Powder comprising crystals having inclusions encapsulated therein
阅读说明：本技术 包含了其中封有内含物的晶体的粉末 (Powder comprising crystals having inclusions encapsulated therein ) 是由 科利亚·贝伦斯 帕特里克·奥特 尼古拉斯·皮雄 纳丁·施米特迈尔 约恩·维德曼 于 2017-06-07 设计创作，主要内容包括：本发明主要涉及一种用于制造粉末的方法,所述粉末包含大量包封在晶体中的胶囊,其中所述胶囊包含一种或多种内含物。此外,本发明涉及一种相应的粉末以及一种包含所述粉末的产品,一种粉末的应用以及一种用于制造相应的产品的方法和一种用于对底物添加香气的方法。(The present invention generally relates to a method for manufacturing a powder comprising a plurality of capsules encapsulated in crystals, wherein the capsules comprise one or more inclusions. Furthermore, the invention relates to a corresponding powder and a product comprising said powder, to the use of a powder and to a method for producing a corresponding product and to a method for adding an aroma to a substrate.)
1. A method for manufacturing a powder consisting of or comprising a multitude of capsules encapsulated in crystals, said capsules comprising one or more inclusions, said method consisting of or comprising the steps of:
(i) providing one or more solvents for the one or more solvents,
providing one or more crystallizable materials, and
providing one or more capsules (K) containing one or more contents,
(ii) optionally, increasing the temperature of the solvent/solvents,
(iii) will be provided with
(iii.1) one or more of the provided crystallizable materials, and
(iii.2) optionally, adding the provided capsules (K) to the solvent/solvents before, after or simultaneously with the crystallizable material/s and dissolving the crystallizable material/s provided in the solvent/s in order to obtain a mixture (M1),
(iv) reducing the temperature of the mixture (M1) to a temperature below the crystallization temperature of the provided crystallizable material/materials or up to the crystallization temperature,
(v) (iv) adding the provided capsule (K) or further capsules (K), wherein step (v) is optional in case step (iii.2) is performed,
(vi) further reducing the temperature of said mixture (M1) so as to obtain a mixture (M2) comprising a plurality of capsules (K) encapsulated in crystals and containing one or more inclusions,
(vii) collecting the capsules (K) comprising the crystals, the capsules containing one or more inclusions.
2. The method of claim 1, wherein the first and second light sources are selected from the group consisting of,
wherein the/one, more or all solvents are selected from: water and water-miscible solvents, preferably ethanol, isopropanol, acetone, DMSO.
3. The method according to claim 1 or 2,
wherein the/one, more or all crystallizable materials are capable of crystallizing in a solvent miscible with or with water and/or are selected from: salts, preferably alkali metal and alkaline earth metal salts, particularly preferably sodium sulfate, sodium chloride or sodium carbonate, sugars and urea.
4. The method according to any one of the preceding claims,
wherein a plurality or all of the capsules (K) comprise one or more of the following: flavoring agents, cosmetic inclusions, pharmaceutically effective substances, insect repellents, inclusions for oral and dental care agents, latent heat storage agents and adsorbents.
5. The method according to any one of the preceding claims,
wherein a plurality or all of the capsules (K) have a wall material consisting of one or more substances selected from the group consisting of: natural, semisynthetic and fully synthetic casing materials, preferably composed of melamine-formaldehyde resins, gelatin, alginates, polyurethanes, polyamides and polyureas, or comprising or based on one or more of these substances.
6. The method according to any one of the preceding claims,
wherein in step (ii) the solvent/solvents, if present, are raised to a temperature in the range of 23 ℃ to 50 ℃, preferably in the range of 25 ℃ to 40 ℃, particularly preferably in the range of 30 ℃ to 35 ℃.
7. The method according to any one of the preceding claims,
wherein step (iii) comprises: stirring in order to dissolve the crystallizable material/materials in the solvent/solvents or to simplify the process, preferably at a stirring speed in the range from 100U/Min to 1871U/Min, preferably in the range from 500U/Min to 1300U/Min, particularly preferably in the range from 1000U/Min to 1200U/Min, preferably by means of a guided jet stirrer.
8. The method according to any one of the preceding claims,
wherein in step (vi) the temperature of the mixture (M1) is reduced to a temperature of <20 ℃, preferably <15 ℃, more preferably <10 ℃, especially preferably <5 ℃, wherein the reduction in temperature is preferably carried out over a time period of 0.25 to 3 hours, preferably of 0.5 to 2 hours, especially preferably of 0.75 to 1.5 hours.
9. The method according to any one of the preceding claims,
wherein step (vii) comprises or consists of one, two or all of the following steps:
-pouring the solvent/solvents,
-isolating the crystals,
-drying the mixture (M2) obtained in step (vi) and/or the filtered crystals,
in order to obtain a powder consisting of or comprising a plurality of capsules (K) comprising one or more inclusions, encapsulated in the crystals.
10. The method according to any one of the preceding claims,
wherein the weight ratio of the total amount of solvent(s) to the total amount of crystallizable material(s), to the total amount of capsules (K) and/or capsule dispersions, provided and added in this form, is in the following ranges: 1-10:0.5-5:0.1-3, preferably in the following ranges: 3-7:1-3:0.5-2.
11. Powder consisting of or comprising a multitude of capsules encapsulated in crystals, said capsules having one or more inclusions, preferably being manufactured by or being manufactured by a method according to one or more of the preceding claims.
12. A product selected from the group consisting of: detergent and cleaning agent, body care product, preparation for nutrition or diet, cosmetic or pharmaceutical preparation, perfumed, for or to be perfumed product, preferably perfumed rinse, wherein the product comprises a powder according to claim 11.
13. Use of a powder according to claim 11, wherein a plurality or all of the capsules (K) comprise one or more inclusions selected from the group consisting of: cooling agents, flavor enhancers and flavoring agents, preferably in amounts sufficient to cause a cooling effect and/or to impart, modify or enhance a sensory impression, preferably an odor and/or a taste impression, for imparting, modifying or enhancing a sensory impression, preferably an odor and/or a taste impression, or for adding a flavor to a product, preferably to a product according to claim 12.
14. A method for manufacturing a product according to claim 12, comprising or consisting of the steps of:
(a) provide for
(a.1) the powder according to claim 11, and
(a.2) one or more other components, and
(b) mixing the components (a.1) and (a.2).
15. A method for perfuming a substrate, preferably hair, skin, leather or textile fibres, comprising or consisting of the steps of:
(a) providing a powder according to claim 11 or a product according to claim 12, wherein a plurality or all of the capsules (K) comprise one or more inclusions selected from the group consisting of: odorants and flavourings, preferably in an amount sufficient to impart, modify or enhance a sensory impression, preferably an odor and/or taste impression, and
(b) the powder or product is applied to the substrate(s) to be perfumed, preferably hair or skin or fibres or leather, preferably in an organoleptically effective amount, preferably in an amount sufficient for the consumer to perceive one or more odors or tastes, with respect to the capsules (K) contained therein.
Technical Field
The invention relates generally to a method for producing a powder consisting of or comprising a plurality of capsules containing one or more inclusions, which are enclosed in crystals.
The invention furthermore relates to a powder consisting of or comprising a plurality of capsules comprising one or more inclusions encapsulated in crystals, to products comprising such a powder, to the use of such a powder, preferably in such products, and to a process for manufacturing such a product and to a process for adding an aroma to a substrate.
Further aspects and preferred embodiments of the invention emerge from the following embodiments, the appended examples and in particular the appended claims.
Background
The addition of capsules, for example containing perfume oil, to laundry powder can be carried out, for example, by spraying the capsules onto the already prepared laundry powder. However, in this case the capsules are unprotected and the probability of a part of the capsule being broken up during further manufacturing processes (e.g. mixing and conveying the powder) due to shear forces occurring in the laundry powder is very high. As long as the capsules do not adhere sufficiently to the laundry powder particles, a separation of the capsules in the powder may also occur. Thus, the distribution of the capsules in the laundry powder is no longer uniform. Another method for incorporating capsules into laundry powder consists in spray drying the capsules together with the other components of the laundry powder. However, in this case, the capsule is significantly subjected to thermal loads. Due to this thermal load, the following risks arise: changing the quality of the capsules used or even destroying said capsules.
Disclosure of Invention
The main object of the present invention is now to provide a method for producing powders in which the above-mentioned disadvantages do not occur or occur only to a very much reduced extent. Other aspects of the object and other tasks will be derived from the following embodiments.
According to the invention, the object set forth above is achieved by a method for producing a powder consisting of or comprising a plurality of capsules (K) containing one or more inclusions, enclosed in crystals, consisting of or comprising the following steps:
(i) providing one or more solvents for the one or more solvents,
providing one or more crystallizable materials, and
providing one or more capsules (K) containing one or more contents,
(ii) optionally, the temperature of the solvent/solvents is increased,
(iii) will be provided with
(iii.1) the crystallizable material/materials provided, and
(iii.2) optionally, before, after or simultaneously with the crystallizable material/materials, providing a capsule (K)
Adding to the solvent/solvents and dissolving the provided crystallizable material/materials in the solvent/solvents, so as to obtain a mixture (M1),
(iv) reducing the temperature of the mixture (M1) to a temperature below or until crystallization of the provided crystallizable material/materials,
(v) (iv) adding the provided capsule (K) or further capsules (K), wherein step (v) is optional in case step (iii.2) is performed,
(vi) further reducing the temperature of the mixture (M1) so as to obtain a mixture (M2) comprising a plurality of capsules (K) comprising one or more inclusions, encapsulated in crystals,
(vii) collecting the capsule (K) comprising one or more inclusions encapsulated in the crystals.
The capsules (K) are at least partially encapsulated in and/or by the crystals formed during the crystallization process (see fig. 1).
Preferably, the crystallizable material/materials are present in the solvent/solvents in a concentration that allows crystallization to begin at a temperature above the freezing point of the solvent/solvents.
The capsules (K) provided in step (i) containing one or more inclusions can be present as a powder in a dispersion or in another form.
The onset of crystallization is understood as the point in time at which the first crystals are visible when the mixture M1 is observed with the naked eye.
Preferably, in the method according to the invention, step (v) is carried out immediately after step (iv).
The crystals produced according to the invention or the powder produced according to the invention can advantageously be mixed without problems with the already produced laundry powder formulation or the usual constituents of laundry powders. In this case, the contained or encapsulated capsules are better protected against mechanical loads when added to laundry powder than capsules added loosely to laundry powder.
If necessary, the particle size of the crystals produced according to the invention can be adapted to the particle size of the washing powder by setting corresponding parameters (e.g. temperature or temperature profile during the process and process duration) such that segregation phenomena during the preparation of the washing powder are avoided.
In addition, strong thermal stresses, such as occur, for example, in spray drying, are avoided.
Due to the fact that the products produced according to the invention are powders, the costs necessary for transport and packaging are considerably reduced compared to, for example, liquid capsule dispersions.
The capsules (K) provided in step (i) and containing one or more inclusions can, for example, contain one or more odorous substances:
the odorants preferably used according to the invention include, for example, essential oils, which consist, for example, of the following raw materials:
extracts from natural sources, such as ethereal oils, extract oils, absolute oils (absolutes), resins, lipids, balsam resins, tinctures, for example ambergris; sandalwood oil; angelica seed oil; angelica root oil; anise oil; valerian oil; basil oil; sphagnum absolute (Baummoos-absolute); laurel oil; mugwort oil; benzoin resin; citrus oil; beeswax absolute; birch tar oil; bitter almond oil; savory oil; oil of Bukuye leaf; carrousel oil; juniper oil; calamus oil; camphor oil; adding oil to the Kanan; cardamom oil; kailu oil; cassia seed oil; absolute oil of acacia; castor oil; cedar leaf oil; cedar wood oil; cistus oil; citronella oil; lemon oil; bitter is added to the balsam of the fenugreek; balsam of herba Trifolii Pratentis; coriander oil; oleum radix aucklandiae; cumin oil; cedar wood oil; artemisia annua oil; dill herb oil; dill seed oil; eau de brouts neat oil; cleaning oak moss oil; elemi oil; tarragon oil; lemon eucalyptus oil; eucalyptus oil; fennel oil; spruce seed oil; glasswort oil; a glassine resin; geranium oil; grapefruit oil; guaiac oil; gule-rue-fat; oil of crura oil; purifying the helichrysum oil; helichrysum oil; ginger oil; iris tectorum oil; orris oil; jasmine absolute oil; calamus oil; essential oil of blue chamomile; roman chamomile essential oil; carrot seed oil; balsam of bitter wood; pine needle oil; spearmint oil; caraway oil; labdanum oil; labdanum essential oil; a Liberbant resin; mixed lavender absolute oil; mixed lavender oil; lavender absolute oil; lavender oil; citronella oil; angelica oil; distilling lime oil; squeezing lemon oil; flail wood oil; litsea cubeba oil; laurel leaf oil; nutmeg oil; marjoram oil; orange oil; sweet osmanthus oil; acacia virgata absolute; abelmoschus esculentus oil; musk tincture; red sage oil; nutmeg oil; purifying Myrrha with oil; myrrh oil; cherokee rose fruit oil; clove leaf oil; clove oil; neroli oil; purifying Olibanum oil; mastic oil; hongyun medicinal oil; neroli absolute; orange oil; oregano oil; palmarosa oil; patchouli oil; perilla oil; mulu fragrant oil; parsley leaf oil; parsley seed oil; orange leaf oil; peppermint oil; pepper oil; all-grass of common people's sesame oil; pine oil; peppermint oil; rose absolute oil; rosewood oil; rose oil; rosemary oil; grasswort maria tail oil; spanish sage oil; sandalwood oil; celery seed oil; lavender oil; anise oil; storax oil; marigold oil; pine needle oil; tea tree oil; turpentine oil; thyme oil; tulu balsam; black bean absolute; tuberose absolute oil; soaking vanilla in liquid; violet leaf absolute oil; verbena oil; vetiver oil; juniper oil; brewing oil yeast oil; wormwood oil; wintergreen oil; cananga oil; hyssop oil; civet absolute oil; cinnamon leaf oil; cinnamon bark oil, and fractions thereof, or contents isolated therefrom;
-a single fragrance selected from: hydrocarbons, such as 3-carene; alpha-pinene; beta-pinene; alpha-terpine; gamma-terpine; p-isopropylbenzene Jiakang; red myrrh terpene; camphene; caryophyllene; cedrene; farnesene; limonene; longifolene; myrcene; ocimene; marrubiin hemiterpene (Valencen); (E, Z) -1,3, 5-undecatriene; styrene; diphenylmethane;
aliphatic aldehydes and acetals thereof, such as hexanal; heptanal; octanal; nonanal; decanal; undecalaldehyde; dodecanal; tridecanal; 2-methyl octanal; 2-methylnonanal; (E) -2-hexenal; (Z) -4-heptenal; 2, 6-dimethyl-5-heptenal; 10-undecenal; (E) -4-decenal; 2-dodecenal; 2,6, 10-trimethyl-9-undecenal; 2,6, 10-trimethyl-5, 9-undecadinaldehyde; heptanal diethyl acetal; 1, 1-dimethoxy-2, 2, 5-trimethyl-4-hexene; citronellyl oxyacetaldehyde; 1- (1-methoxy-propoxy) - (E/Z) -3-hexene;
aliphatic ketones and oximes thereof, such as 2-heptanone; 2-octanone; 3-octanone; 2-nonanone; 5-methyl-3-heptanone; 5-methyl-3-heptanone oxime; 2,4,4, 7-tetramethyl-6-octen-3-one; 6-methyl-5-hepten-2-one;
aliphatic sulfur-containing compounds, such as 3-methylthiohexanol; 3-methylthiohexyl acetic acid; 3-mercaptohexanol; 3-mercaptohexyl acetate; 3-mercaptohexyl butyrate; 3-acetylthiohexyl acetate; 1- □ en-8-thiol;
aliphatic nitriles, such as 2-nonenenitrile; 2-undecenenitrile; 2-tridecenenitrile; 3, 12-tridecadienoic acid nitrile; 3, 7-dimethyl-2, 6-octadienenitrile; 3, 7-dimethyl-6-octenenitrile;
esters of aliphatic carboxylic acids, such as (E) -and (Z) -3-hexenyl formate; hexyl acetoacetate; isoamyl acetate; hexyl acetate; 3,5, 5-trimethylhexyl acetate; 3-methyl-2-butenyl acetate; (E) -2-hexenyl acetate; (E) -and (Z) -3-hexenyl acetate; octyl acetate; 3-octyl acetate; 1-octen-3-yl-acetate; ethyl butyrate; butyl butyrate; isoamyl butyrate; hexyl butyrate; (E) -and (Z) -3-hexenyl isobutyrate; hexyl crotonate; ethyl isovalerate; 2-methyl pentanoic acid ethyl ester; ethyl caproate; allyl hexanoate ester; ethyl heptanoate; allyl heptanoate; ethyl octanoate; (E, Z) -2, 4-decadienoic acid ethyl ester; especially ethyl 2-trans-4-cis-decadienoate; 2-octynoic acid methyl ester; 2-nonanoic acid methyl ester; allyl-2-isopentyloxy acetate; methyl 3, 7-dimethyl-2, 6-octadienoate; 4-methyl-2-pentyl-crotonate;
the formate, acetate, propionate, isobutyrate, butyrate, isovalerate, valerate, hexanoate, crotonate, carotenoate or 3-methyl-2-butenoate of acyclic terpene alcohols, for example citronellol; geraniol; nerol; linalool; lavender alcohol; nerolidol; farnesol; tetrahydrolinalool; tetrahydrogeraniol; 2, 6-dimethyl-7-octen-2-ol; 2, 6-dimethyloctan-2-ol; 2-methyl-6-methylene-7-octen-2-ol; 2, 6-dimethyl-5, 7-octadien-2-ol; 2, 6-dimethyl-3, 5-octadien-2-ol; 3, 7-dimethyl-4, 6-octadien-3-ol; 3, 7-dimethyl-1, 5, 7-octatrien-3-ol; 2, 6-dimethyl-2, 5, 7-octatrien-1-ol;
acyclic terpene aldehydes and ketones, such as geranial; neral; citronellal; 7-hydroxy-3, 7-dimethyloctanal; 7-methoxy-3, 7-dimethyloctanal; 2,6, 10-trimethyl-9-undecenal; geranylacetone and its dimethyl and diethyl acetals; especially geranial, neral, dimethyl and diethyl acetals of 7-hydroxy-3, 7-dimethyloctanal;
-formates, acetates, propionates, isobutyrates, butyrates, isovalerates, valerates, caproates, crotonates, tiglenes and 3-methyl-2-butenoates of cyclic terpene alcohols, such as menthol; isopulegol; alpha-terpineol; terpinenol-4; menthane-8-ol; menthane-1-ol; menthane-7-ol; borneol; isoborneol; linalool oxide; nopol; cedrol; farnesol; vetiverol; guaiol;
cyclic terpene aldehydes and ketones, such as menthone; isomenthone; 8-sulfanyl-menth-3-one; carvone; camphor; fenchone; alpha-ionone; beta-ionone; α -n-methylinogenone; beta-n-methylinogenyl ketone; alpha-isometyl ionone; beta-isometyl ionone; α -irone; (ii) a Alpha-damascone; beta-damascenone; beta-damascenone; delta-damascone; gamma-damascone; 1- (2,4, 4-trimethyl-2-cyclohexen-1-yl) -2-buten-1-one; 1,3,4,6,7,8 a-hexahydro-1, 1,5, 5-tetramethyl-2H-2, 4 a-methanonaphthalen-8 (5H) -one; 2-methyl-4- (2,6, 6-trimethyl-1-cyclohexen-1-yl) -2-butenal; nocardone; dihydronootkatone; 4,6, 8-megastigmatrienol-3-one; alpha-hesperidone; beta-mone; acetylated cedarwood oil (methyl cedryl ketone);
cyclic and alicyclic ethers, such as eucalyptol; methyl cedryl ether; cyclododecyl methyl ether; 1, 1-dimethoxycyclododecane; (ethoxymethoxy) cyclododecane; alpha-cedrene epoxide; 3a, 6,6,9 a-tetramethyldodecahydronaphtho [2,1-b ] furan; 3 a-ethyl-6, 6,9 a-trimethyldodecahydronaphtho [2,1-b ] furan; 1,5, 9-trimethyl-13-oxabicyclo [10.1.0] tribo-4, 8-diene; rose oxide; 2- (2, 4-dimethyl-3-cyclohexen-1-yl) -5-methyl-5- (1-methylpropyl) -1, 3-dioxane;
cyclic and macrocyclic ketones, such as 4-tert-butylcyclohexanone; 2,2, 5-trimethyl-5-pentylcyclopentanone; 2-heptyl cyclopentanone; 2-pentylcyclopentanone; 2-hydroxy-3-methyl-2-cyclopenten-1-one; 3-methyl-cis-2-penten-1-yl-2-cyclopenten-1-one; 3-methyl-2-pentyl-2-cyclopenten-1-one; 3-methyl-4-cyclopentadecanone; 3-methyl-5-cyclopentadecanone; 3-methylcyclopentadecanone; 4- (1-ethoxyvinyl) -3,3,5, 5-tetramethylcyclohexanone; 4-tert-amylcyclohexanone; 5-cyclohexadecen-1-one; 6, 7-dihydro-1, 1,2,3, 3-pentamethyl-4 (5H) -indanone; 8-cyclohexadecen-1-one; 7-cyclohexadecan-1-one; (7/8) cyclohexadecen-1-one; 9-cyclopentadecen-1-one; cyclopentadecanone; cyclohexadecanone;
cycloaliphatic aldehydes, such as 2, 4-dimethyl-3-cyclohexenecarbaldehyde; 2-methyl-4- (2,2, 6-trimethylcyclohexen-1-yl) -2-butyraldehyde; 4- (4-hydroxy-4-methylpentyl) -3-cyclohexenecarbaldehyde; 4- (4-methyl-3-penten-1-yl) -3-cyclohexenecarbaldehyde;
cycloaliphatic ketones, such as 1- (3, 3-dimethylcyclohexyl) -4-penten-1-one; 2, 2-dimethyl-1- (2, 4-dimethyl-3-cyclohexen-1-yl) -1-propanone; 1- (5, 5-dimethyl-1-cyclohexen-1-yl) -4-penten-1-one; 2,3,8, 8-tetramethyl-1, 2,3,4,5,6,7, 8-octahydro-2-naphthylmethylketone; methyl-2, 6, 10-trimethyl-2, 5, 9-cyclododecatrienyl ketone; tert-butyl- (2, 4-dimethyl-3-cyclohexen-1-yl) ketone;
esters of cyclic alcohols, such as 2-tert-butylcyclohexylacetate; 4-tert-butylcyclohexyl acetate; 2-tert-amylcyclohexylacetate; 4-tert-amylcyclohexylacetate; 3,3, 5-trimethylcyclohexyl acetate; decahydro-2-naphthaleneacetic acid acetate; 2-cyclopentyl crotonate; 3-pentyltetrahydro-2H-pyran-4-ylacetic acid ester; decahydro-2, 5,5,8 a-tetramethyl-2-naphthalenyl acetate; 4, 7-methylene-3 a,4,5,6,7,7 a-hexahydro-5 or 6-indenyl acetate; 4, 7-methylene-3 a,4,5,6,7,7 a-hexahydro-5 or 6-indenylpropanoate; 4, 7-methylene-3 a,4,5,6,7,7 a-hexahydro-5 or 6-indenyl isobutyrate; 4, 7-methylene-octahydro-5 or 6-indenyl acetate;
esters of cycloaliphatic alcohols, such as ethyl 1-cyclohexylcrotonate;
esters of alicyclic carboxylic acids, such as allyl 3-cyclohexylpropionate; allyl cyclohexyloxy acetate; cis and trans methyl dihydrojasmonate; cis and trans methyl jasmonate; methyl-2-hexyl-3-oxocyclopentanecarboxylic acid; ethyl-2-ethyl-6, 6-dimethyl-2-cyclohexene carboxylate; ethyl-2, 3,6, 6-tetramethyl-2-cyclohexene carboxylate; ethyl-2-methyl-1, 3-dioxolane-2-acetate;
esters of araliphatic alcohols and aliphatic carboxylic acids, for example benzyl acetate; benzyl propionate; benzyl isobutyrate; benzyl isovalerate; 2-phenethyl acetate; 2-phenylethyl propionate; 2-phenylethyl isobutyrate; 2-phenylethyl isovalerate; 1-phenylethyl acetate; α -trichloromethylbenzyl acetate; α, α -dimethylphenylethyl acetate; α, α -dimethylphenylethylbutyrate; cinnamyl acetate; 2-phenoxyethyl isobutyrate; 4-methoxybenzyl acetate;
araliphatic ethers, such as 2-phenylethylmethyl ether; 2-phenylethyl isoamyl ether; 2-phenylethyl-1-ethoxyethyl ether; phenylacetaldehyde dimethyl acetal; phenylacetaldehyde diethyl acetal; hydrogenated atoxal dimethyl acetal; phenylacetaldehyde glycerol acetal; 2,4, 6-trimethyl-4-phenyl-1, 3-dioxane; 4,4a,5,9 b-tetrahydroindeno [1,2-d ] -m-dioxin; 4,4a,5,9 b-tetrahydro-2, 4-dimethylindeno [1,2-d ] -m-dioxine;
aromatic and araliphatic aldehydes, such as benzaldehyde; phenylacetaldehyde; 3-phenylpropionaldehyde; hydrogenating atoxal; 4-methylbenzaldehyde; 4-methylphenylacetal; 3- (4-ethylphenyl) -2, 2-dimethylpropanal; 2-methyl-3- (4-isopropylphenyl) propanal; 2-methyl-3- (4-tert-butylphenyl) propanal; 2-methyl-3- (4-isobutylphenyl) propanal; 3- (4-tert-butylphenyl) propanal; cinnamic aldehyde; alpha-butylcinnamaldehyde; alpha-amyl cinnamic aldehyde; alpha-hexyl cinnamic aldehyde; 3-methyl-5-benzenevaleraldehyde; 4-methoxybenzaldehyde; 4-hydroxy-3-methoxybenzaldehyde; 4-hydroxy-3-ethoxybenzaldehyde; 3, 4-methylenedioxybenzaldehyde; 3, 4-dimethoxybenzaldehyde; 2-methyl-3- (4-methoxyphenyl) propanal; 2-methyl-3- (4-methylenedioxyphenyl) propanal;
aromatic and araliphatic ketones, for example acetophenone; 4-methyl-acetophenone; 4-methoxyacetophenone; 4-tert-butyl-2, 6-dimethylacetophenone; 4-phenyl-2-butanone; 4- (4-hydroxyphenyl) -2-butanone; 1- (2-naphthyl) ethanone; 2-benzofuranylethanone; (3-methyl-2-benzofuranyl) ethanone; benzophenone; 1,1,2,3,3, 6-hexamethyl-5-indenylmethylketone; 6-tert-butyl-1, 1-dimethyl-4-indenylmethylketone; 1- [2, 3-dihydro-1, 1,2, 6-tetramethyl-3- (1-methylethyl) -1H-5-indenyl ] ethanone; 5',6',7',8' -tetrahydro-3 ',5',5',6',8',8' -hexamethyl-2-acetonaphthalene;
aromatic and araliphatic carboxylic acids and esters thereof, for example benzoic acid; phenylacetic acid; methyl benzoate; ethyl benzoate; hexyl benzoate; benzyl benzoate; methyl phenyl acetate; ethyl phenylacetate; geranyl phenylacetate; phenyl ethyl acetate; methyl cinnamate; ethyl cinnamate; cinnamic acid benzyl ester; phenyl ethyl cinnamate; cinnamic acid cinnamyl ester; phenoxyacetic acid allyl propionic acid; methyl salicylate; isoamyl salicylate; hexyl salicylate; cyclohexyl salicylate; cis-3-hexenylsalicylate; benzyl salicylate; phenyl ethyl salicylate; methyl-2, 4-dihydroxy-3, 6-dimethylbenzoate; ethyl-3-phenylglycidic acid ester; ethyl-3-methyl-3-phenylglycidic acid ester;
nitrogen-containing aromatic compounds, such as 2,4, 6-trinitro-1, 3-dimethyl-5-tert-butylbenzene; 3, 5-dinitro-2, 6-dimethyl-4-tert-butylacetophenone; cinnamonitrile; 3-methyl-5-phenyl-2-pentenenitrile; 3-methyl-5-phenylpentanenitrile; methyl anthranilate; methyl N-methylanthranilate; schiff bases of methyl anthranilate and 7-hydroxy-3, 7-dimethyloctanal, 2-methyl-3- (4-tert-butylphenyl) propanal or 2, 4-dimethyl-3-cyclohexenecarbaldehyde; 6-isopropylquinoline; 6-isobutylquinoline; 6-sec-butylquinoline; 2- (3-phenylpropyl) pyridine; indole; skatole; 2-methoxy-3-isopropylpyrazine; 2-isobutyl-3-methoxypyrazine;
phenyl ethers and phenyl esters, such as estragole; anethole; eugenol methyl ether; isoeugenol methyl ether; diphenyl ether; beta-naphthyl methyl ether; beta-naphthyl ethyl ether; beta-naphthyl isobutyl ether; 1, 4-dimethoxybenzene; butyl phenol acetate; p-cresol phenylacetate;
heterocyclic compounds, such as 2, 5-dimethyl-4-hydroxy-2H-furan-3-one; 2-ethyl-4-hydroxy-5-methyl-2H-furan-3-one; 3-hydroxy-2-methyl-4H-pyran-4-one; 2-ethyl-3-hydroxy-4H-pyran-4-one; and
-dihydrocoumarin; octahydro coumarin; lactones, such as 1, 4-octalactide; 3-methyl-1, 4-octalactide; 1, 4-nonanolide; 1, 4-decanolide; 8-decene-1, 4-lactide; 1, 4-undecanolide; 1, 4-dodecanolide; 1, 5-decanolide; 1, 5-dodecanolide; 4-methyl-1, 4-decanolide; 1, 15-pentadecanoic acid; cis-and trans-11-pentadecen-1, 15-lactide; cis-and trans-12-pentadecen-1, 15-lactide; 1, 16-hexadecanolide; 9-hexadecene-1, 16-alkolide; 10-oxa-1, 16-hexadecanolide; 11-oxa-1, 16-hexadecanolide; 12-oxa-1, 16-hexadecanolide; ethylene 1, 12-dodecanedioate; ethylene 1, 13-tridecanedioic acid; coumarin; 2, 3-dihydrocoumarin; octahydro coumarin. Also suitable as fragrance substances are so-called fragrance substance precursors (Pro-Drug). Such compounds are compounds which release the desired molecules of the odor and/or fragrance substance by breaking of chemical bonds, for example by hydrolysis. In general, to form the fragrance precursor, the desired fragrance raw material is chemically linked to a carrier, which is preferably a slightly or moderately volatile carrier. The combination results in less volatile and more hydrophobic fragrance precursors with improved accumulation on the substance. The fragrance substance is thereafter released by breaking the bond between the fragrance substance raw material and the carrier, for example by changing the pH during storage or drying on the clothesline (e.g. due to transpiration of the carrier), air humidity, heat and/or sunlight.
In addition or alternatively, one or more insect repellents can be included, such as N, N-diethyl-m-toluidine, 1, 2-pentanediol and/or ethyl butylacetamidopropionate.
Additionally or alternatively, one or more cooling agents can be included. Cooling agents are compounds that produce a cold sensation on the skin. Typically, it is here a menthol compound, which-in addition to the base menthol itself-is selected, for example, from: menthone methyl ether, menthone glycerol acetal (FEMA GRAS 3807), menthone glycerol ketal (FEMA GRAS 3808), menthyl lactate (FEMA GRAS 3748), menthone ethylene carbonate (FEMA GRAS3805), menthone propylene carbonate (FEMA GRAS 3806) menthyl-N-ethyl oxalate, monomethyl succinate (FEMA GRAS 3810), monomenthyl glutamate (FEMA GRAS 4006), menthyl-1, 2-propanediol (FEMA GRAS3784), menthyl-2-methyl-1, 2-propanediol (FEMA GRAS 3849), and menthane carboxylic acid esters and amides WS-3, WS-4, WS-5, WS-12, WS-14 and WS-30 and mixtures thereof. The most important representative of these materials is monomenthyl succinate (FEMA GRAS 3810). Not only succinic acid but also similar monomenthyl glutarates (FEMA GRAS 4006) are important representatives of monomenthyl esters based on di-and polycarboxylic acids:
examples of the use of these substances are found, for example, in the documents WO 2003043431 (Unilever) or EP1332772A1 (IFF).
A second important group of menthol compounds which are preferred in the sense of the present invention comprises: carbonates of menthol and polyhydric alcohols, e.g. ethylene glycol, glycerol or carbohydrates, e.g. menthol ethylene glycol carbonate (FEMA GRAS)) Menthol propylene glycol carbonate (FEMA GRAS)
Additionally or alternatively, one or more of the following substances, which the skilled person refers to as TRPV1 and TRPV3 modifiers, can be used. Examples of such substances are: vanillyl derivatives, preferably vanillyl ether, capsaicin, allyl isothiocyanate, ginger oil, 4- (I-menthoxymethyl) -2-phenyl-1, 3-dioxolane, 4- (I-menthoxymethyl) -2- (3',4' -dihydroxyphenyl) -1, 3-dioxolane, 4- (I-menthoxymethyl) -2- (2' -hydroxy-3 ' -methoxyphenyl) -3-dioxolane, 4- (I-menthoxymethyl) -2- (4' -methoxyphenyl) -3-dioxolane, 4- (I-menthoxymethyl) -2- (3',4' -methylenedioxolane) -3-dioxolane, 4- (1-menthoxymethyl) -2- (3 '-methoxy-4' -hydroxyphenyl) -3-dioxolane, red chilli oil, red chilli oleoresin, ginger oleoresin, vanillylnonanoic acid amide, jambu oleoresin, zanthoxylum bungeanum extract, zanthoxylum bungeanum I, zanthoxylum bungeanum II, zanthoxylum piperitum, black pepper extract, black pepper essence and others such as mentioned in patent application US 6780443.
In addition or alternatively, one or more flavoring agents, one or more cosmetic inclusions, one or more pharmaceutically active substances, one or more heat-storage agents, one or more adsorbents and/or one or more inclusions for oral and/or dental care agents can be contained.
Thus, in the process according to the invention, preferably in what has been previously referred to as preferred embodiments, a plurality of or all of the capsules (K) preferably comprise one or more of the following contents: flavoring agents, cosmetic inclusions, pharmaceutically effective substances, insect repellents, inclusions for oral and dental care agents, latent heat storage agents and adsorbents.
In a preferred embodiment of the process according to the invention, preferably in what has been referred to previously as preferred embodiments, a plurality of or all of the capsules (K) have a wall material which is composed of one or more substances from the group consisting of: natural, semisynthetic and fully synthetic casing materials, preferably composed of, or comprising or based on one or more of melamine-formaldehyde resins, gelatin, alginates, polyurethanes, polyamides and polyureas.
The capsules provided in step (i) preferably have capsule walls composed of a material suitable for the intended purpose of use. Suitable capsule wall materials can be, for example: natural shell materials, such as acacia, agar, agarose, maltodextrin, alginic acid or salts thereof, such as sodium alginate or calcium alginate, fats and fatty acids, cetyl alcohol, collagen, chitosan, lecithin, gelatin, albumin, shellac, polysaccharides, such as starch or dextran, polypeptides, protein hydrolysates, sucrose and waxes, semisynthetic shell materials, such as, inter alia, chemically modified celluloses, in particular cellulose esters and ethers, such as, for example, cellulose acetate, ethylcellulose, hydroxypropylcellulose, hydroxypropylmethylcellulose and carboxymethylcellulose, and starch derivatives, in particular starch ethers and esters, or fully synthetic shell materials, such as, for example, polymers, such as, for example, polyacrylates, polyamides, polyvinyl alcohols, aminoplasts, phenolic plastics or polyvinylpyrrolidone.
Capsules (K) which can be used for the purposes of the present invention are commercially available, for example the following commercial products (the shell materials are given in parentheses): hallcrest microcapsules (gelatin, acacia), Coletica Thalapheres (marine collagen), Lipotec microcapsules (alginic acid, agar), Induchem Unispheres (lactose, microcrystalline cellulose, hydroxypropyl methylcellulose), Unicerin C30 (lactose, microcrystalline cellulose)Hydroxypropyl methylcellulose), Kobo glycerospheres (modified starch, fatty acid esters, phospholipids), Softspheres (modified agar) and Kuhs Probiol Nanospheres (phospholipids), and Primaspheres (chitosan, alginate) and Primasys (phospholipids). And from synthetic polymers
According to a preferred embodiment of the invention, the capsules (K) are provided in the form of a capsule dispersion in the process according to the invention (as described therein) for further use. Such capsules can be manufactured, for example, as follows: the substance which can be crystallized from solution is dissolved in a suitable solvent. Next, the capsules were added and the following conditions were achieved: the material dissolved under the conditions crystallizes out again.
In a preferred embodiment of the process according to the invention, one, more or all solvents are selected from: water and water-miscible solvents, preferably ethanol, isopropanol, acetone and DMSO.
It is particularly advantageous to select a solvent in which the crystallizable material/materials crystallize particularly well.
In the process according to the invention, in particular in a preferred embodiment, one, more or all crystallizable materials can be crystallized in a solvent which can be mixed with or has water and/or is preferably selected from: salts, preferably alkali metal and alkaline earth metal salts, particularly preferably sodium sulfate, sodium chloride or sodium carbonate, sugars and urea.
Particularly advantageous are soluble salts, sugars or urea, since they dissolve well in, for example, water or a liquid that can be mixed with water and easily release the contained capsules (K) when the powder is used according to the invention.
In the process according to the invention, in particular in the design referred to as preferred above, in step (ii), the solvent/solvents, if present, are raised or heated to a temperature in the range from 23 ℃ to 50 ℃, preferably in the range from 25 ℃ to 40 ℃, particularly preferably in the range from 30 ℃ to 35 ℃.
If the solvent/solvents are raised or heated to such a temperature, the crystallizable material/materials advantageously dissolve particularly well or particularly quickly in the solvent/solvents.
Preferably, in the process according to the invention, preferably in the embodiment previously referred to as preferred, step (iii) comprises: stirring in order to dissolve the crystallizable material/materials in the solvent/solvents or to simplify the process, preferably at a stirring speed in the range from 100U/Min to 1871U/Min, preferably in the range from 500U/Min to 1300U/Min, particularly preferably in the range from 1000U/Min to 1200U/Min, preferably by means of a guided jet stirrer.
In a preferred embodiment of the process according to the invention, preferably in what has been previously referred to as a preferred embodiment, in step (vi) the temperature of the mixture (M1) is reduced to a temperature of <20 ℃, preferably <15 ℃, more preferably <10 ℃, particularly preferably <5 ℃, wherein the reduction in temperature is preferably carried out over a period of time in the range from 0.25 hours to 3 hours, preferably from 0.5 hours to 2 hours, particularly preferably over a period of time from 0.75 hours to 1.5 hours.
Advantageously, the crystallization of the crystallizable material/materials takes place at the above-mentioned temperatures and within the above-mentioned time period. When the temperature is reduced in the course of time into the abovementioned range, the crystallization of the crystallizable material/materials proceeds under particularly advantageous conditions and leads to the formation of structures which ensure particularly good encapsulation of the capsules (K) containing one or more inclusions into the crystals produced, which in the use according to the invention again lead to protection of the capsules (K), for example against disintegration due to occurring shearing forces.
Preferably, step (vii) of the method according to the invention, preferably in what has been previously referred to as the preferred embodiment, comprises or consists of one, two or all of the following steps:
-pouring the solvent/solvents,
(by filtration and/or centrifugation) of the crystals,
-drying the mixture (M2) obtained in step (vi) and/or the filtered crystals,
in order to obtain a powder consisting of or comprising a plurality of capsules (K) comprising one or more inclusions, encapsulated in crystals.
By preferably pouring and/or filtering and/or drying in step (vii), the powder according to the invention is obtained, which, owing to its powder form, is particularly advantageously added to or mixed with different liquid or solid products.
In the process according to the invention, in particular in one preferred embodiment, the weight ratio of the total amount of solvent(s) to the total amount of crystallizable material(s), to the total amount of capsules (K) and/or capsule dispersions (see above) in step (i) lies in the following ranges: 1-10:0.5-5:0.1-3, preferably in the following ranges: 3-7:1-3:0.5-2.
The abovementioned ranges of the weight ratios are particularly advantageous since in these ranges a particularly advantageous amount of the crystallizable material/materials for the crystallization process is/are present in the solvent/solvents and the crystals produced are able to encapsulate a particularly advantageous amount of capsules (K) so that a particularly advantageous amount of capsules (K) is present in the powder produced for the use according to the invention, but no unnecessary loss of the capsules (K) used occurs in the production of the powder.
Another aspect of the invention relates to a powder which consists of or comprises a plurality of capsules encapsulated in crystals, which capsules contain one or more inclusions, preferably produced by or producible by the method according to the invention, preferably in one preferred embodiment.
Correspondingly suitable for the preferred embodiments of such powders are those mentioned above in connection with the process according to the invention, in particular those mentioned in connection with the preferred embodiments, more particularly those capsules to be (preferably) used according to the invention, their shell material and contents and also (preferably) the crystallizable material to be used.
As already mentioned, the crystals produced according to the invention or the powder produced according to the invention can advantageously be mixed without problems with the already produced laundry powder formulation or the usual constituents of laundry powders. Other products can also contain the crystals or powders described herein.
Accordingly, another aspect of the invention relates to a product selected from the group consisting of: detergents and cleaning agents, body care products, preparations for nutrition or diet, cosmetic or pharmaceutical preparations, aromatized, for aromatized or to be aromatized products, preferably aroma rinses, wherein the products comprise the powder according to the invention.
In addition to the powders described herein, the product also contains other inclusions common to and suitable for such products. These inclusions are very well known to the person skilled in the respective art and are selected accordingly depending on the desired application.
The products according to the invention therefore preferably additionally comprise one or more customary constituents or inclusions of detergents and cleaning agents, body-care products, preparations for nutrition or diet, cosmetic or pharmaceutical preparations or products with added aroma, for added aroma or to be added aroma.
Furthermore, one aspect of the invention relates to the use of the powder according to the invention, wherein a plurality or all of the capsules (K) comprise one or more inclusions selected from the group consisting of: cooling agents, taste enhancers (preferably as described above) and flavouring agents, preferably in amounts sufficient to induce a cooling effect and/or to impart, modify or enhance a sensory impression, preferably an odor and/or taste impression, in order to impart, modify or enhance a sensory impression, preferably an odor and/or taste impression, or to add flavour to a product, preferably a product according to the invention.
Another aspect of the invention relates to a method for manufacturing a product according to the invention, comprising or consisting of the following steps:
(a) provide for
(a.1) the powder according to the invention, and
(a.2) one or more further components, preferably one or more common components or inclusions of detergents and cleaning agents, body care products, preparations for nutrition or diet, cosmetic or pharmaceutical preparations or perfumed, for perfumed or to be perfumed products, and
(b) mixing the components (a.1) and (a.2).
Another aspect of the invention relates to a method for perfuming a substrate, preferably hair, skin, leather or textile fibres, comprising or consisting of the steps of:
(a) providing a powder or product according to the invention as described herein, wherein a plurality or all of the capsules (K) contain one or more inclusions selected from the group consisting of: flavoring agents (preferably as described hereinabove) and flavoring agents, preferably in amounts sufficient to impart, modify or enhance a sensory impression, preferably an odor and/or taste impression, and
(b) the powder or product is applied to the substrate(s) to be perfumed, preferably hair or skin or fibres or leather, preferably in an organoleptically effective amount, preferably in an amount sufficient for the consumer to perceive one or more odors or tastes, with respect to the capsules (K) enclosed therein.
For the preferred embodiments of the use and method described above, the ones mentioned above in connection with the other aspects of the invention, in particular in connection with the preferred embodiments, more particularly the capsules to be (preferably) used according to the invention, their shell material and contents and the (preferably) crystallizable material to be used, apply accordingly.
Detailed Description
The invention is explained in detail below on the basis of selected examples. All statements relate to weight, unless otherwise specified.
Example 1 (according to the invention):
450g of water was heated to about 33 ℃. Subsequently, 200g of sodium sulfate was dissolved with stirring and slowly cooled. Subsequently, 150g of capsule dispersion (710544Symcap Tomcap, Symrise) were added at the beginning of crystallization and cooled to about 2 ℃ and the precipitate was immediately filtered off. The filter cake is subsequently dried.
Example 2 (according to the invention):
450g of water was heated to about 40 ℃, after which 167g of sodium carbonate was added and dissolved with stirring. Immediately thereafter, 150g of capsule dispersion (710544Symcap Tomcap, Symrise) and a further 50g of water were added. Followed by cooling to 1.0 ℃. After filtration, the filter residue was dried.
Example 3 (according to the invention):
250g of water are heated to approximately 37 ℃ and 200g of sodium acetate are subsequently dissolved with stirring. Immediately thereafter, the mixture was cooled to 26 ℃ and 150g of capsule dispersion (710544 SymcapTomcap, Symrise) was added at the beginning of crystallization and cooled to 1.7 ℃ in about 1 hour. After this time, the precipitate was filtered off and the filter cake was dried at room temperature.
Example 4 (comparative example):
a mixture of 330g of water, 206g of modified maize starch (Capsul, Ingretion), 27.0g of maltose monohydrate, 17.5g of Luviskol K-30 and 150g of capsule dispersion (710544Symcap Tomcap, Symrise) was spray dried (inlet temperature 190 ℃ C., outlet temperature 90 ℃ C.) in a spray dryer (B ü chi B290).
Example 5 (according to the invention):
450g of water was heated to about 80 c and subsequently 450g of urea was dissolved with stirring. Subsequently, 150g of the capsule dispersion (710544Symcap Tomcap, Symrise) were added, followed by cooling to room temperature and filtration of the precipitate. The filter cake is then dried.
Example 6 (according to the invention):
500g of water are heated to approximately 40 ℃ and subsequently 100g of sodium sulphate are dissolved with stirring. Immediately thereafter, 20g of the capsule dispersion (710544Symcap Tomcap, Symrise) were added, immediately followed by cooling to 25 ℃. Thereafter, the precipitate was cooled further to about 1.7 ℃ and subsequently an additional 20g of sodium sulfate was added as seed crystals and the resulting precipitate was filtered off. The filter cake is then dried.
Example 7: control test
To prepare a sensory control study, 0.200g of the sample according to example 4, 0.207g of the sample according to example 1 and 40g of detergent are provided, respectively, and 0.08g of 710544Symcap Tomcap (Symrise AG, Holtmden, Germany) is provided per 40g of detergent (Denk mitVollwasschmitt Ultra Sensitive detergent, dm-hydrogerie markt GmbH + CO. KG, Carlsrue, Germany) and mixed. The samples thus produced were subsequently washed in 2kg of terry cloth (Fa. Karl Heinz Hesse GmbH, Delensfeld, Germany, towel TB1, 80% BW, 20% PES, 30X 30cm) in a commercially available European washing machine at 40 ℃. Next, the terry cloth was dried on the clothesline at room temperature. The anonymous samples were then individually settled by a panel of 14 experts without mechanical load (untreated), after gentle kneading of the laundry (kneading) and after rubbing the cloths against each other (crushing) and evaluated for fragrance intensity according to scale 1-9. The results (see fig. 2) show that the release of capsules produced by the process according to the invention or their contents in laundry powder is not reduced compared to spray-dried capsules (according to example 4) or compared to the use of liquid capsule dispersions alone (710544Symcap Tomcap).
Example 8 (according to the invention):
500g of water are heated to approximately 33 ℃ and 200g of sodium sulphate are subsequently dissolved with stirring. Immediately thereafter, the mixture was slowly cooled, crystallization started and the first small crystals formed. 198g of Folco Microdeur (Follmann GmbH & Co. KG, Mingde, Germany) were then added and cooled to 1.7 ℃. Next, the precipitate was filtered off and the filter cake was dried.
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