal, microbial, marine, or forestry materials. Preferably, the compositions of the present invention comprise such bio-based or bio-derived materials. Therefore, bio-derived materials are preferably used in the preparation of tablets and thus in the compositions according to the present invention.
[0119] Therefore, in another preferred variant of the invention, preferably, at least one adhesive is selected from the group consisting of bio-based materials, such as naturally occurring animal waxes and / or plant waxes.
[0120] According to an alternative preferred variant, at least one adhesive is paraffin wax.
[0121] The adhesive components are incorporated into the polymer matrix.
[0122] Preferably, the adhesive used as component (c) according to the second aspect of the invention comprises 2% to 32% by weight based on the total weight of the tablets, more preferably 3% to 20% by weight of the tablets, and more preferably 4% to 17% by weight, and most preferably 5% to 10% by weight.
[0123] The addition of adhesives within the specified range allows for an improved balance between microcapsule protection, adhesion promotion, and fragrance enhancement.
[0124] Furthermore, it has been found that if the concentration of the polymer matrix (preferably PEG matrix) is in the range of 0.95 g / cm³ to 1.10 g / cm³, and preferably 0.99 g / cm³ to 1.05 g / cm³, a further improved balance between microcapsule protection and release properties can be achieved. Moreover, if the density is within the above range, it has been found that the homogeneity of the tablets according to the invention is improved, and the preparation of the tablets according to the invention becomes further facilitated.
[0125] Density was determined as bulk density, which is defined as the mass of particles per volume of a continuous fluid / solvent mixture in the cavity between solid bulk material and filling particles.
[0126] As mentioned above, a lower amount of polymer component implicitly implies a higher amount of microencapsulated component. Because the microencapsulated component is preferably added in the form of an aqueous slurry, the increased water content will result in a softer and more viscous composition, making the preparation of the tablets more challenging (see [link to article]). Figure 6 and Figure 7 Surprisingly, this effect can be partially compensated by adding an adhesive as specified herein. However, it is preferred that the total amount of adhesive be kept low, and preferably less than 10% by weight of the spinneret, to avoid potential disadvantages such as the formation of stains on textiles, for example, caused by water-insoluble adhesive components (such as waxes) during the textile washing process.
[0127] Free fragrance or unencapsulated fragrance (fragrance emulsifier) : According to the present invention, the composition further comprises a free fragrance agent. The term "free fragrance agent" refers to a single fragrance agent substance or a mixture of two or more fragrance agent substances dispersed in an unencapsulated (or non-encapsulated) form within a polymer matrix, i.e., the fragrance component is not present in the form of discrete microcapsules.
[0128] The compositions according to the invention additionally must contain a single free aromatic substance or a mixture of two or more aromatic substances (i.e., a free aromatic mixture or a free fragrance oil), that is, the compositions according to the invention additionally contain at least one unencapsulated or free aromatic substance as an additional component. Sensory data show that the addition of free oil / free aromatic components provides a better odor impression.
[0129] Therefore, olfactory properties can be further enhanced, and the final product, as well as freshly treated textiles, immediately exhibit perceptible olfactory properties. In the case of encapsulated fragrances, the rupture of microcapsules adds an additional, intense aroma.
[0130] Preferably, the free fragrance substance or a mixture of free fragrance substances (a mixture of two or more fragrance substances) is contained in an amount of 0.1% to 10% by weight based on the total weight of the tablets, and more preferably in an amount of 2% to 8% by weight, and more preferably in an amount of 2% to 5% by weight.
[0131] Suitable aromatic substances and their mixtures are described above in the context of microencapsulation.
[0132] When the encapsulated active ingredient is a fragrance or a mixture of fragrance substances, the free fragrance component (a single free fragrance substance or a mixture of two or more fragrance substances) may be the same as or different from the encapsulated fragrance component in terms of quantity and / or chemical composition.
[0133] The free fragrance component serves as an emulsifier (“fragrance emulsifier”) and further facilitates the preparation of the tablets according to the invention in a more uniform manner, while increasing olfactory benefits.
[0134] Surprisingly, the presence of free aromatic components dispersed within the polymer matrix resulted in further improved release properties. Figure 1 Furthermore, a relatively high initial fragrance experience can be achieved before the microcapsules are mechanically broken, thereby releasing the encapsulated fragrance. Figure 1 Therefore, the aroma experience achieved by the composition according to the invention is (i) prolonged and present from the beginning (i.e., immediately after treatment), and (ii) enhanced and more uniform over time.
[0135] Surprisingly, the included free fragrance component further improves the final product properties, allowing for effective tuning of the viscosity and flexibility of the polymer matrix, resulting in a less brittle and more flexible matrix with improved cushioning and thus better protection for fragile microcapsules, as well as facilitated incorporation into solid consumer product formulations without altering the fundamental chemical properties of the plasticizer (see [link to product description]). Figures 1 to 4 ).
[0136] Furthermore, it was surprisingly found that the free fragrance component promotes tablet formation and significantly improves the miscibility of the microcapsule component, polymer component, and other optional components or additives, thereby allowing for a more uniform distribution of the microcapsules (and therefore the active ingredient) within the polymer matrix. The presence of the free fragrance surprisingly reduces the viscosity of the composition and thus positively impacts the composition's properties by allowing for a more uniform distribution of the tablet components. Additionally, processability is facilitated. This allows for the preparation of more stable tablets with improved release properties. For fragrance microcapsules, improved and more uniform aroma release was observed when combined with the free fragrance. Furthermore, the compositions according to the invention allow for an immediately perceptible aroma experience.
[0137] Even more surprisingly, it was found that the aforementioned beneficial effects could not be achieved by using only common plasticizers and / or structuring agents (such as isopropyl myristate, which is not a fragrance substance).
[0138] These beneficial effects can be observed in a wide range of aromatic substances and their mixtures, and are not limited to specific chemical classes of aromatic substances.
[0139] However, for fragrance substances (such as Agrumex LC, citronellol, decanal, dodecaldehyde (lauraldehyde), methyl nonacetaldehyde, so-called tetradecanal, allyl hexanoate, amarose, imperial ambergris, amyl salicylate, benzaldehyde, benzyl acetate, benzyl acetone, benzyl salicylate, borneol / isoborneol 65:35, pogiflorin, citronellol 950, styracil, CM20 santalin substitute, styracil, coumarin, styracil aldehyde, cyclohexyl salicylate, daumatone, butyrate, etc.) O-Turkeyone, Decenol, Dihydromyrcenol, Dimethylbenzyl alcohol, Dimethylbenzyl acetate, Diphenyl ether, Dipropylene glycol, Dynasty ketone, Ethyl decanoate, Eucalyptus oil, Eugenol, Sea bast aldehyde, Lily of the valley pyran BM / Lily of the valley pyran, Supergeraniol, Geraniyl acetate 60, Hexyl acetate, Hexyl salicylate, α-Hexylcinnamaldehyde, Isoboronyl acetate, Isooctone, Isodralein 70 70), p-cresol methyl ether, resveratrol, citrate, lily aldehyde, linalool, linalyl acetate, chamomile ester, cucurbitacinol, methyl octyne carboxylate, osmanthus aldehyde, lily of the valley oil, orange oil, patchouli oil, paeonol, phenylethanol acetate, phenylethanol, methyl phenethyl ether, pine acetaldehyde, high cis-rose oxide, oleinone, styrax acetate, BHT-free tamarin base, terpineol, timothymol, 2-undecenone, methyl decenol, methyl cypressone, ambroxol, YlangColipa Base, and mixtures thereof), yielded particularly good results.
[0140] Other particularly suitable fragrance substances are selected from the group consisting of hydrocarbons, such as natural δ-carene, natural refined caryophyllene, natural L-pinene, γ-terpinene, and mixtures thereof.
[0141] Other suitable free aromatic substances are selected from the group consisting of esters (such as benzyl butyrate) and / or aldehydes (such as decanal) and mixtures thereof. Figure 3 and Figure 4 ).
[0142] Plasticizer: The compositions according to the invention may also contain a certain amount of at least one plasticizer as an additive. Therefore, the compositions according to the invention may contain a single plasticizer or a mixture of two or more such plasticizers.
[0143] Plasticizers are substances used to increase the flexibility and plasticity of a particular substance or composition and may additionally reduce the viscosity and friction of the substance or composition.
[0144] Suitable plasticizers are known to those skilled in the art. Suitable plasticizers include, for example, water, polyethylene glycol, phthalates, trimellitates and their esters, (organic) phosphate esters, aliphatic diesters, benzoates, polyesters, citrates, bio-derived plasticizers based on epoxidized soybean oil, epoxidized linseed oil, castor oil, palm oil, other vegetable oils, starch, sugars, etc., chlorinated paraffins, alkyl sulfonates, dicarbonates, and fatty acid esters.
[0145] Preferably, the plasticizer is selected from water or polyethylene glycol, etc. The water plasticizer may be derived, for example, from the manufacturing process of the tablets or may be added subsequently.
[0146] According to a preferred variant, the plasticizer, and preferably the water plasticizer, is provided by the addition of an aqueous microcapsule slurry (component (a)), wherein the aqueous phase of the microcapsule slurry is used as the plasticizer.
[0147] According to an alternative preferred variant, polyethylene glycol is used as a plasticizer component. Preferably, in this case, the molecular weight of the plasticizer polyethylene glycol is less than 4,000 Da, more preferably less than 3,500 Da, and most preferably less than 3,000 Da.
[0148] Preferably, the amount comprising 0.5% to 10% by weight, more preferably 2% to 8% by weight, and more preferably 3% to 6% by weight of the total weight of the tablets, is the plasticizer used as an additive according to the invention.
[0149] Within the specified range, the addition of plasticizers allows for the effective adjustment of the viscosity and flexibility of the polymer matrix, resulting in a less brittle and more flexible matrix with improved cushioning and thus better protection for fragile microcapsules and facilitating incorporation into solid consumer product formulations, without altering the fundamental chemical properties of the plasticizer.
[0150] Structured agents : Alternatively or additionally, one or more structuring agents may be added to the compositions according to the invention as specified above as additional components or additives. Therefore, the compositions according to the invention may comprise a single structuring agent or a mixture of two or more such structuring agents.
[0151] Therefore, according to another preferred embodiment, the composition according to the first and second aspects of the invention comprises at least one surfactant.
[0152] The structuring agent is preferably contained in an amount of 0.1% to 10% by weight, preferably 1% to 8% by weight, and even more preferably 2% to 7% by weight, based on the total weight of the tablets.
[0153] Suitable structuring agents are commercially available surfactants or emulsifiers and esters known in the art, such as isopropyl myristate.
[0154] The addition of such structured substances leads to improved spheroid formation during droplet formation. Based on this, the incorporation of microcapsules / tablets into the final product formulation is enhanced in a uniform manner. These substances are, for example, additives that increase the viscosity of the composition to a viscous liquid, semi-solid, or solid state.
[0155] Furthermore, it was surprisingly found that the addition of a structuring agent further improved the homogeneity of the compositions of the present invention, particularly in the presence of wax. Mixtures of wax and polyethylene glycol tend to separate and form distinct phases. However, by adding a structuring agent as specified herein, a homogeneous formulation can be obtained.
[0156] Therefore, the structuring agent can be an emulsifier or a surfactant.
[0157] The addition of surfactants is particularly suitable for compositions containing adhesives as specified herein. Compositions according to the invention may contain any kind of surfactant, namely anionic surfactants, cationic surfactants, nonionic surfactants, amphoteric / amphoionic surfactants, and any mixtures thereof. Among these surfactants, nonionic surfactants are particularly preferred.
[0158] Suitable surfactants are selected from the group consisting of ammonium derivatives, esters, sulfonates, sulfates, sorbates and related surfactants and mixtures thereof.
[0159] Nonionic detergents are particularly advantageous for preparing “green” compositions.
[0160] The surfactants specified above may be used alone or in the form of a mixture of two, three or more surfactants from the same surfactant class (anionic, cationic, nonionic, amphoteric / amphoionic) or as a mixture of surfactants from different surfactant classes.
[0161] Preferably, the composition according to the second aspect of the invention comprises at least one surfactant, preferably a nonionic surfactant.
[0162] Therefore, in another preferred variant, the present invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of the following: (a) 0.5% to 10% by weight of at least one microcapsule encapsulating the active ingredient. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) 60% to 80% by weight of at least one polymer, preferably polyethylene glycol; (c) at least one adhesive, ranging from 2% to 32% by weight. The adhesive is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; The above items are based on the total weight of the tablets; and (d) 0.1% to 10% by weight of free fragrance or mixtures of free fragrance; The above items are based on the total weight of the tablets. The at least one tablet further comprises or consists of the following: At least one structuring agent, preferably a surfactant, and even more preferably a nonionic surfactant, comprising 0.1% to 10% by weight. The structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; The above items are based on the total weight of the tablets.
[0163] Additionally, if desired, the compositions according to the invention may contain other suitable additives. Other suitable additives are, for example, dyes, laundry active ingredients, etc.
[0164] Composition / tablets : The composition according to the invention comprises or consists of at least one tablet having the composition specified above. Preferably, the composition is present in the form of a plurality of tablets. Alternatively, the composition is present in a single tablet of the composition specified above according to the first or second aspect.
[0165] According to a first aspect of the invention, the composition of the invention comprises or consists of at least one tablet, the at least one tablet comprising an encapsulated active ingredient (preferably a fragrance (mixture)), a polymer forming a polymer matrix (preferably polyethylene glycol), and a free fragrance (mixture).
[0166] According to the first aspect, the composition therefore comprises or consists of at least one tablet, wherein the tablet comprises or consists of the following: (a) At least one microcapsule containing an active ingredient, based on 0.5% to 10% by weight of the total weight of the tablets, wherein the active ingredient is preferably a fragrance or a mixture of fragrances; (b) 92% to 98% by weight of a polymer based on the total weight of the tablets, wherein the polymer is preferably polyethylene glycol (PEG); and (c) 0.1% to 10% by weight of free fragrance or mixture of free fragrance; The above items are based on the total weight of the tablets.
[0167] Optionally, in another preferred embodiment, the tablets of the composition according to the first aspect further comprise or consist of the following: (d) 0.5% to 10% by weight (based on the total weight of the tablets) of at least one plasticizer, wherein the plasticizer is preferably water or polyethylene glycol.
[0168] According to another embodiment, the composition of the present invention comprises or consists of at least one tablet, the at least one tablet comprising an encapsulated active ingredient (preferably a fragrance (mixture)), a polymer forming a polymer matrix (preferably polyethylene glycol), a free fragrance (mixture), and optionally at least one binder.
[0169] Therefore, according to the second aspect, the composition comprises or consists of at least one tablet, wherein the tablet comprises or consists of the following: (a) At least one microcapsule containing an active ingredient, based on 0.5% to 10% by weight of the total weight of the tablets, wherein the active ingredient is preferably a fragrance or a mixture of fragrances; (b) at least one polymer, preferably polyethylene glycol, comprising 60% to 80% by weight of the total weight of the tablets; (c) at least one binder, comprising 2% to 32% by weight of the total weight of the tablets, wherein the binder is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; and (d) 0.1% to 10% by weight of free fragrance or mixtures of free fragrance; The above items are based on the total weight of the tablets.
[0170] Optionally, the tablets of the composition according to the second aspect may also optionally contain or consist of the following: (e) at least one plasticizer, based on 0.5% to 10% by weight of the total weight of the tablets, wherein the plasticizer is preferably water or polyethylene glycol; and / or (f) at least one structuring agent, comprising 0.1% to 10% by weight of the total weight of the tablets, wherein the structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; The above items are based on the total weight of the tablets.
[0171] Therefore, in another preferred variant, the present invention relates to a composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of the following: (a) 0.5% to 10% by weight of at least one microcapsule encapsulating the active ingredient. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) 60% to 80% by weight of at least one polymer, preferably polyethylene glycol; (c) at least one adhesive, ranging from 2% to 32% by weight. The adhesive is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; The above items are based on the total weight of the tablets; and (d) 0.1% to 10% by weight of free fragrance or mixtures of free fragrance; The above items are based on the total weight of the tablets. The at least one tablet further comprises or consists of the following: At least one structuring agent, preferably a surfactant, and even more preferably a nonionic surfactant, comprising 0.1% to 10% by weight. The structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; The above items are based on the total weight of the tablets.
[0172] Compositions according to the second aspect of the invention, which further include an adhesive as specified herein, exhibit improved protective and release properties. Furthermore, it has been found that the presence of the adhesive improves the preparation of such tablet compositions, resulting in more uniform, more flexible, and less brittle tablets with enhanced microcapsule distribution (see also Example 5).
[0173] In a preferred embodiment of the invention, the solidification point of the composition and therefore the tablets according to the invention is 25°C to 100°C, preferably 30°C to 90°C, more preferably 35°C to 85°C, and most preferably 40°C to 75°C.
[0174] The freezing point within this range allows for the facilitation treatment of the compositions and their tablets according to the invention.
[0175] According to another preferred embodiment, the composition according to the invention and thus the corresponding tablets have a viscosity η in the range of 500 mPas to 1,000 mPas at a temperature of 70°C and a shear pressure of 6.4 Pa, preferably in the range of 760 mPas to 980 mPas, and even more preferably in the range of 800 mPas to 950 mPas.
[0176] For the composition according to the invention, at a temperature of 70°C and a shear pressure of 6.4 Pa, the viscosity η is even more preferably in the range of 750 mPas to 1,000 mPas, preferably in the range of 760 mPas to 980 mPas, and even more preferably in the range of 800 mPas to 950 mPas. If the viscosity of the composition is within the above range, the composition is considered to be "solid" at room temperature.
[0177] Therefore, preferably, the composition according to the invention is a solid composition.
[0178] Furthermore, it was found that the viscosity of the composition affects the formation of the tablets through the dripping itself and the stability of the tablets (see [link]). Figure 6 and Figure 7 If the viscosity of the composition is within the aforementioned range, the processing of the composition (particularly in ingot-making processes as specified herein) and its incorporation into solid consumer product formulations become easier. Furthermore, if the viscosity is within the aforementioned range, an ideal balance between microencapsulation protection and microencapsulation performance can be achieved. Due to the low viscosity, the mixture can be better homogenized, while the lower viscosity allows for improved dripping behavior. In addition, if the viscosity of the composition is within the aforementioned range, the encapsulated active material can be distributed more uniformly within the ingot. Moreover, such viscosity provides improved ingot flexibility, i.e., the ingot is less brittle and simultaneously exhibits improved cushioning.
[0179] The viscosity can be adjusted accordingly by adjusting the amount of adhesive and plasticizer.
[0180] As the shear rate increases, the viscosity decreases within the range where dripping is still possible, thereby further improving the characteristics of the final product, particularly the stability, homogeneity, and processability of the tablet formulation.
[0181] Based on another preferred variant of the invention, the compositions and therefore corresponding tablets according to the invention have a Young's modulus E of more than 100 Pa and less than 1 GPa, preferably 1 kPa to 100 MPa, and even more preferably 10 kPa to 1 MPa.
[0182] Young's modulus E describes the tensile or compressive stiffness of a solid but elastic material in the linear elastic region of the material, based on tensile / compressive stress (force per unit area) and axial strain (proportional deformation).
[0183] The elasticity within this range allows for an ideal balance between microcapsule protection and its effective incorporation into solid consumer product formulations, while also allowing for excellent release characteristics.
[0184] In another preferred variant, the total water content in the composition according to the invention, and therefore the total water content of the corresponding tablets, is 2% to 12% by weight based on the total weight of the tablets. Preferably, the water content is in the range of 3% to 9% by weight, and even more preferably in the range of 4% to 8% by weight.
[0185] This amount of water is advantageous in terms of flexibility because the water component can act as a plasticizer, and is therefore valuable in terms of improved cushioning and thus better protection of fragile microcapsules, as well as facilitated incorporation into solid consumer formulations without altering the basic chemical properties of the plasticizer. Higher amounts of water would reduce viscosity too much, making incorporation into solid formulations more difficult, while low water content makes the tablet material brittle for incorporation.
[0186] Furthermore, it was found that if the total water content is within the range specified above, the preparation of the tablets becomes easier, resulting in a uniform tablet shape.
[0187] The above-described properties of the compositions according to the invention can be adjusted based on the specific amounts of the components, the molecular weights of the polymer and free fragrance components, and the optional addition of additives (such as the plasticizers and structuring agents described above).
[0188] Additionally, it is advantageous that, in order to achieve ideal distribution of the tablets within the final solid consumer product formulation, and thus, consequently, ideal distribution of the microcapsules embedded therein, the particle size of the tablets in the composition according to the invention is 1 µm to 1 cm, preferably 100 µm to 7 mm, and even more preferably 500 µm to 5 mm. Tablets that are too large result in uneven distribution within the final product formulation.
[0189] In another preferred variant of the invention, the ratio between the size of the microcapsules and the size of the final granules / tablets is in the range of 1:5 to 1:200, preferably 1:10 to 1:100.
[0190] The tablets or granules are preferably in the form of tablets, pills, spheres, etc., having spherical, hemispherical, compressed hemispherical, lentil-shaped, and rectangular shapes, and can be prepared by any method known to those skilled in the art (see [link to relevant documentation]). Figure 6 ).
[0191] Furthermore, the compositions and tablets of the present invention may also include one or more ingredients that improve the visual aesthetics of the final product, such as colorants. Additionally, the compositions may contain further additives and / or active ingredients, such as optical brighteners, detergents, laundry active substances, etc.
[0192] If desired, additional additives, such as balancing agents, glycerols or alkyl glycols, or fillers, may be added. However, preferably, the compositions according to the invention do not contain balancing agents and / or fillers.
[0193] Method for preparing the composition of the present invention: According to a third aspect, the present invention relates to a method for preparing a composition comprising a plurality of tablets or of a plurality of tablets, the method comprising the following steps: (i) Providing at least one microcapsule or an aqueous dispersion containing at least one microcapsule; (ii) Melting at least one polymer and optionally at least one adhesive; (iii) Incorporate at least one microcapsule into the polymer melt of step (ii); (iv) Mixing free fragrances or mixtures of free fragrances; (v) Forming an ingot from the mixture of step (iv) by dripping; and (vi) Optional cooling; Optionally, it may also include the step of adding at least one plasticizer and / or at least one structuring agent in or after steps (ii), (iii) and / or (iv).
[0194] In the context of this invention, the components specified above in the context of the first and second aspects are equally applicable to the subject matter of the third aspect, namely the terms “microcapsule,” “polymer,” “free fragrance,” “adhesive,” “plasticizer,” “tablet,” “structuring agent,” etc., and the corresponding amounts and properties as specified above.
[0195] Based on the corresponding adjustment of the required amount, the method as specified in the third aspect herein is applicable to the preparation of compositions according to the first and second aspects of the present invention.
[0196] In the first step (i) of the method according to the invention, microcapsules as specified herein are provided. The microcapsules may be present on their own or alternatively in the form of an aqueous dispersion comprising one or more microcapsules, preferably a plurality of microcapsules.
[0197] Preferably, the microcapsules are dispersed in an aqueous phase. According to the present invention, the microcapsules are dispersed in an aqueous phase, preferably wherein the concentration of microcapsules in the aqueous phase is greater than 5% by weight and less than 70% by weight based on the weight of the dispersion, preferably greater than 20% by weight and less than 60% by weight, and most preferably greater than 30% by weight and less than 50% by weight.
[0198] Further discovery has shown that, advantageously, 30% by weight or less of this aqueous microcapsule slurry is used in the method of the present invention (see [link to invention]). Figure 6 And Example 6), and more preferably 20% by weight or less, and even more preferably 15% by weight or less. When 5% to 10% by weight of such an aqueous microcapsule dispersion (“microcapsule slurry”, preferably in a capsule-to-water ratio of 2:3 by weight of the slurry) is added, desirable results in terms of stability, flexibility and performance are observed.
[0199] Offering microcapsules in the form of a dispersion is advantageous for more uniform distribution of microcapsules within the final tablet formulation. Furthermore, the water contained in the continuous or external phase of the dispersion can serve as a plasticizer, which helps improve the final product characteristics specified above, allows for effective tuning of the viscosity and flexibility of the polymer matrix, resulting in a less brittle and more flexible matrix with improved cushioning and thus better protection for fragile microcapsules, as well as facilitated incorporation into solid consumer product formulations without altering the fundamental chemical properties of the plasticizer.
[0200] Therefore, preferably, in step (i) of the method according to the third aspect of the invention, the microcapsules are provided in the form of an aqueous dispersion.
[0201] In a subsequent step (ii) of the method according to the invention, at least one polymer is melted. According to the method, a binder may be added, which is heated and melted together with the polymer specified herein. Alternatively, the two substances may be melted separately, and the resulting corresponding melts may subsequently be combined and homogenized.
[0202] To achieve uniform distribution of microcapsules within a polymer matrix, polymers as specified herein are more preferably used, and polyethylene glycol is preferred, wherein at least one polymer has a melting point, and polyethylene glycol preferably has a melting point in the range of 25°C to 100°C, and more preferably in the range of 40°C to 80°C.
[0203] Therefore, according to another preferred variant of the invention, the polymers of the first, second and / or third aspects of the invention, preferably having a molecular weight of about 3,000 Da to 20,000 Da, preferably have a melting point in the range of 25°C to 100°C, and more preferably 40°C to 80°C, so as to effectively and uniformly encapsulate the microcapsules in the polymer matrix.
[0204] In a preferred variant of the method according to the invention, in order to achieve uniform distribution of microcapsules in the polymer buffer matrix, the melting step (ii) is correspondingly carried out at a temperature in the range of 25°C to 100°C, preferably 40°C to 80°C, and even more preferably at 80°C.
[0205] In this step, additional additives, such as adhesives, surfactants, plasticizers and / or structuring agents, may be added and mixed to obtain a homogeneous mixture.
[0206] At least one microcapsule or microcapsule dispersion is mixed into the polymer melt of step (ii), and the resulting mixture is homogenized in a further process step (iii) to obtain a uniform distribution of discrete microcapsules in the melt.
[0207] The polymer composition thus prepared is then mixed with free (i.e. unencapsulated) fragrance components (a single fragrance substance or a mixture of two or more fragrance substances) (step (iv)).
[0208] The resulting mixture is homogenized to obtain a uniform distribution of components.
[0209] Finally, in the subsequent step (v), an ingot is formed by dripping the mixture from step (iv) using a prior art ingot-making process known to those skilled in the art.
[0210] Tablet forming is a granulation process in which a droplet former is typically used to create tablets, which are then cooled to obtain discrete granules. Methods for preparing tablets or granules are commercially available, and tablets can be formed into various shapes, including tablets, pills, spheres, etc. Furthermore, scale-up methods using a pulse generator to drop the tablets in air or vegetable oil have also shown promising results.
[0211] Optionally, the obtained granules are cured in an additional cooling step (vi).
[0212] If necessary, at least one plasticizer and / or structuring agent and / or surfactant may be added in or after steps (ii), (iii) and / or (iv).
[0213] Alternatively, in another preferred embodiment of the method according to the invention, the free fragrance component is mixed with a molten polymer, and then microcapsules are added.
[0214] According to this embodiment, the composition is prepared based on the following steps: (i) Providing at least one microcapsule or an aqueous dispersion containing at least one microcapsule; (ii) Melting at least one polymer and optionally at least one adhesive; (iii) Incorporate the free fragrance or a mixture of free fragrances into the polymer melt of step (ii); (iv) Mix at least one microcapsule into the mixture from step (iii). (v) Forming an ingot from the mixture of step (iv) by dripping; and (vi) Optional cooling; Optionally, it may also include the step of adding at least one plasticizer and / or at least one structuring agent in or after steps (ii), (iii) and / or (iv).
[0215] According to an alternative embodiment, the free fragrance component and the microcapsule component are simultaneously added to the melt polymer.
[0216] Surprisingly, the mixing order did not affect the final product properties. This means that the molten polymer, microcapsule components, free fragrance components, and any other (optional) ingredients (if present) can be mixed in any order or simultaneously.
[0217] To achieve uniform distribution of microcapsules within the protective matrix, it is advantageous to use microcapsules with a particle size in the range of 150 μm to 5 mm, preferably in the range of 500 μm to 3 mm.
[0218] Therefore, according to a preferred variant of the invention, the particle size of the microcapsules according to the first, second and / or third aspects of the invention is preferably in the range of 150 μm to 5 mm, and more preferably in the range of 500 μm to 3 mm.
[0219] According to another aspect, the present invention also relates to a composition comprising or consisting of at least one tablet obtained by the method according to the invention, wherein the at least one tablet comprises or consists of the following: (a) At least one microcapsule encapsulating an active ingredient, wherein the at least one microcapsule is preferably dispersed in a polymer matrix, and wherein the active ingredient is preferably a fragrance or a mixture of fragrances; (b) at least one polymer (forming the polymer matrix), wherein the polymer is preferably polyethylene glycol; (c) Optionally at least one adhesive, wherein the adhesive is preferably selected from the group consisting of: fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; and (d) Free fragrance or a mixture of free fragrances, preferably dispersed in the polymer matrix; The composition has a viscosity η of less than 900 mPa·s at 80°C.
[0220] The reduced viscosity allows for more uniform formulation preparation. Simultaneously, the lower viscosity results in better dripping behavior, thus facilitating the formation of more uniform tablets.
[0221] Surprisingly, viscosity was found to be positively affected by both free fragrance components and matrix components such as PEG matrix.
[0222] Furthermore, another aspect of the invention relates to compositions prepared according to the method of the invention.
[0223] consumer goods : In another aspect, the present invention relates to the use of the compositions according to the invention in the preparation of consumer product formulations. The terms "consumer product formulation" and "consumer product" are used synonymously in the context of this invention.
[0224] Therefore, any of the above compositions is suitable for the preparation of consumer product formulations, namely compositions according to the first aspect of the invention, compositions according to the second aspect of the invention, and / or compositions obtained based on the method according to the third aspect of the invention, as well as mixtures thereof.
[0225] Furthermore, consumer products can advantageously contain two or more different compositions according to the invention, differing, for example, in the composition and / or amount of the encapsulated active ingredient / fragrance component, the composition and / or amount of the free fragrance component, and / or the composition of the polymer matrix. This allows for further improvement in olfactory performance and its complexity. Additionally, this approach allows for the combination of different active ingredients that would otherwise be incompatible.
[0226] The particular advantages of the tablet composition of the present invention have been discovered in consideration of the preparation of solid consumer products such as powdered detergents, laundry soaps, solid fabric softeners, deodorizing sticks, etc. Therefore, it is preferable that the consumer product according to the present invention is a solid consumer product.
[0227] When incorporated into consumer product formulations, microcapsules must be chemically stable in a fairly aggressive environment, but also mechanically stable under mechanical stress, such as during mixing and optionally pressing into solid consumer product formulations. However, increased shell thickness typically leads to poorer release properties (release of the active ingredient) due to high capsule breakage caused by shear during processing. Surprisingly, compositions according to the invention, based on a combination of microcapsules embedded in a polymer matrix and a free fragrance dispersed in said matrix, have been found to be particularly suitable for incorporation into solid consumer product formulations. The polymer matrix protects the microcapsules while allowing for high release performance.
[0228] Additional free fragrances dispersed within the polymer matrix further improve processability, homogeneity, and release characteristics. Furthermore, it immediately enhances the consumer's fragrance experience from the outset.
[0229] Therefore, in another preferred variant, the invention also relates to the use of the compositions according to the invention in the preparation of consumer products and formulations thereof, wherein the consumer products or consumer product formulations are solid products, such as textile care products (such as powdered detergents, laundry soaps, solid fabric softeners), solid soaps, household products (such as solid toilet cleaners, solid general-purpose cleaners, powdered carpet cleaners, powdered detergents for washing dishes or cleaning various surfaces), personal care products (such as deodorants, soaps), fragrance enhancers, aroma enhancers, pharmaceutical products, and mixtures thereof.
[0230] Finally, in another aspect, the present invention relates to consumer products or consumer product formulations themselves, which comprise or consist of compositions according to the invention, namely compositions according to the first aspect of the invention, compositions according to the second aspect of the invention, and / or compositions obtained based on the method according to the third aspect of the invention, and mixtures thereof.
[0231] The compositions of this invention allow for the effective incorporation of active ingredients into solid product formulations, thereby enabling the effective and targeted release of said active ingredients. Example
[0232] The invention is described in more detail and specifically below with reference to embodiments, however, it is not intended to limit the invention.
[0233] Example 1: Combination of microcapsules in powder detergents, with and without added free fragrance. Object-Sensory Evaluation .
[0234] According to a first embodiment, a composition comprising at least one tablet containing microcapsules or at least one tablet containing microcapsules is prepared as follows: In a first step, core-shell microcapsules (microcapsule size: 10 μm to 50 μm) comprising a melamine-formaldehyde-based shell material and an aroma agent core are provided. The microcapsules are prepared according to prior art. Subsequently, 78.8 wt% of a polymer mixture comprising PEG-150 and PEG-450 is mixed with 7.5 wt% of rapeseed wax and melted at 80°C. Then, 2.5 wt% of a nonionic surfactant (Imbentin AG / 168S / 500 G) is added, followed by 3.2 wt% of a free aroma agent (free aroma agent mixture 1: a mixture of aldehydes, alcohols, ketones, and hydrocarbons). In a next step, 8 wt% of a microcapsule slurry (the ratio of capsules to water in the slurry is 2:3 by weight of the slurry) is mixed with the resulting polymer melt. Finally, using existing ingot-making processes, a viscous mixture is dripped through a small opening to form multiple ingots with an average particle size of approximately 2 mm, wherein microcapsules are embedded in a polyethylene glycol matrix, followed by cooling to solidify the ingots. The polyethylene glycol portion of the final ingots is approximately 78.8% by weight based on the total weight of each ingot. The amounts of the above components are based on the total weight of the final ingots.
[0235] The following fragrance compositions / mixtures are used as free fragrance components: Free fragrance mixture 1 General-purpose fragrance Mixture of the following substances: Agrumex LC, Citronellol, Decanal, Lauraldehyde, Methylnonacetaldehyde, So-called Tetradecaldehyde, Allyl Hexanoate, Amarose, Ambroxol, Amyl Salicylate, Benzaldehyde, Benzyl Acetate, Benzyl Acetone, Benzyl Salicylate, Borneol / Isobornol 65:35, Porgional, Citronellol 950, Cyanocyanine, CM20 Santal Alkyl ... O-Turkeyone, Decenol, Dihydromyrcenol, Dimethylbenzyl alcohol, Dimethylbenzyl acetate, Diphenyl ether, Dipropylene glycol, Dynasty ketone, Ethyl decanoate, Eucalyptus oil, Eugenol, Sea bast aldehyde, Lily of the valley pyran BM / Lily of the valley pyran, Supergeraniol, Geraniyl acetate 60, Hexyl acetate, Hexyl salicylate, α-Hexylcinnamaldehyde, Isoboronyl acetate, Isooctone, Isodralein 70 70) P-cresol methyl ether, riboflavin, citrate, lily aldehyde, linalool, linalyl acetate, chamomile ester, cucurbitacinol, octyne carboxylic acid methyl ester, osmanthus aldehyde, lily of the valley oil, orange oil, patchouli oil, paeonol, phenylethanol acetate, phenylethanol, methyl phenethyl ether, pine acetaldehyde, high cis-rose oxide, oleinone, styrax acetate, BHT-free tamarin base, terpineol, timothymol, 2-undecenone, methyl decenol, methyl cypressone, ambroxol, ylang-ylang toiletry and fragrance association base.
[0236] Sensory evaluation was performed as follows: Once the composition according to the invention was prepared, the resulting tablets were mixed with and homogenized with a commercially available powder detergent. The final dosage of the microcapsules in 40g of powder detergent was 0.5% by weight (corresponding to 6.25% by weight of tablets in 40g of powder detergent).
[0237] Finally, add the product to the washing machine and wash the fabric (terry cloth) at 30°C.
[0238] After rinsing, air dry the fabric at room temperature.
[0239] A corresponding powdered detergent was used as a reference. Therefore, a comparative tablet containing no free fragrance components was prepared in a similar manner.
[0240] All microcapsules have a particle size ranging from 10 μm to 50 μm.
[0241] The fragrance release is performed in four steps. The first step describes the odor of freshly washed, i.e., damp or slightly damp cloth. The second step describes the odor of untreated dry cloth (“before rubbing”). The third step describes the odor of dry cloth after light rubbing; for this purpose, the cloth is subjected to slight mechanical stress by moving it back and forth between hands several times, causing the capsule to break. The fourth step describes the odor after the dry cloth has been vigorously rubbed and the capsule has broken. The fragrance intensity is evaluated after each step.
[0242] To evaluate sensory performance, eight to nine testers assessed the aroma intensity on a scale of 1 (odorless) to 9 (very strong odor).
[0243] The results of the sensory evaluation are shown in Figure 1 middle.
[0244] Mechanical treatment of textiles causes fragile microcapsules to rupture, thereby releasing the active ingredient (here: the fragrance composition). Surprisingly, samples containing compositions according to the invention (comprising core-shell microcapsules embedded in a polyethylene glycol matrix) exhibited significantly improved performance, indicating effective protection of the fragile microcapsules within the solid product formulation while allowing for efficient release of the active ingredient. The polymer matrix serves as a shock-absorbing layer in the production of consumer products. Samples without such a shock-absorbing layer and those containing only a coating performed poorly because most of the microcapsules were destroyed during the preparation of the consumer product.
[0245] Furthermore, it was surprisingly found that the presence of free aromatic components dispersed within the polymer matrix led to further improved release characteristics. Figure 1"Before" (before rubbing), "after" (after rubbing). Furthermore, a relatively high initial fragrance experience can be achieved before the mechanical rupture of the microcapsules and the release of the encapsulated fragrance. Figure 1 “Wet” means freshly washed textiles. Therefore, the fragrance experience achieved by the composition according to the invention is (i) prolonged and present from the beginning (i.e., immediately after treatment) and (ii) enhanced, thereby achieving a lasting and intense olfactory perception during and after application.
[0246] Example 2: Compositions containing microcapsules with and without added free fragrances—viscosity depends on the free fragrance. The presence of fragrance .
[0247] According to the second embodiment, a composition comprising at least one tablet containing microcapsules or a tablet containing at least one microcapsule was prepared according to Example 1. Subsequently, the tablets were analyzed using a rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
[0248] Similarly, a tablet composition without additional free fragrance components was used as a reference.
[0249] The results of the viscosity analysis are shown in Figure 2 middle.
[0250] The analyzed samples showed a decrease in viscosity with increasing temperature. In conventional emulsions, the addition of oil droplets (e.g., free fragrance oils) is associated with a sharp increase in viscosity and the emergence of shear-thinning flow behavior. Similar behavior is expected for the compositions of the present invention. However, it was surprisingly found that for the compositions according to the invention, samples containing additional free fragrance components dispersed in a polymer matrix exhibited lower viscosity, i.e., increased flowability.
[0251] Surprisingly, the low viscosity allowed for better homogenization of the composition mixture, while also allowing for better dripping, resulting in a more uniform tablet. Furthermore, sensory data showed that the addition of free oil further enhanced the sensory experience from the outset.
[0252] Furthermore, it was surprisingly found that the viscosity decreased reproducibly, independent of the functional groups of the free fragrance component. Therefore, this viscosity reduction effect can be achieved with any fragrance substance / fragrance mixture.
[0253] Example 3: Composition containing microcapsules with additional free aromatics – viscosity depends on free aromatics Types of agents .
[0254] According to another embodiment, a composition comprising at least one tablet containing microcapsules or of at least one tablet containing microcapsules is prepared as follows: In a first step, core-shell microcapsules (microcapsule size: 10 μm to 50 μm) comprising a melamine-formaldehyde-based shell material and a fragrance core are provided. The microcapsules are prepared according to prior art. Subsequently, 78.8 wt% of polymer PEG-150 is mixed with 7.5 wt% of rapeseed wax and melted at a temperature of 80°C. Then, 2.5 wt% of nonionic surfactant (Imbentin AG / 168S / 500 G) is added, followed by 3.2 wt% of free fragrance and 8 wt% of capsule slurry (capsule to water ratio of 2:3).
[0255] The following fragrance compositions / mixtures are used as free fragrance components: Free fragrance mixture 1 General-purpose fragrance Mixture of the following substances: Agrumex LC, Citronellol, Decanal, Lauraldehyde, Methylnonacetaldehyde, So-called Tetradecaldehyde, Allyl Hexanoate, Amarose, Ambroxol, Amyl Salicylate, Benzaldehyde, Benzyl Acetate, Benzyl Acetone, Benzyl Salicylate, Borneol / Isobornol 65:35, Porgional, Citronellol 950, Cyanocyanine, CM20 Santal Alkyl ... O-Turkeyone, Decenol, Dihydromyrcenol, Dimethylbenzyl alcohol, Dimethylbenzyl acetate, Diphenyl ether, Dipropylene glycol, Dynasty ketone, Ethyl decanoate, Eucalyptus oil, Eugenol, Sea bast aldehyde, Lily of the valley pyran BM / Lily of the valley pyran, Supergeraniol, Geraniyl acetate 60, Hexyl acetate, Hexyl salicylate, α-Hexylcinnamaldehyde, Isoboronyl acetate, Isooctone, Isodralein 70 70) P-cresol methyl ether, riboflavin, citrate, lily aldehyde, linalool, linalyl acetate, chamomile ester, cucurbitacinol, octyne carboxylic acid methyl ester, osmanthus aldehyde, lily of the valley oil, orange oil, patchouli oil, paeonol, phenylethanol acetate, phenylethanol, methyl phenethyl ether, pine acetaldehyde, high cis-rose oxide, oleinone, styrax acetate, BHT-free tamarin base, terpineol, timothymol, 2-undecenone, methyl decenol, methyl cypressone, ambroxol, ylang-ylang toiletry and fragrance association base.
[0256] Free fragrance mixture 2 Hydrocarbon mixture A mixture of the following substances: natural δ-carene, natural refined caryophyllene, natural L-α-pinene, and γ-terpinene.
[0257] Free fragrance mixture 3 : Hydrocarbon mixture (= Free aromatics mixture 2) + ester, wherein the ester component is benzyl butyrate.
[0258] Free fragrance mixture 4 : Hydrocarbon mixture (= Free aromatics mixture 2) + aldehyde, wherein the aldehyde component is decanal.
[0259] Subsequently, the tablets were analyzed using a rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
[0260] Similarly, a tablet composition without additional free fragrance components was used as a reference.
[0261] The results of the viscosity analysis are shown in Figure 3 middle.
[0262] The analyzed samples showed that viscosity decreased with increasing temperature. Furthermore, hydrocarbon compounds were found to have a stronger effect on viscosity. Further reduction in viscosity depended on additional fragrance additives, such as esters and aldehydes. This leads to the conclusion that viscosity can be affected by the choice of fragrance components, i.e., fragrance emulsifiers. This allows for more homogeneous samples, resulting in more uniform particle sizes.
[0263] Example 4: Composition containing microcapsules with additional free fragrance – viscosity depends on polymer base molecular weight of matter .
[0264] According to the fourth embodiment, a composition comprising at least one tablet containing microcapsules or at least one tablet containing microcapsules is prepared as follows: In a first step, core-shell microcapsules (microcapsule size: 10 μm to 50 μm) comprising a melamine-formaldehyde-based shell material and an aroma agent core are provided. The microcapsules are prepared according to the prior art. Subsequently, 78.8 wt% of polymer PEG is mixed with 7.5 wt% of rapeseed wax and melted at a temperature of 80°C. Then, 2.5 wt% of nonionic surfactant (Imbentin AG / 168S / 500 G) is added, followed by 3.2 wt% of free aroma agent and 8 wt% of capsule slurry (capsule to water ratio of 2:3) (free aroma agent mixture 1).
[0265] The PEG composition is modified by using polymers with different molecular weights. The following PEG compounds are used: PEG 10,000 g / mol PEG 8,000 g / mol PEG 6,000 g / mol Subsequently, the tablets were analyzed using a rheometer (HAAKE Rheometer RS 1 (RheoStress)) and the viscosity was tested at different temperatures.
[0266] Similarly, lozenge compositions without additional free fragrance components were used as references in combination with different polymer components.
[0267] The results of the viscosity analysis are shown in Figure 4 middle.
[0268] The analyzed samples demonstrate the beneficial effects of the presence of free fragrance components (i.e., fragrance emulsifiers). Additionally, it was surprisingly found that lower molecular weight PEG resulted in lower viscosity. Mixtures of different PEGs resulted in lower viscosity, meaning that both mixtures with free fragrance oils and the pure addition of PEG contribute to viscosity reduction and the benefits specified above. However, the additional addition of free fragrance has a surprising dual benefit: improved odor and reduced viscosity.
[0269] Typically, PEG with a molecular weight higher than 3,000 g / mol is a solid with a fairly similar melting point range. However, it was surprisingly found that molecular weight has a considerable influence on the melting behavior and viscosity of the resulting compositions.
[0270] The results showed that the combination of microcapsules embedded in a polymer-binder-matrix with a specific amount of free fragrance components resulted in even better performance of consumer products.
[0271] Example 5: Compositions containing microcapsules with additional free fragrances for different adhesives – Sensitive Official evaluation .
[0272] According to the fifth embodiment, different compositions comprising at least one lozenge containing microcapsules or at least one lozenge containing microcapsules are prepared. The different samples containing the binder are prepared as follows: In a first step, core-shell microcapsules (microcapsule size: 10 μm to 50 μm) containing a melamine-formaldehyde-based shell material and a fragrance core are provided. The microcapsules are prepared according to prior art. Subsequently, 78.8% by weight of a polymer mixture containing PEG-150 and PEG-450 is mixed with 7.5% by weight of the binder (see [link to previous embodiment]). Figure 5 The mixture was then melted at 80°C. Next, 2.5 wt% of a nonionic surfactant (Imbentin AG / 168S / 500 G) was added, followed by 3.2 wt% of a free aromatic agent (free aromatic agent mixture 1: a mixture of aldehydes, alcohols, ketones, and hydrocarbons). In the next step, 8.0 wt% of a microcapsule slurry (with a capsule-to-water ratio of 2:3 by weight of the slurry) was mixed with the resulting polymer melt. Finally, using a conventional ingot-making process, the viscous mixture was dripped through a small opening to form multiple ingots with an average particle size of approximately 2 mm, wherein the microcapsules were embedded in a polyethylene glycol matrix, followed by cooling to solidify the ingots. The polyethylene glycol portion of the final ingots was approximately 78.8 wt% based on the total weight of each ingot. The amounts of the above components are based on the total weight of the final ingots.
[0273] In all samples of the aforementioned samples, the ratio of PEG to adhesive was approximately 10:1.
[0274] Additionally, as a reference, a comparative tablet (“capsules in PEG” – without any binder) was prepared in a similar manner. The tablet was prepared as follows: In a first step, core-shell microcapsules (microcapsule size: 10 μm to 50 μm) comprising a melamine-formaldehyde-based shell material and an aroma agent core were provided. The microcapsules were prepared according to existing techniques. Subsequently, 86.3 wt% of a polymer mixture containing PEG-150 and PEG-450 was melted at 80 °C. Then, 2.5 wt% of a nonionic surfactant (Imbentin AG / 168S / 500 G) was added, followed by 3.2 wt% of a free aroma agent (free aroma agent mixture 1: a mixture of aldehydes, alcohols, ketones, and hydrocarbons). In the next step, 8.0 wt% of a microcapsule slurry (the ratio of capsules to water in the slurry was 2:3 by weight of the slurry) was mixed with the resulting polymer melt. Finally, using a conventional ingot-making process, a viscous mixture is dripped through a small opening to form multiple ingots with an average particle size of approximately 2 mm, wherein microcapsules are embedded in a polyethylene glycol matrix, followed by cooling to solidify the ingots. The polyethylene glycol portion of the final ingots is approximately 86.3% by weight based on the total weight of each ingot. The amounts of the above components are based on the total weight of the final ingots.
[0275] To evaluate sensory performance, 8 to 9 testers assessed the aroma intensity on a scale of 1 (odorless) to 9 (very strong odor) according to the method in Example 1.
[0276] The results of the sensory evaluation are shown in Figure 5 To evaluate sensory performance, the particles were incorporated into a standard powdered detergent and then dissolved in water. A terry cloth was then washed in the resulting solution. After air-drying at room temperature, sensory evaluation was performed according to the method of Example 1.
[0277] A comparison of samples with and without an additional binder showed that the addition of a binder not only improved the manufacture and preparation of more uniform tablets, but also led to an improved sensory experience by allowing for more effective protection of fragile microcapsules and thus more targeted release of fragrances. It was further found that different types of waxes can be appropriately used as binders.
[0278] In addition, both animal waxes and plant waxes have been found to be suitable as binders for the compositions used in this invention.
[0279] Example 6: Composition containing microcapsules with an additional free fragrance according to the invention – microcapsules Effect of slurry content .
[0280] According to the sixth embodiment, a composition comprising at least one tablet containing microcapsules or of at least one tablet containing microcapsules was prepared according to Example 1. Therefore, the tablets are based on PEG, rapeseed wax, and microcapsule slurry (the ratio of capsules to water in the slurry is 2:3 by weight of the slurry). However, the amount of capsule slurry used in the preparation of the corresponding tablet compositions varies.
[0281] The composition of a single sample is shown in Table 1.
[0282] Table 1: Composition of five different samples .
[0283] *The ratio of capsules to water in the slurry is 2:3 by weight. Figure 6 Photographs of these different samples with varying amounts of microcapsule slurry used in the composition are shown, thus illustrating the effect of microcapsule slurry content on the final tablet formulation.
[0284] The amount of microcapsule slurry used in the preparation varied as follows: 8% by weight of microcapsule slurry (the ratio of capsules to water in the slurry was 2:3 by weight) was used to prepare the first sample. Figure 6 (Left). This amount is considered ideal in terms of flexibility, protective properties, and performance (i.e., release properties). Additional samples were prepared using microcapsule slurries of 15%, 20%, 30%, and 40%, respectively. Figure 6 (From left to right in the middle).
[0285] It has been found that increasing the slurry content in the method according to the invention leads to increased viscosity of the tablets, resulting in 30% or more of a less homogeneous but stable product. Optimal results are found when the amount of slurry is in the range of 0.5% to 10% by weight based on the total tablet composition. This corresponds to a corresponding pure microcapsule content in the same range of 0.5% to 10% by weight, and preferably 3% to 8% by weight, based on the total weight of the tablets.
[0286] Example 7: Compositions with added free fragrances – Effect of plasticizer / water content .
[0287] According to the seventh embodiment, a composition comprising at least one tablet or consisting of at least one tablet was prepared, similar to that in Example 1. The tablets were based on PEG, rapeseed wax, and water. However, the tablets did not contain microcapsules to demonstrate the effect of the water content itself. However, the amount of plasticizer / water used in the preparation of the corresponding tablet compositions varied between 0% by weight and 30% by weight (see [link to relevant documentation]). Figure 7 (From left to right). No plasticizer was used in the first sample (0%, left). The composition of a single sample is shown in Table 2.
[0288] Table 2: Composition of five different samples .
[0289] Figure 7 Photographs of these different samples of the composition are shown, varying with the amount of water used as plasticizer, thus illustrating the effect of water content / plasticizer content.
[0290] It has been found that increasing the content of capsule slurry in the method according to the invention leads to an increase in viscosity for tablets with 10% or more water content, resulting in a less uniform and stable product with 30% or more of the content.
[0291] therefore, Figure 7 This indicates that, in addition to its plasticizing properties, the very high water content leads to increased viscosity.
[0292] In addition, it was found that stickiness led to an increase in residues (e.g., wax residues) on textiles treated with the corresponding laundry detergent.
[0293] Example 8: Compositions with added free fragrances – Effect of plasticizer / water content .
[0294] According to the eighth embodiment, a composition comprising at least one tablet containing microcapsules or a tablet containing at least one microcapsule is prepared according to the present invention.
[0295] The composition of individual samples is shown in Table 3.
[0296] Table 3: Composition of five different samples with increased plasticizer / water content .
[0297] *The ratio of capsules to water in the slurry is 2:3 by weight. The results of ingot production are shown in Figure 8 middle. Figure 8 This indicates that the increased amount of plasticizer component / water content does not allow for the preparation of suitable tablets. One effect not observed in Sample 1 is that water is used as a "plasticizer," therefore the small amount used as in Samples 2 through 4 is ideal. On the other hand, in Sample 5, our water content resulted in small pellet volumes and, simultaneously, very sticky after evaluation by the expert panel.
[0298] Optimal results are achieved when the plasticizer content is in the range of 0.5% to 10% by weight based on the total weight of the tablets. A small amount of plasticizer is sufficient to provide adequate flexibility to the tablets. This ensures their stability when mixed with other components of the final formulation, such as other detergent components, without breaking apart. However, excessive amounts of plasticizer do not produce tablets and exhibit a high degree of stickiness. This stickiness is detrimental when the tablets according to the invention are mixed with other components of the final formulation, such as other detergent components, and may cause individual components to stick together, thereby reducing the stability of, for example, detergent powder.
[0299] Furthermore, the embodiments show that, in order to provide the ideal tablets according to the invention, a polymer content between 60% and 80% by weight is required.
[0300] Example 9: Laundry Soap Furthermore, the laundry soap is prepared by directly incorporating fragrance microcapsules (0.1 wt% of the final product) and free (unencapsulated) fragrance (0.7 wt% of the product) into a commercially available soap blank during the extrusion process. The resulting laundry soap is shown in... Figure 9 Therefore, Figure 9 This demonstrates the direct incorporation of microcapsules without using the protective system of the present invention.
[0301] Furthermore, compositions according to the present invention were prepared based on the following formulation: 72% PEG-150, 7.5% rapeseed wax, 2.5% Imbentin, 8% capsule slurry (fragrance capsules to water in a 2:3 ratio), and 10% free (unencapsulated) fragrance. The resulting product is shown in... Figure 10 Therefore, Figure 10 Microcapsules and free aromatic oils incorporated into a protective polymer matrix are shown.
[0302] It has been found that the compositions / tablets of the present invention can be effectively incorporated into solid consumer products such as laundry soap.
[0303] Laundry soap - sensory evaluation To evaluate the sensory properties of the laundry soap prepared according to the present invention and according to Example 9, eight to nine testers assessed the fragrance intensity on a scale of 1 (odorless) to 9 (very strong odor).
[0304] The results of the sensory evaluation are shown in Figure 11 The sensory evaluation was conducted in the same manner as described in Example 1.
[0305] The soap base is incorporating the tablets (72% PEG-150, 7.5% rapeseed wax, 2.5% Imbentin, 8% capsule slurry (capsule to water ratio of 2:3) and 10% free (unencapsulated) fragrance) as described above into the soap base to obtain laundry soap.
[0306] Subsequently, the release characteristics of the obtained laundry soap were tested and compared with those of laundry soap directly incorporating fragrance components.
[0307] The results confirmed that direct incorporation of the component into the product did not exhibit the desired release characteristics, indicating insufficient homogeneity, stability, and incorporation of the key component. During the manufacturing process of the final consumer product (i.e., laundry soap), the unprotected, fragile microcapsules were crushed and destroyed.
[0308] On the other hand, by incorporating free fragrance oils and encapsulated fragrance components into a protective polymer matrix via the tablets according to the invention, effective protection of fragile microcapsules is achieved during the manufacturing process, while allowing for the effective and targeted release of the active ingredient, i.e., the encapsulated fragrance. This is due to... Figure 11 The effective release characteristics shown reflect this.
[0309] Further findings indicate that the addition of binders, as specified herein, is crucial for the formulation of such solid consumer products, particularly extruded products such as laundry soap, in order to ensure effective incorporation of active ingredients and to provide suitable consistency and effective release of active ingredients encapsulated in microcapsules.
[0310] Based on these results, it can be concluded that microcapsules and free oils can only be efficiently incorporated into laundry soaps (or similar solid consumer products) when these components are provided in tablet form according to the present invention. Furthermore, it has been found that additional binders, as specified herein, are beneficial or even necessary for achieving effective, uniform, and stable incorporation of the aforementioned components. This allows for the preparation of products with high efficiency and long-term stability.
Claims
1. A composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of the following: (a) 0.5% to 10% by weight of at least one microcapsule encapsulating the active ingredient. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) 92% to 98% by weight of a polymer, preferably polyethylene glycol; and (c) 0.1% to 10% by weight of free fragrance or mixtures of free fragrance; The above items are based on the total weight of the tablets.
2. The composition according to claim 1, wherein the at least one tablet further comprises or consists of the following: (d) at least one plasticizer, based on the total weight of the tablets, at a rate of 0.5% to 10% by weight. The plasticizer is preferably water or polyethylene glycol.
3. A composition comprising or consisting of at least one tablet, wherein the tablet comprises or consists of the following: (a) 0.5% to 10% by weight of at least one microcapsule encapsulating the active ingredient. The active ingredient is preferably a fragrance or a mixture of fragrances; (b) 60% to 80% by weight of at least one polymer, preferably polyethylene glycol; (c) at least one adhesive, ranging from 2% to 32% by weight. The adhesive is preferably selected from the group consisting of fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; The above items are based on the total weight of the tablets; and (d) 0.1% to 10% by weight of free fragrance or mixtures of free fragrance; The above items are based on the total weight of the tablets.
4. The composition according to claim 3, wherein the at least one tablet further comprises or consists of the following: (e) 0.5% to 10% by weight of at least one plasticizer, The plasticizer is preferably water or polyethylene glycol; and / or (f) 0.1% to 10% by weight of a structuring agent, The structuring agent is preferably selected from the group consisting of esters, such as isopropyl myristate or other emulsifiers; The above items are based on the total weight of the tablets.
5. The composition according to any one of the preceding claims, wherein the at least one polymer is water-soluble and / or the composition does not contain any inorganic or organic salts.
6. The composition according to any one of the preceding claims, wherein the at least one polymer, and preferably polyethylene glycol, has a molecular weight of about 3,000 Da to 20,000 Da.
7. The composition according to any one of the preceding claims, wherein the shell of the at least one microcapsule comprises or is composed of a shell material selected from the group consisting of: sol-gel polymers, polyacrylates, polyacrylamide, poly(acrylate-co-acrylamide), polyurea, polyurethane, peptides, polysaccharides, polyphenol polymers, poly(melamine-formaldehyde), poly(resorcinol-formaldehyde), poly(urea-formaldehyde), or combinations thereof.
8. The composition according to any one of the preceding claims, wherein the at least one adhesive is selected from the group consisting of animal waxes and / or plant waxes, preferably beeswax.
9. A method for preparing a composition comprising a plurality of tablets or of a plurality of tablets, the method comprising the following steps: (i) Providing at least one microcapsule or an aqueous dispersion containing at least one microcapsule; (ii) Melting at least one polymer and optionally an adhesive; (iii) Mixing the at least one microcapsule into the polymer melt of step (ii); (iv) Mixing free fragrances or mixtures of free fragrances; (v) Forming a tablet by dripping the mixture from step (iv); as well as (vi) Optional cooling; Optionally, it may also include the step of adding at least one plasticizer and / or at least one structuring agent in or after steps (ii), (iii) and / or (iv).
10. The method for preparing a composition according to the preceding claims, wherein the melting point of the at least one polymer, preferably polyethylene glycol, is in the range of 25°C to 100°C, preferably 40°C to 80°C.
11. The method for preparing a composition according to any one of claims 9 or 10, wherein the melting step (ii) is carried out at a temperature in the range of 25°C to 100°C, preferably 40°C to 80°C, and even more preferably at 80°C, and / or wherein the particle size of the microcapsules is in the range of 150 μm to 5 mm, and / or wherein the microcapsules are provided in the form of an aqueous dispersion.
12. A composition comprising or consisting of the following: At least one tablet obtained by the method according to any one of claims 9 to 11, wherein the tablet comprises or is composed of the following: (a) At least one microcapsule encapsulating an active ingredient, The active ingredient is preferably a fragrance or a mixture of fragrances; (b) at least one polymer, preferably polyethylene glycol; (c) Optionally at least one adhesive, The adhesive is preferably selected from the group consisting of: fatty acids, fatty alcohols, fatty acid esters, or mixtures thereof, such as waxes; and (d) Free aromatics or mixtures of free aromatics; The composition described herein has a viscosity η of less than 900 mPa·s at 80°C.
13. Use of the composition according to any one of claims 1 to 8 or 12 in the preparation of a consumer product formulation.
14. Use of the composition according to claim 13, wherein the consumer product formulation is a solid product, such as textile care products, household products, personal care products, cosmetic products, pharmaceutical products, and mixtures thereof.
15. A consumer product formulation, wherein the consumer product formulation comprises or consists of the following: The composition according to any one of claims 1 to 8 or 12.