CN103249826B - Fragrance granules for detergents - Google Patents

Fragrance granules for detergents Download PDF

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Publication number
CN103249826B
CN103249826B CN201080070369.XA CN201080070369A CN103249826B CN 103249826 B CN103249826 B CN 103249826B CN 201080070369 A CN201080070369 A CN 201080070369A CN 103249826 B CN103249826 B CN 103249826B
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release particles
acid
particles according
perfume compound
released
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CN103249826A (en
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诺贝特·A·布老恩
蒂·扬·泰
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Symrise AG
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Symrise AG
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039Coated compositions or coated components in the compositions, (micro)capsules
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/72Ethers of polyoxyalkylene glycols
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2003Alcohols; Phenols
    • C11D3/2006Monohydric alcohols
    • C11D3/201Monohydric alcohols linear
    • C11D3/2013Monohydric alcohols linear fatty or with at least 8 carbon atoms in the alkyl chain
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2003Alcohols; Phenols
    • C11D3/2006Monohydric alcohols
    • C11D3/2017Monohydric alcohols branched
    • C11D3/202Monohydric alcohols branched fatty or with at least 8 carbon atoms in the alkyl chain
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2003Alcohols; Phenols
    • C11D3/2006Monohydric alcohols
    • C11D3/2027Monohydric alcohols unsaturated
    • C11D3/2031Monohydric alcohols unsaturated fatty or with at least 8 carbon atoms in the alkenyl chain
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2093Esters; Carbonates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/34Organic compounds containing sulfur
    • C11D3/3409Alkyl -, alkenyl -, cycloalkyl - or terpene sulfates or sulfonates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/34Organic compounds containing sulfur
    • C11D3/3418Toluene -, xylene -, cumene -, benzene - or naphthalene sulfonates or sulfates
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/37Polymers
    • C11D3/3703Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3707Polyethers, e.g. polyalkyleneoxides
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/50Perfumes
    • C11D3/502Protected perfumes
    • C11D3/505Protected perfumes encapsulated or adsorbed on a carrier, e.g. zeolite or clay
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/26Organic compounds containing oxygen
    • C11D7/261Alcohols; Phenols
    • C11D7/262Alcohols; Phenols fatty or with at least 8 carbon atoms in the alkyl or alkenyl chain
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/26Organic compounds containing oxygen
    • C11D7/265Carboxylic acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/22Organic compounds
    • C11D7/26Organic compounds containing oxygen
    • C11D7/266Esters or carbonates

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Dispersion Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Fats And Perfumes (AREA)

Abstract

The present invention relates to encapsulated fragrances, products comprising such encapsulated fragrances and corresponding methods of manufacture and uses. The particles comprise a) a substance to be released, b) a carrier, wherein said carrier is a hydrotrope which is a solid at 20 DEG C, c) a shell comprising hydrophobic shell material having a melting point of at most 65 DEG C, preferably of 40-60 DEG C, and d) a disintegrator material comprised in the shell for disintegrating the shell after immersion in water.

Description

For the perfume compound particulate of washing composition
The present invention relates to through encapsulating perfume compound, comprising this type of through encapsulating product of perfume compound and corresponding preparation method and purposes.
In scouring agent field, perfume compound is used to giving clean olfactory impression through washing on material.In the preparation process of this type of laundry composition, must carefully avoid the critical conditions that chemically can change perfume compound to avoid the loss of perfume compound quality and intensity.Therefore attempted by protecting them with protectiveness material as solid carrier or encapsulating shell hold perfume compound.
Such as, US5336665 discloses a kind of perfume particle, and it is applicable in detergent for washing clothes or bleaching composition to make the intensity of spices in composition obtain controlling, suppressing undesirable perfume loss and serve as the delivery means to fabric, skin or other article.Described spices is preferentially absorbed in hydrophobic porous inorganic carrier particle by such as spraying.Described inorganic carrier is endowed hydrophobicity by being such as heat-treated to many three hours at the temperature of 500 to 1000 DEG C.
US5500223 relates to a kind of encapsulating method of hydrophobic liquid.First emulsion is prepared with silicon-dioxide, perfume compound and water.Then by carrying out gelation process with hcl acidifying to emulsion.
WO99/38945A1 discloses final by separating and the water-dispersible microparticles encapsulated by water-soluble or water dispersible Solid Organic Matrix.The emulsion of organic substrate and spices and water is made to stand drying process at the temperature of paramount 150 DEG C.
US6932982 relates to a kind of microparticulate delivery systems, and described system comprises and is distributed in seasonings in whole Agar substrate or perfume compound.In agar-agar soln, add the mixture of sucrose, Star Dri 5 and water and this mixture is heated to the temperature of 123 DEG C.In heavy syrup, add perfume compound and emulsifying agent to form uniform melt, then extrude this melt under stress and dry.
EP816484A2 relates to a kind of for the fragrance carrier in detergent composition.Spices is adsorbed on inorganic carrier and is also then added in polyoxyethylene glycol by the high molecular weight polyethylene glycol of melting and spices are mixed or be ejected on solid inorganic carrier.Make the temperature of high molecular weight polyethylene glycol maintenance needed for liquid state within the scope of 60 to 80 DEG C.
US7485610 and EP816484 is similar, and its heating perfume compound makes it to be dissolved in the mixture of solid fatty alcohol, lipid acid, fatty alcohol ethoxylate and/or polyoxyethylene glycol.Then make this mixture solidify and can be applicable in such as soap, washing composition and fabric softening agent.
Although there are these to attempt, so far, the problem of perfume compound is protected not obtain gratifying solution.Especially disadvantageously, according to prior art, perfume compound usually must heat the quite a while.In addition, be usually considered to too expensive, particularly in cost sensitivity market for the material encapsulated and corresponding technique.
In addition, the perfume compound in detergent composition usually needs to be attached to and still exists with the problem of giving permanent pure and fresh clean impression on washing product.But due to the existence of cleaning substance, particularly washing composition in laundry composition, such attachment is very difficult to realize.Cleaning substance due to laundry composition is substantially chosen as and removes not yet firm attachment all things thereon from article to be washed, therefore they will resist perfume compound effectively to any potential attachment on article to be washed.Therefore people usually attempt the concentration of perfume compound in increase laundry composition with the attachment perfume compound minimally measured, even if cleaned component is washed off by most of perfume compound.But the concentration increasing perfume compound in laundry composition will affect the price of such composition greatly.In addition, it has been generally acknowledged that it is inadequate for only making perfume compound be attached to article.Need perfume compound can not evaporate immediately after the drying but leave permanent impression on the contrary.
But, the invention is not restricted to encapsulate perfume compound.On the contrary, overall object of the present invention is to provide the method for stabilizing activity material, particularly under laundry situation.
According to the present invention, because herein is provided a kind of release particles, it comprises
A) material to be released, preferred fragrance agent,
B) carrier, wherein said carrier is the hydrotropic agent for paste or solid at 20 DEG C,
C) shell, it comprises, and fusing point is 65 DEG C at the most, the preferred hydrophobic shell material (fusing point of 15 DEG C to 20 DEG C represents that material will be at room temperature liquid) of 40 to 60 DEG C, and
D) disintegrating agent material, it is included in shell for making shell disintegration after being immersed in the water.
According to the present invention, finding, by using hydrotropic agent as the carrier of one or more of active substance, especially one or more of perfume compound, the harmful effect that these materials make it from encapsulating and/or the necessary heat of spraying dry can be protected.Its with fusing point be the shell material of 65 DEG C at the most combined time especially handy.These melt temperatures make it possible to avoid harsh temperature condition with the hydrotropic combination as carrier and encapsulate material to be released, particularly perfume compound.Especially, the perfume compound be adsorbed on hydrotropic agent carrier need not be exposed to high temperature encapsulating material for a long time with other materials; On the contrary, with carrier contact after, can cool fast compared with the shell material of low melting point.Further, the combination of hydrotropic agent and low melting point shell material can avoid chemical corrosion encapsulating method, such as, needs pH sharply to change to realize the sol-gel method of solidifying of shell material.Particularly advantageously, release particles of the present invention can be prepared in anhydrous situation, if needed like this.The preferred method preparing release particles of the present invention by later therewith other advantages of class methods describe together.
By comprising disintegrating agent material in hydrophobic shell, release particles of the present invention is specially adapted to laundry situation.After contact with water, disintegrating agent material can break or pierce through shell, and active substance such as perfume compound or fragrance blend also can be contacted with water, such as, be dissolved in wherein or react with water or the compound be dissolved in water.
By selecting disintegrating agent material, can adjustment release particle to the tolerance of water.Therefore, release particles of the present invention is particularly suitable for h substance (such as perfume compound) after particle is immersed in the water predetermined time.Therefore, what can make material, particularly one or more of perfume compound is released in the time that Late phase in laundry processes works as, make perfume compound or other active substances laundry processes close at the end of release.Usually, at the end of laundry processes by with water rinse article to be washed to remove or to reduce the amount of the washing composition be adsorbed on article.Therefore, by postponing the release of material, particularly perfume compound, the situation that this type of material is exposed to harsh washing composition condition can be avoided or reduce.Therefore active substance more easily will be made to be attached on article to be washed or to prevent described material to be destroyed as high ph-values because of washing composition and disadvantageous laundry situation or to remove.
For practical purposes, disintegrating agent material is water-soluble material.Therefore disintegrating agent material can remove from shell along with contacting with water, thus leaves room or the passage of the sensible hydrotropic agent carrier of possibility.In addition, the room left by the disintegrating agent material removed from shell because of contact liq water can weaken shell or make shell unstable, makes release particles to break or to split in typical laundry situation process.But, the invention is not restricted to specific disintegrating agent material model or effect; Disintegrating agent material is adjustable, and release particles to be immersed time of releasing of active substance after in liquid water just enough.
Equally for practical purposes, described Water soluble disintegrating agents's material is solid or mashed prod at 20 DEG C.This will guarantee that disintegrating agent material does not leak or evaporation from release particles in dry conditions, namely not be exposed to liquid water.
The fusing point of hydrophobic shell material is preferably 35 to 65 DEG C, is even more preferably 40 to 60 DEG C.Therefore preferred shell material is heated to 60 DEG C or 60 DEG C of liquefaction being just enough to realize the enough degree of shell material is at the most heated to allow encapsulation vehicle material on particulate by such as shell material being ejected into carrier or particle for most preferred shell material.
For preferred release particles of the present invention, the total amount of material to be released is at the most 40 % by weight of the amount of hydrotropic agent carrier, is preferably 5 to 10 % by weight.Find, for release particles of the present invention, perfume compound and other active substances to be released can be adsorbed on hydrotropic agent effectively, thus shield the impact that material to be released makes it from harsh encapsulating condition.
The total amount of hydrophobic shell material and disintegrating agent material is at most 1: 1 relative to the ratio of the total amount of hydrotropic agent carrier and material to be released, is preferably 1: 9 to 2: 5.Find, according to the present invention, even if consider typical laundry situation, also only need hydrophobic shell material low like this and disintegrating agent quantity of material just effectively can encapsulate material to be released and hydrotropic agent carrier.
The carrier of release particles of the present invention is preferably or comprises such hydrotropic agent, it is selected from the salt of Phenylsulfonic acid, toluenesulphonic acids, xylene monosulfonic acid, isopropyl sulfonic acid, methyl isopropyl Phenylsulfonic acid, hydroxyl naphthoic acid, croceine acid, ethylhexyl sulfuric acid, preferably their sodium salt, and in these materials both or more the mixture of person, be preferably sodium xylene sulfonate and/or toluenesulfonic acid sodium salt.Described hydrotropic agent is particularly suitable for the perfume compound adsorbing material to be released, particularly fragrance blend, even in anhydrous situation.Also find further, described hydrotropic agent, particularly sodium xylene sulfonate and/or toluenesulfonic acid sodium salt make it the harmful effect of the mixture from the hydrophobic shell material and disintegrating agent material being exposed to melting by effectively protecting material to be released such as perfume compound or fragrance blend.
The disintegrating agent material of release particles of the present invention is preferably selected from nonionogenic tenside, preferred Soxylat A 25-7 and polyoxyethylene glycol, and described polyoxyethylene glycol preferably has the molecular weight of at least 2000.Find, the selection of these materials can under typical laundry situation disintegration described above release particles of the present invention, particularly by weakening its shell or forming hole and passage wherein, be immersed in the water rear predetermined time to postpone the particle that is released into of material as perfume compound or fragrance blend.
In addition, the hydrophobic shell material of release particles of the present invention is preferably selected from side chain or straight chain, saturated or undersaturated C15-C24
-lipid acid, and
-fatty alcohol, and
Their ester.
Particularly preferred hydrophobic shell material is selected from hexadecanol, cetostearyl alcohol, stearyl alcohol, palmitinic acid, stearic acid, tetradecanoic acid, diglycol stearate and ethylene glycol monostearate.Use this type of preferred or particularly preferred hydrophobic shell material, solid or the hydrotropic encapsulating of pasty state can realize under low temperature described above, thus restriction is adsorbed onto the exposure of material to be released, particularly perfume compound or the fragrance blend of carrier.
The shell material that particularly preferably release particles of the present invention has comprises following combination or by forming as follows: a) preferred hydrophobic shell material, preferably, hexadecanol, cetostearyl alcohol, stearyl alcohol, palmitinic acid, stearic acid, tetradecanoic acid, their glycol ester and their mixture, and b) be selected from the disintegrating agent material that Soxylat A 25-7 and molecular weight are the polyoxyethylene glycol of 2000 to 8000.Under typical laundry situation, component a) and b) and respective mixture ratio can be selected to make the seclected time of the hang-over n. of material to be released after being immersed in the water by those skilled in the art.
Usually, time of releasing increases with the increase being used as the polyoxyethylene glycol of disintegrating agent material and the molecular weight of Soxylat A 25-7, because the higher temperature of such material require and longer time are dissolved in water.In addition, the amount of the ester of C15-C24 lipid acid, fatty alcohol and this type of lipid acid and/or fatty alcohol is higher, chain length is longer, also needs for longer periods to be exposed to water and/or higher laundering temperatures just can make the content of particle discharge.Particularly preferred example combinations will be described below.
Material to be released is preferably the mixture of perfume compound or two kinds, three kinds or more kind perfume compound.Any perfume compound known in the art or spices is can be for the perfume compound in the present invention or spices, particularly S.Arctander, Perfume and Flavor Chemicals, privatepublishing house, Montclair, N.J., 1969 and Surburg, Panten, CommonFragrance and Flavor Materials, 5th Edition, Wiley-VCH, those described in Weinheim2006, in preferred US2008/0070825 specifically mentioned those.One of the present invention is characterised in that, can use perfume compound or the spices of the scope of non-constant width.Example comprises succsinic acid two geraniol ester, succsinic acid two flores aurantii ester, succsinic acid spiceleaf flores aurantii ester, geranyl phenylacetate, neryl phenylacetate, lauric acid geraniol ester, lauric acid flores aurantii ester, toxilic acid two (lemongrass) ester, dinonyl maleate, toxilic acid two phenoxy ethyl, succsinic acid two (3,7-dimethyl-1-octyl group) ester, toxilic acid two (cyclohexyl-ethyl) ester, hexanodioic acid two (phenylethyl) ester, Iso E super, methylionone, cetone gamma, vertofix coeur, methyl dihydrojasmonate, methyl 1,6,10-trimethylammonium-2,5,9-cyclododecatriene-1-base ketone, 7-ethanoyl-1,1,3,4,4,6-HMT, 4-ethanoyl-6-the tertiary butyl-1,1-dimethylindane, to hydroxy-phenyl-butanone, benzophenone, methyl betanaphthyl ketone, 6-ethanoyl-1,1,2,3,3,5-hexamethyl indane, 5-ethanoyl-3-sec.-propyl-1,1,2,6-tetramethyl-indane, 1-dodecanal, 4-(4-hydroxy-4-methyl amyl group)-3-cyclohexene-1-formaldehyde, 7-hydroxyl-3,7-dimethyl octanal, 10-hendecene-1-aldehyde, isohexenyl hexahydrobenzaldehyde, formyl tristane, the condensation product of laurine and methyl oaminobenzoate, the condensation product of laurine and indoles, the condensation product of phenylacetic aldehyde and indoles, 2-methyl-3-(to tert-butyl-phenyl)-propionic aldehyde, vanirone, vanillin food grade,1000.000000ine mesh, piperonylaldehyde, hexyl cinnamic aldehyde, amyl cinnamic aldehyde, 2-methyl-(2-p-isopropyl phenyl) propionic aldehyde, tonka bean camphor, γ-decalactone, thibetolide, 16-hydroxyl-palmitoleic acid lactone, cyclohexadecanone, 8-ring hexadecylene ketone, 1,3,4,6,7,8-six hydrogen-4,6,6,7,8,8-pregnancy basic ring penta-γ-2-chromene, 2-Naphthol methyl ether, ambrox, ten dihydro-3a, 6,6,9a-tetramethyl-naphtho-[2,1b] furans, cypress camphor, 5-(2,2,3-front three basic ring penta-3-thiazolinyl)-3-methylpent-2-alcohol, 2-ethyl-4-(2,2,3-trimethylammonium-3-cyclopentenes-1-base)-2-butylene-1-alcohol, caryophyllenol, tricyclo decenyl propionate, verdy acetate, Whitfield's ointment benzene methyl, cedryl acetate, acetic acid p-(tertiary butyl) cyclohexyl, essential oil, resinoid and the resin from multiple source, described source includes but not limited to orange oil, lemon oil, Wrinkled Gianthyssop Herb, Surinam balsam, olibanum resinoid sample material, Styrax, ladanum resin, Semen Myristicae, oil of bay, styrax resinoid, coriandrum, assorted lavandula angustifolia and lavandula angustifolia, phenylethyl alcohol, terpinol, linalool, linalyl acetate, Geraniol, vernol, 2-(1,1-dimethyl ethyl) adnoral acetate, jasmal, orange terpenes, oxymethoxyallylbenzene, diethyl phthalate, and their combination.
According to the present invention, additionally provide a kind of cleaning composition, it comprises washing composition and according to release particles of the present invention.In view of release particles of the present invention, such cleaning composition can realize above-mentioned advantage.
Preferably, described cleaning composition comprises anionic detergent.More preferably, described cleaning composition not only comprises one or more of anionic detergent but also comprise one or more of nonionic detergent.
According to the present invention, additionally provide a kind of method preparing release particles of the present invention, it comprises step:
I () makes hydrotropic agent absorb material to be released to obtain slug particle,
(ii) heat and mix hydrophobic shell material and disintegrating agent material to obtain the coated mixture of liquid,
(iii) with the slug particle of coated mixture encapsulation steps (i) of liquid of step (ii) to obtain release particles.
For the coated mixture of coated liquid in step (iii), preferably there is 100 DEG C at the most, the preferred temperature of 80 DEG C at the most.Due to the low melting point of hydrophobic shell material described above, therefore such temperature is enough to coated slug particle.Similarly, as described above, coated mixture or liquefy completely or at least liquefy as making it can via nozzle ejection with coated slug particle.Through coated particle, preferably there is the size that length and width or height are no more than 1cm.
The present invention is also further described by some embodiments.But generally speaking, these embodiments should not be construed as restriction claims or scope of the present invention.Unless otherwise stated, all percentage ratio is all based on weighing scale.
Embodiment 1
Following formula is used to test, using stearyl alcohol as unique encapsulating composition.
The sodium xylene sulfonate of grinding in granule, so that gained powder and particulate have larger surface-area to adsorb perfume compound (part A).The stearyl alcohol (part B) of melting is added to form slurry to the sodium xylene sulfonate adsorbing perfume compound.This mixture of continuously stirring, hardens under the fusing point (60 DEG C) dropping to stearyl alcohol along with slurry mix Yin Wendu, produces particulate.
In containing 1 premium on currency of 5 grams of standard detergent powder, soluble test is carried out to these particulates with 1 gram of particulate.On mechanical stirrer, continuously stirring is not after one hour heatedly, and perfuming particulate keeps almost insoluble in detergent solution.Therefore, in cold water washing scheme, detergent solution can not make the particulate disintegration release perfume compound of coated stearyl alcohol.
Embodiment 2
Following formula stearyl alcohol and polyoxyethylene glycol (molecular weight 8000) is used to test.
Also fully mixing (part A) on sodium xylene sulfonate is adsorbed onto according to making perfume compound in embodiment 1.The melt blended material (part B) of stearyl alcohol, polyoxyethylene glycol and oil-soluble colourant is added to form slurry to the sodium xylene sulfonate adsorbing perfume compound.This mixture of continuously stirring, hardens under the fusing point (60 DEG C) dropping to stearyl alcohol along with slurry mix Yin Wendu, produces particulate.
Due to higher stearyl alcohol content, the perfuming particulate of formula C shows as has harder quality than the perfuming particulate of formula B.Soluble test is carried out according to embodiment 1.After 1 hour, nearly all perfuming particulate disintegration all of two kinds of formulas.Therefore, water soluble ingredient is needed to be used as the disintegration of perfuming particulate to discharge the auxiliary agent of perfume compound.
Embodiment 3
Use following formula to test, compare the perfume compound carrying capacity of on hydrotropic agent sodium xylene sulfonate 5% and 10%.
Perfuming particulate is formed according to the program in embodiment 1 and 2.
In the soluble test provided in the aforementioned embodiment, these perfuming particulates are not disintegration completely after 1h.The minimizing of the relative preceding embodiment of polyoxyethylene glycol shows, the amount by water soluble ingredient controls disintegration rate.
Embodiment 4
Use following formula stearyl alcohol and test as water soluble ingredient with nonionogenic tenside.
Perfuming particulate is formed according to the program in embodiment 1 and 2.
In the soluble test provided in the aforementioned embodiment, compared with the perfuming particulate of formula G, the perfuming particulate almost disintegration completely of formula F.Therefore, also disintegration rate can be regulated with the tensio-active agent with different HLB value or different water-soluble degree simply.
Embodiment 5
Using following formula to test, wherein diglycol stearate as can not be water-soluble or hydrophobic component.
Perfuming particulate is formed according to the program in embodiment 1 and 2.
In the soluble test provided in the aforementioned embodiment, the perfuming particulate of formula H has the disintegration rate similar to the perfuming particulate of formula G.Therefore, the impact of this hydrophobic components on disintegration rate is large less than water soluble ingredient.
Embodiment 6
Machine-wash in the detergent powder of routine with the perfuming particulate of formula C, D, E, F, G and H.
Detergent powder powder formulation
Control sample is prepared by allowing the pure perfume compound (Quick Flash) only in detergent powder with 0.15%.
Because the perfuming particulate of C and D of filling a prescription has the perfume compound carrying capacity of 10% on hydrotropic agent, thus its with 1.4% dosage introduce in detergent powder with the perfume compound carrying capacity providing 0.1%.Formula E, F, G and H have the perfume compound carrying capacity of 5% on hydrotropic agent, therefore its with 2.8% dosage introduce in detergent powder with the perfume compound carrying capacity providing 0.1%.Total perfume compound carrying capacity on detergent powder is 0.15%, and wherein free perfume compound carrying capacity is 0.05%.Total perfume compound carrying capacity is set to lower than 0.2%, can evaluate the performance difference owing to perfuming particulate from sense of smell better.
Laundry load is 3kg, and wash(ing)cycle is made up of 1 washing stage and 2 rinse stages.Draining and water smoking is had between washing and each rinse stage.Wash(ing)cycle (cold water washing) completed after about one hour.The amount of detergent powder used is 25 grams of tests at every turn.
Evaluation result
After rinsing Dried overnight
Control sample Can perception Can not detect
C Faintly perceive Can not detect
D Can perception Faintly perceive
E By force Can perception
F Can perception Can not detect
G Can perception Can perception
H Can perception Faintly perceive
Control sample has the perfume compound carrying capacity of 0.15% on detergent powder.Without perfuming particulate.
Formula C has the perfume compound carrying capacity of 10% on hydrotropic agent, uses 24 parts of stearyl alcohol to 16 parts of polyoxyethylene glycol.
Formula D has the perfume compound carrying capacity of 10% on hydrotropic agent, uses 28 parts of stearyl alcohol to 12 parts of polyoxyethylene glycol.
Formula E has the perfume compound carrying capacity of 5% on hydrotropic agent, uses 28 parts of stearyl alcohol to 12 parts of polyoxyethylene glycol.
Formula F has the perfume compound carrying capacity of 5% on hydrotropic agent, uses 28 parts of stearyl alcohol to 12 parts of Ceteareth-12.
Formula G has the perfume compound carrying capacity of 5% on hydrotropic agent, uses 28 parts of stearyl alcohol to 12 parts of Steareth-2.
Formula H has the perfume compound carrying capacity of 5% on hydrotropic agent, uses 28 parts of diglycol stearates to 12 parts of Steareth-2.
Interpretation of result
Control sample:
Under the low dosage of 0.15%, perfume compound can not be detected in the drying stage from sense of smell, this is not unexpected.Under low perfume compound dosage, any free perfume compound adhering to fabric after complete wash(ing)cycle will be MIN and expection can not have impact to drying fabric.
Formula C:
Perfume compound after rinsing on fabric faintly perceives.In this, the performance of this formula is not as control sample.Weak owing to showing perfume compound performance after rinse stage, therefore unexpectedly the external drying stage can't detect perfume compound from sense of smell.
Formula D:
After rinse stage, formula D and control sample have equal performance, and good in drying stage outline, and perfume compound still faintly can perceive from sense of smell.
Formula C and D compares with control sample:
The water-soluble height of formula C ratio formula D, because it has the water soluble ingredient polyoxyethylene glycol of more a large amount.In the drying fabric of formula D perfume compound sense of smell on exist and show to have the deposition level slightly higher than the perfuming particulate of control sample or formula C.Therefore the advantage of the release postponing perfume compound in wash(ing)cycle is had, particularly when discharging under the existence of perfume compound in detergent active.
But although water-soluble lower than control sample, the performance of formula C is not as control sample.Therefore, the mechanism of wash(ing)cycle has effect.The perfuming particulate of the D that there is realistic possibility that some perfuming particulates lose at bleeding stage and this possibility is also applicable to fill a prescription.Perfuming particle loss amount assuming that fill a prescription in wash(ing)cycle between C and formula D is similar, then the amount being discharged into the perfume compound in wash(ing)cycle by lower than 0.15% control sample.
Under the existence of detergent active, the perfume compound of control sample release 0.15% is in the washing stage.A part for this perfume compound of 0.15% will be lost as emulsified substance matter and lose in bleeding stage due to detergent active.Therefore, in this perfume compound of 0.15%, only a part will deposit on fabric.
Water-soluble low than control sample of perfuming particulate of formula C, therefore under detergent active exists, the release of perfume compound postpones to the centre of washing stage or ending phase.The a part of perfume compound discharged in this stage is by by detergent active (that is, be not attached to other detergent active) from the emulsification dirt of the fabric institute's emulsification dissociated.It is expected that, some perfuming particulates can not will utilize at rinse stage physics to discharge perfume compound in bleeding stage loss.Because the performance of the C that fills a prescription after rinse stage is not as control sample, therefore be enough to show that the amount of the perfume compound be deposited on fabric is lower.Therefore, the C that fills a prescription is lost to the semi-invariant of detergent active and bleeding stage more than control sample.
Formula D is than formula C water-soluble low and sense of smell shows better than control sample.Due to still can perception perfume compound (this is contrary to the C that fills a prescription control sample) in drying fabric, therefore fabric deposited the perfume compound of higher amount.Assuming that loss and can not to utilize with the amount of release through encapsulating the micro-material of perfuming of perfume compound for formula C and formula D at rinse stage physics be similar (being used in detergent powder with identical dosage because of them) in bleeding stage, then the amount that will be as being lost by the emulsified substance of detergent active institute emulsification of difference.The release that perfume compound is more late under the existence of detergent active compared to formula C makes the amount as being lost by the emulsified substance of detergent active institute emulsification lower.Therefore, the perfume compound of higher amount discharges at rinse stage, and now, the concentration of detergent active is significantly lower.
Formula E:
With the drying stage after rinse stage, the performance of formula E is all better than control sample, formula C and D, shows have the perfume compound of higher amount to be deposited on fabric.
Formula E is similar in amount and the composition of encapsulating material with the D that fills a prescription.But the perfume compound carrying capacity on hydrotropic agent is 10% of 5% instead of formula D.Therefore, for making perfume compound be 0.1%, in detergent powder, the amount of perfuming particulate is 1.4% of 2.8% instead of formula D.
Mechanism due to wash(ing)cycle had been discussed and had been similar for formula E and the D that fills a prescription, therefore the amount of perfuming particulate that difference will be to lose in bleeding stage.Loss each perfuming particulate for formula E for containing 5% perfume compound and for formula D for containing 10% perfume compound.If loss perfuming particulate quantity for formula E and formula D be similar, then accumulation get up, fill a prescription D will lose the perfume compound of higher amount in bleeding stage.Therefore, the E that fills a prescription will deposit the perfume compound of higher amount on fabric than formula D.
In this, what is interesting is and notice, by reducing the perfume compound carrying capacity on perfuming particulate, in the perfume compound deposition on fabric, have appreciable beneficial effect.This deviates from mutually with the method for prior art, and the encapsulating process of prior art concentrates on increases perfume compound carrying capacity on capsule to usual 20% to higher than in the scope of 40%.In wash(ing)cycle, when the perfuming capsule that perfume compound load is 20% to 40% loses in bleeding stage, it represents the loss of this perfume compound of 20% to 40%, the perfume compound carrying capacity of this and perfuming particulate be 5% to 10% the present invention form contrast.Similarly, when perfuming capsule designs is dissolving or disintegration immediately in presence of water, it will discharge perfume compound and therefore will have higher amount by the emulsification of detergent active institute under the existence of detergent active.
Formula F:
Formula F is similar to formula E, and hydrotropic agent has the perfume compound carrying capacity of 5%, but replaces water soluble ingredient polyoxyethylene glycol with nonionic Ceteareth-12.Show similar to control sample and similar to formula C part.Therefore, formula F is applicable to about control sample and the mechanism of the wash(ing)cycle of formula C.
Formula G:
Formula G is similar to formula F, but replaces nonionic Ceteareth-12 to have compared with low water solubility degree or compared with another nonionic Steareth-2 of low hlb.Outperform formula F and control sample, after rinsing, all have good Olfactive evaluation with drying stage.
The mechanism of wash(ing)cycle is identical, and difference is attributable to the non-ionic use of lower HLB, and it reduces the water-soluble of perfuming particulate.As previously discussed, the water-soluble aft section of hang-over n. to wash(ing)cycle making perfume compound of reduction.
Formula H:
Formula H is similar to formula G, but with the component stearyl alcohol that diglycol stearate replacement can not be water-soluble or hydrophobic.Show similar to formula G, therefore, the impact that the change of hydrophobic components does not have the change of water soluble ingredient to show it on the impact that it shows is large.
Embodiment 7
Carry out according to formula below the experiment introducing cation activity thing according to the program in embodiment 1 and 2.
As the control sample of the existence of anionic-cationic mixture in confirmation detergent solution, prepare two beakers with 1 premium on currency.The cation activity thing Rewoquat WE15 of 5 grams of not spiced detergent powders and 1% is added in a beaker.5 grams of not spiced detergent powders are added in contrast in another beaker.By mechanical stirrer at ambient temperature continuously stirring within 30 minutes, make the detergent powder in two beakers dissolve.Then by detergent solution in left at ambient temperature two hours.At the end of during this period of time, insoluble builder such as zeolite is deposited in the bottom place of beaker.Relatively showing of these two kinds of detergent solutions, compared with the control sample of no cationic actives, the detergent powder with the cation activity thing of 1% wants how muddyly and have more precipitation, see Fig. 1 at the bottom place of beaker.
Machine-washing according to embodiment 6 with identical not spiced detergent powder basis used in control experiment with the particulate that formula PFC and formula FC are formed.
Detergent formulation:
Supplier 1 2 3
Not spiced detergent powder 94.35 80 80
PFC 5.6
FC 20
FC2 20
Quick Flash (spices) Symrise 0.05
Amount to 100 100 100
Detergent formulation 1 cationic active matter content is 0.1%, close to 1% in detergent formulation 2.
Washing test is analyzed:
Detergent formulation 1
Although cation activity thing content is low, to fabric slightly ramollescence, show fabric to deposited cation activity thing.Fabric there is no the particle of anionic-cationic mixture.
Detergent formulation 2
Similar to the control experiment of the existence confirming anionic-cationic mixture close to the cation activity thing content of 1% in formula, therefore, in wash(ing)cycle, form the possibility of anionic-cationic mixture higher than detergent formulation 1.But through washing any existence of fabric not shown anionic-cationic mixture.
Under normal conditions, fabric softening agent or fabric softener add when the last rinsing of laundry cycles.This method will prevent cation activity thing from forming anionic-cationic mixture because the last time in rinsing the content of Anionic Active significantly reduce.The particulate with cation activity thing formed in detergent formulation 2 is under the main washing stage is the existence in Anionic Active, but it occurs in the comparatively latter stage of wash(ing)cycle from the release of formed particulate, and now the content of Anionic Active reduces.Therefore, the cation activity thing the same comparatively latter stage in wash(ing)cycle under normal conditions that coexists is introduced and is not formed anionic-cationic mixture.
Detergent formulation 3
This formula cationic active matter content is about 3%.The dosage of 3% cation activity thing is suitable with the median doses of fabrics in general tenderizer or softener.Due to the cation activity agent amount that it is higher, therefore its possibility forming anionic-cationic mixture in wash(ing)cycle is higher than detergent formulation 1 and 2.But any existence of anionic-cationic mixture is not shown through washing fabric.
Therefore, the present invention illustrates, can postpone the release of cation activity thing under dosage higher in detergent powder.

Claims (19)

1. a release particles, it comprises:
A) material to be released,
B) carrier, wherein said carrier is the hydrotropic agent for solid at 20 DEG C,
C) shell, it comprises the hydrophobic shell material that fusing point is 65 DEG C at the most, and
D) disintegrating agent material, it is included in described shell to make described shell disintegration after being immersed in the water.
2. release particles according to claim 1, the fusing point of wherein said hydrophobic shell material is 40 to 60 DEG C.
3. release particles according to claim 1, the total amount of wherein said material to be released is at most 40 % by weight of the total amount of described hydrotropic agent carrier.
4. release particles according to claim 1, the total amount of wherein said material to be released is 5 to 10 % by weight of the total amount of described hydrotropic agent carrier.
5. release particles according to claim 3, the ratio of the total amount of wherein said hydrophobic shell material described hydrotropic agent carrier relative to the total amount of described disintegrating agent material and described material to be released is at most 1: 1.
6. release particles according to claim 3, the ratio of the total amount of wherein said hydrophobic shell material described hydrotropic agent carrier relative to the total amount of described disintegrating agent material and described material to be released is 1: 9 to 2: 5.
7. release particles according to any one of claim 1 to 6, wherein said hydrotropic agent carrier to be selected from Phenylsulfonic acid, toluenesulphonic acids, xylene monosulfonic acid, isopropyl sulfonic acid, methyl isopropyl Phenylsulfonic acid, hydroxyl naphthoic acid, croceine acid, the salt of ethylhexyl sulfuric acid and these materials both or more the mixture of person.
8. release particles according to any one of claim 1 to 6, wherein said hydrotropic agent carrier is selected from the sodium salt of Phenylsulfonic acid, toluenesulphonic acids, xylene monosulfonic acid, isopropyl sulfonic acid, methyl isopropyl Phenylsulfonic acid, hydroxyl naphthoic acid, croceine acid, ethylhexyl sulfuric acid, and in these materials both or more the mixture of person.
9. release particles according to any one of claim 1 to 6, wherein said hydrotropic agent carrier is sodium xylene sulfonate and/or toluenesulfonic acid sodium salt.
10. release particles according to any one of claim 1 to 6, described disintegrating agent material is selected from nonionogenic tenside.
11. release particles according to any one of claim 1 to 6, described disintegrating agent material is selected from Soxylat A 25-7 and polyoxyethylene glycol.
12. release particles according to any one of claim 1 to 6, the molecular weight of described disintegrating agent material is at least 2000.
13. release particles according to any one of claim 1 to 6, wherein said hydrophobic shell material is selected from side chain or straight chain, saturated or undersaturated C15-C24
-lipid acid, and
-fatty alcohol, and
Their ester.
14. release particles according to any one of claim 1 to 6, wherein said material to be released is perfume compound.
15. 1 kinds of cleaning composition, it comprises washing composition and the release particles according to any one of claim 1 to 14.
16. cleaning composition according to claim 15, wherein said washing composition comprises anionic detergent.
17. 1 kinds of methods preparing the release particles according to any one of claim 1 to 14, said method comprising the steps of:
I () makes hydrotropic agent absorb material to be released to obtain slug particle,
(ii) heat and mix hydrophobic shell material and disintegrating agent material to obtain the coated mixture of liquid,
(iii) with the described slug particle of coated mixture encapsulation steps (i) of described liquid of step (ii) to obtain release particles.
18. methods according to claim 17, wherein in step (iii), have 100 DEG C at the most for the coated coated mixture of described liquid in step (iii).
19. methods according to claim 17, wherein in step (iii), have the temperature of 80 DEG C at the most for the coated coated mixture of described liquid in step (iii).
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DE102016219292A1 (en) * 2016-09-26 2018-03-29 Henkel Ag & Co. Kgaa Fast-dissolving, perfume-containing enamel body
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