Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/38—Products with no well-defined composition, e.g. natural products
  • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
  • C11D3/38672—Granulated or coated enzymes
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
  • C11D17/0013—Liquid compositions with insoluble particles in suspension
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/16—Organic compounds
  • C11D3/38—Products with no well-defined composition, e.g. natural products
  • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
  • C11D3/38618—Protease or amylase in liquid compositions only

Definitions

• the invention relates to an aqueous liquid washing and cleaning agent containing surfactant (s) and other conventional ingredients of detergents and cleaners.
• the invention also relates to processes for the preparation of an aqueous liquid detergent and cleaner and to its use.
• liquid detergents and cleaning agents which, even after storage and transport, develop optimally at the time of use. This implies that the ingredients of the liquid detergent and cleaning agent have previously neither sedimented, decomposed or volatilized.
• capsules that contain these ingredients.
• two types are distinguished. On the one hand, there are capsules with a core-shell structure in which the ingredient is surrounded by a wall or barrier. On the other hand, there are capsules in which the ingredient is distributed in a matrix of a matrix-forming material. Such capsules are also referred to as "speckles”.
• the EP 0 266 796 A1 describes a water-soluble microcapsule containing enzymes which can be stably suspended in a concentrated aqueous surfactant-containing solution and which dissolves on dilution with water.
• the water-soluble microcapsule has a coating of polyvinyl alcohol.
• the GB 1 390 503 A discloses aqueous liquid detergents containing capsules that are insoluble in the liquid detergent but release their entrapped contents as soon as the ionic strength decreases when diluted with water.
• the capsule preferably has a water-soluble coating of cellulose ether, polyacrylate, polyvinyl alcohol or polyethylene oxide.
• the GB 1 461 776 A describes aqueous liquid detergents containing capsules which dissolve when diluted with water.
• the capsules contain either hardened carrageenan or a modified pectin and a water-dispersible pigment.
• the WO 97/14780 describes encapsulated bleaches containing a coating of a gelled polymer material.
• the gelled polymer material is preferably an alginate.
• the WO 97/24178 describes particles having a polymeric matrix containing enzymes or other detergent-active agents, the matrix being formed from a copolymer.
• the matrix swells on contact with wash water and thus allows the release of the active ingredients.
• the particles additionally comprise a sheath of a polymeric material.
• capsules each comprising a hydrophilic core comprising an enzyme and a polymer and a shell prepared by interfacial polymerization.
• the US 6,242,406 B1 describes core-shell capsules in which a liquid detergent phase, an enzyme and a polymer are present in the core.
• the shell which is formed from a condensation polymer, is permeable to water and low molecular weight compounds.
• the DE 10205872 A1 describes a microcapsule for immobilizing solids, liquids and / or gases which has a core-shell structure. Inside the capsule, a phase boundary of two immiscible substances prevents diffusion of an active ingredient.
• EP 1 149 149 A1 discloses a detergent composition comprising a matrix-encapsulated active ingredient.
• the matrix of capsules contains a hydrated anionic gum and the encapsulated active ingredient is preferably a perfume.
• a disadvantage of such a capsule is that the active ingredient must be sufficiently large, ie have a high molecular weight, so that the active ingredient does not diffuse out of the capsule into the surrounding detergent and cleaner composition (so-called bleeding).
• small molecules can get into the cleaning fluid and there undesirable discoloration. Agglomerations, odor problems and destruction of active washing substances cause or even be destroyed.
• an aqueous liquid washing and cleaning agent containing surfactant (s) and other common ingredients of detergents and cleaners wherein the composition contains at least one capsule, the capsule comprises an active ingredient in a matrix, and the active ingredient is immobilized by attachment to a substrate specific for the active ingredient, and the active ingredient is selected from the group of enzymes and that the matrix is selected from a material selected from the group comprising carrageenan, alginate and gellan gum.
• the size and also the molecular weight of the active ingredient is increased, thus preventing bleeding or diffusing out of the active ingredient from the capsule in the surrounding detergent and cleaner composition or significantly minimized.
• an active ingredient is targeted and effectively immobilized.
• Enzymes can easily pass from the capsules to the surrounding detergent and cleaner composition. There, the enzymes can be destroyed, for example, by existing bleaching agents and are then in the actual washing process no longer or significantly reduced concentration available. This has a negative effect on the washing and cleaning performance.
• the enzyme form an enzyme-substrate complex with the substrate.
• Enzyme-substrate complexes are particularly stable and form very specific. By forming such an enzyme-substrate complex, a specific enzyme can be specifically and effectively immobilized as an active ingredient in a capsule.
• the enzyme is selected from the group of cellulases, proteases, amylases, and lipases.
• these enzymes provide an indispensable contribution to the washing and cleaning performance.
• Cellulases for example, degrade carbohydrate-containing impurities, while the proteases have the ability to degrade proteinaceous impurities or the lipases have fat-splitting activity.
• the amylases show activity in the breakdown of starch, glycogen and / or dextrin. The immobilization and thus stabilization of one or more sensitive enzymes in capsules is therefore particularly advantageous.
• a particularly preferred embodiment of the invention provides that the enzyme is a cellulase and the substrate is cellulose.
• the cellulase is a particularly important enzyme in detergents and cleaners, as it makes an important contribution to the secondary washing performance in addition to the degradation of carbohydrate-containing impurities, as it has an anti-redeposition effect as well as smoothing and color-refreshing effect on textiles.
• the substrate cellulose is specific for the cellulases and thus effectively immobilizes and stabilizes the cellulases used in the washing and cleaning agent.
• the capsule additionally contains at least one hollow microspheres.
• Hollow microspheres have a diameter of 2 to 500 ⁇ m, in particular of 5 to 20 ⁇ m, and a specific gravity of less than 1 g ⁇ cm -3 .
• the density of the capsules can be adjusted to the density of the surrounding detergent composition to prevent unwanted settling or floating (creaming) of the capsules.
• Carrageenan, alginate and gellan gum are particularly well crosslinked with cations to crosslinked insoluble gels. By dropping solutions of these materials into cation-containing solutions, spherical capsules containing a matrix can be prepared in a simple manner.
• the capsule additionally contains a filler. This is preferably selected from the group of silicic acids and aluminum silicates.
• the matrix is reinforced and thus obtain particularly robust capsules.
• the fillers in particular the silicas, in the actual washing process can improve the solubility of the capsules.
• the washing and cleaning agent contains dispersed capsules whose diameter along their largest spatial extent is 0.01 to 10,000 microns.
• a process for the preparation of an aqueous liquid detergent and cleaner containing surfactant (s) and other common ingredients of detergents and cleaners and at least one capsule wherein the capsule comprises an active ingredient in a matrix, wherein the active ingredient is bound to a substrate specific for the active ingredient and the active ingredient is selected from the group of enzymes and the matrix is selected from a material selected from the group comprising carrageenan, alginate and gellan gum.
• the invention also claims the use of a washing and cleaning agent according to the invention for cleaning textile fabrics.
• washing and cleaning agents according to the invention are described in detail below, inter alia, by way of examples.
• the detergents and cleaning agents according to the invention contain as a compulsory component at least one capsule comprising an active ingredient in a matrix, wherein the active ingredient is immobilized by attachment to a substrate.
• the matrix of the capsule comprises carrageenan, alginate or gellan gum. These materials can be crosslinked to insoluble gels using mono- or polyvalent cations.
• Alginate is a naturally occurring salt of alginic acid and is found in all brown algae (Phaeophycea) as a cell wall component.
• Alginates are acidic, carboxy group-containing polysaccharides having a relative molecular weight M R of about 200,000, consisting of D-mannuronic acid and L-guluronic acid in different ratios, which are linked to 1,4-glycosidic bonds.
• the sodium, potassium, ammonium and magnesium alginates are water-soluble.
• the viscosity of alginate solutions depends, inter alia, on the molecular weight and on the counterion.
• Calcium alginates form thermo-reversible gels, for example, in certain proportions.
• Sodium alginates give very viscous solutions with water and can be cross-linked by interaction with di- or trivalent metal ions such as Ca 2+ .
• Ingredients, which are also contained in the aqueous sodium alginate solution, are thus enclosed in an alginate matrix.
• Carrageenan is an extract of the red algae (Chondrus crispus and Gigartina stellata) that belongs to the Floridae . In the presence of K + ions or Ca 2+ ions, carrageenan crosslinks.
• Gellan gum is an unbranched anionic microbial heteroexopolysaccharide having a tetrasaccharide repeat unit consisting of the monomers glucose, glucuronic acid and rhamnose, wherein approximately each repeat unit is esterified with an L-glycerate and every other repeat unit is esterified with an acetate. Gellan gum cross-links in the presence of K + ions, Na + ions, Ca 2+ ions or Mg 2+ ions. Of the materials mentioned for the matrix, alginate is preferred.
• the amount of active ingredient in the aqueous alginate solution is preferably between 0.01 and 40 wt .-%, more preferably between 0.05 and 20 wt .-%, particularly preferably between 0.1 and 5 wt .-% and especially preferably between 0.5 and 1.5% by weight.
• the compounds used as the substrate have a high molecular weight.
• the substrate is specific to the active ingredient. It may be preferred that an enzyme-substrate complex is formed.
• cellulose can be used as a substrate.
• a protease is encapsulated, a protein is suitably used as a substrate.
• a lipase is to be present as an active ingredient in a capsule, it may be bound, for example, to a long-chain triglyceride as substrate.
• the amount of substrate in the aqueous alginate solution is preferably between 0.01 and 10 wt .-%, more preferably between 0.2 and 5 wt .-%, particularly preferably between 1 and 2 wt .-%.
• the capsules may additionally contain hollow microspheres.
• Hollow microspheres are particles having a diameter of 2 to 500 ⁇ m, in particular of 5 to 20 ⁇ m, and a specific gravity of less than 1 g ⁇ cm -3 . Conveniently, the hollow microspheres are round and smooth.
• the hollow microspheres may be made of inorganic material such as water glass, aluminum silicate, borosilicate glass soda lime glass or a ceramic or of organic polymers such as homo- or copolymers of styrene, acrylonitrile and vinylidene chloride.
• Suitable hollow microspheres are commercially available, for example, under the names Fillite® (ex Trelleborg Fillite), Expancel® (ex Akzo Nobel), Scotchlite® (ex 3M), Dualite® (es Sovereign Specialty Chemicals), Sphericel® (ex Potters Industries), Zeeospheres ® (ex 3M), Q-Cel® (ex PQ Corporation) or Extendospheres® (ex PQ Corporation). Further suitable hollow microspheres are available under the product name E-Spheres from OMEGA MINERALS. E-spheres are white, hollow ceramic microspheres, which are available in different grain sizes, particle size distributions, bulk densities and bulk volumes. Many of the hollow microspheres mentioned are chemically inert and are dispersed in the wash liquor after destruction of the capsule and then removed with it.
• the density of the capsules can be varied or adjusted by incorporating hollow microspheres become.
• the amount of hollow microspheres in a capsule depends on the desired density of the capsule. However, it is preferred that the amount of hollow microspheres in the aqueous alginate solution is preferably between 0 and 10% by weight, more preferably between 1 and 5% by weight, and most preferably between 2 and 4% by weight.
• the capins furthermore may also contain fillers, such as preferably silicic acids or aluminum silicates, in particular zeolites.
• fillers such as preferably silicic acids or aluminum silicates, in particular zeolites.
• Silicas that are suitable as fillers are commercially available under the name Aerosil® or Sipernat® (both ex Degussa).
• Other suitable fillers are aluminum silicates and in particular zeolites.
• Suitable zeolites include, for example, commercial products such as Wessalith® (ex Degussa), zeolite MAP® (ex Crosfield) or VEGOBOND AX® (ex SASOL).
• the amount of filler in the aqueous alginate solution is preferably between 0 and 20 wt .-%, more preferably between 1 and 10 wt .-% and particularly preferably between 2 and 10 wt .-%.
• the fillers on the one hand give the capsules a robust structure and thus have a positive effect on the stability of the capsules.
• the fillers, in particular the silicas, in the actual washing process can improve the solubility of the capsules.
• the capsules may have any shape in the production-related framework, but they are preferably approximately spherical. Their diameter along their largest spatial extent, depending on the components contained in their interior and the application between 0.01 microns (not visually recognizable as a capsule) and 10,000 microns. Preferred are visible microcapsules with a diameter in the range of 100 microns to 7,000 microns, in particular from 400 microns to 5,000 microns.
• the capsule may be colored.
• the capsule may contain one or more coloring agents such as a pigment or a dye. It may also be preferred that the capsule contains a preservative.
• an aqueous alginate solution which also contains the active ingredient to be enclosed or the active ingredient to be included and the substrate and optionally other components such as filler (s), hollow microspheres, preservatives and coloring agents is preferably dripped and then hardened in a precipitation bath containing Ca 2+ ions. It is most preferred that first the active ingredient (s) and respective substrate be contacted before the aqueous alginate solution is prepared so as to ensure that the active ingredient is bound to the substrate.
• the preparation of the alginate capsules can be done for example by means of a Vetropfungsanlange the company Rieter Automatik GmbH.
• the dripping of the aqueous alginate solution which contains the active ingredient to be enclosed and the substrate and, if appropriate, filler (s), hollow microspheres, preservatives and coloring agents is effected by impressing a vibration which is generated by means of an oscillating membrane.
• the droplet break is due to the increased shear when swinging back the membrane.
• the dropping itself can be done for example by a single nozzle or through a nozzle plate with 10 to 500, preferably 50 to 100 openings.
• the nozzles preferably have openings with a diameter in the range of 0.2 to 2, preferably 0.3 to 0.8 mm.
• the dripping can be carried out in a precipitation bath, which is designed as a stirred tank or boiler.
• a precipitation bath which is designed as a stirred tank or boiler.
• capsules and the enclosed active ingredient can be destroyed again, since the stirring process by introducing energy also leads to an undesirable increase in temperature.
• drop plants may be used which differ by different droplet formation technologies.
• plants belonging to Gouda, Cavis or GeniaLab may be mentioned here.
• the amount of alginate in the aqueous alginate solution is preferably between 0.01 and 10 wt .-%, particularly preferably between 0.1 and 5 wt .-% and particularly preferably between 1 and 3 wt .-%.
• sodium alginate is used.
• the alginate-based capsules are subsequently washed with water and then washed in an aqueous solution with a complexing agent, such as Dequest, to free Ca 2+ ions, which have undesirable interactions with ingredients of the liquid washing and preserving agents Detergent, such as the fatty acid soaps, can enter, wash out. Subsequently, the alginate-based capsules are again washed with water to remove excess complexing agent.
• a complexing agent such as Dequest
• the capsules can be dried before use in a detergent and cleaning agent, but they are preferably used moist.
• the release of the active ingredient from the capsules is usually during the application of the they contain agents by destruction of the matrix due to mechanical, thermal, chemical or enzymatic action.
• the liquid detergents and cleaners contain identical or different capsules in amounts of from 0.01 to 10% by weight, in particular from 0.2 to 8% by weight and very preferably from 0.5 to 5% by weight. -%.
• the liquid detergents and cleaners contain surfactant (s), wherein anionic, nonionic, cationic and / or amphoteric surfactants can be used. From an application point of view, preference is given to mixtures of anionic and nonionic surfactants.
• the total surfactant content of the liquid washing and cleaning agent is preferably below 40% by weight and more preferably below 35% by weight, based on the total liquid detergent and cleaning agent.
• the nonionic surfactants used are preferably alkoxylated, advantageously ethoxylated, in particular primary, alcohols having preferably 8 to 18 carbon atoms and on average 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, in which the alcohol radical can be linear or preferably methyl-branched in the 2-position or linear and methyl-branched radicals in the mixture can contain, as they are usually present in Oxoalkoholresten.
• alcohol ethoxylates with linear radicals of alcohols of native origin having 12 to 18 carbon atoms, for example of coconut, palm, tallow or oleyl alcohol, and on average 2 to 8 EO per mole of alcohol are preferred.
• the preferred ethoxylated alcohols include, for example, C 12-14 alcohols with 3 EO, 4 EO or 7 EO, C 911 alcohols with 7 EO, C 13-15 alcohols with 3 EO, 5 EO, 7 EO or 8 EO, C 12-18 alcohols with 3 EO, 5 EO or 7 EO and mixtures of these, such as mixtures of C 12-14 -alcohol with 3 EO and C 12-18 -alcohol with 7 EO.
• the degrees of ethoxylation given represent statistical means which, for a particular product, may be an integer or a fractional number.
• Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, NRE).
• fatty alcohols with more than 12 EO can also be used. Examples include tallow fatty alcohol with 14 EO, 25 EO, 30 EO or 40 EO.
• Nonionic surfactants containing EO and PO groups together in the molecule can also be used according to the invention.
• block copolymers with EO-PO block units or PO-EO block units can be used, but also EO-PO-EO copolymers or PO-EO-PO copolymers.
• nonionic surfactants and alkyl glycosides of the general formula RO (G) x can be used in which R is a primary straight-chain or methyl-branched, especially in the 2-position methyl-branched aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms and G is the symbol which represents a glycose unit having 5 or 6 C atoms, preferably glucose.
• the degree of oligomerization x which indicates the distribution of monoglycosides and oligoglycosides, is any number between 1 and 10; preferably x is 1.2 to 1.4.
• nonionic surfactants used either as the sole nonionic surfactant or in combination with other nonionic surfactants are alkoxylated, preferably ethoxylated or ethoxylated and propoxylated fatty acid alkyl esters, preferably having from 1 to 4 carbon atoms in the alkyl chain, especially fatty acid methyl esters as they are
• alkoxylated preferably ethoxylated or ethoxylated and propoxylated fatty acid alkyl esters, preferably having from 1 to 4 carbon atoms in the alkyl chain, especially fatty acid methyl esters as they are
• JP 58/217598 are described or preferably according to the in the international patent application WO 90/13533 be prepared described methods.
• Nonionic surfactants of the amine oxide type for example N-cocoalkyl-N, N-dimethylamine oxide and N-tallowalkyl-N, N-dihydroxyethylamine oxide, and the fatty acid alkanolamides may also be suitable.
• the amount of these nonionic surfactants is preferably not more than that of the ethoxylated fatty alcohols, especially not more than half thereof.
• polyhydroxy fatty acid amides of the formula (2) wherein RCO is an aliphatic acyl group having 6 to 22 carbon atoms, R 1 is hydrogen, an alkyl or hydroxyalkyl group having 1 to 4 carbon atoms and [Z] is a linear or branched polyhydroxyalkyl group having 3 to 10 carbon atoms and 3 to 10 hydroxyl groups.
• the polyhydroxy fatty acid amides are known substances which can usually be obtained by reductive amination of a reducing sugar with ammonia, an alkylamine or an alkanolamine and subsequent acylation with a fatty acid, a fatty acid alkyl ester or a fatty acid chloride.
• the group of polyhydroxy fatty acid amides also includes compounds of the formula (3), in the R is a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms, R 1 is a linear, branched or cyclic alkyl radical or an aryl radical having 2 to 8 carbon atoms and R 2 is a linear, branched or cyclic alkyl radical or an aryl radical or an oxyalkyl radical having 1 to 8 carbon atoms, with C 1-4 alkyl or phenyl radicals being preferred and [Z] being a linear polyhydroxyalkyl radical whose alkyl chain is substituted by at least two hydroxyl groups, or alkoxylated, preferably ethoxylated or propoxylated Derivatives of this residue.
• R is a linear or branched alkyl or alkenyl radical having 7 to 12 carbon atoms
• R 1 is a linear, branched or cyclic alkyl radical or an aryl radical having 2
• [Z] is preferably obtained by reductive amination of a sugar, for example glucose, fructose, maltose, lactose, galactose, mannose or xylose.
• a sugar for example glucose, fructose, maltose, lactose, galactose, mannose or xylose.
• the N-alkoxy- or N-aryloxy-substituted compounds can then, for example, according to the teaching of the international application WO-A-95/07331 be converted by conversion with fatty acid methyl esters in the presence of an alkoxide as catalyst into the desired Polyhydroxyfettklaamide.
• the content of nonionic surfactants is the liquid detergents and cleaners preferably 5 to 30 wt .-%, preferably 7 to 20 wt .-% and in particular 9 to 15 wt .-%, each based on the total agent.
• anionic surfactants for example, those of the sulfonate type and sulfates are used.
• the surfactants of the sulfonate type are preferably C 9-13 -alkylbenzenesulfonates, olefinsulfonates, ie mixtures of alkene and hydroxyalkanesulfonates and disulfonates, as are obtained, for example, from C 12-18 -monoolefins having terminal or internal double bonds by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acid hydrolysis of the sulfonation products into consideration.
• alkanesulfonates which are obtained from C 12-18 alkanes, for example by sulfochlorination or sulfoxidation with subsequent hydrolysis or neutralization.
• esters of ⁇ -sulfo fatty acids for example the ⁇ -sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids.
• sulfated fatty acid glycerol esters are to be understood as meaning the mono-, di- and triesters and mixtures thereof, as obtained in the preparation by esterification of a monoglycerol with 1 to 3 moles of fatty acid or in the transesterification of triglycerides with 0.3 to 2 moles of glycerol.
• Preferred sulfated fatty acid glycerol esters are the sulfonation products of saturated fatty acids having 6 to 22 carbon atoms, for example caproic acid, caprylic acid, capric acid, myristic acid, lauric acid, palmitic acid, stearic acid or behenic acid.
• Alk (en) ylsulfates are the alkali metal salts and in particular the sodium salts of the sulfuric monoesters of C 12 -C 18 fatty alcohols, for example coconut fatty alcohol, tallow fatty alcohol, lauryl, myristyl, cetyl or stearyl alcohol or the C 10 -C 20 oxo alcohols and those half-esters of secondary alcohols of these chain lengths are preferred. Also preferred are alk (en) ylsulfates of said chain length, which contain a synthetic, produced on a petrochemical basis straight-chain alkyl radical, which have an analogous degradation behavior as the adequate compounds based on oleochemical raw materials.
• C 12 -C 16 alkyl sulfates and C 12 -C 15 alkyl sulfates and C 14 -C 15 alkyl sulfates are preferred.
• 2,3-alkyl sulfates which, for example, according to the U.S. Patents 3,234,258 or 5,075,041 which can be obtained as commercial products of the Shell Oil Company under the name DAN® are suitable anionic surfactants.
• EO ethylene oxide
• Fatty alcohols with 1 to 4 EO are suitable. Due to their high foaming behavior, they are only used in detergents in relatively small amounts, for example in amounts of from 1 to 5% by weight.
• Suitable anionic surfactants are also the salts of alkylsulfosuccinic acid, which are also referred to as sulfosuccinates or as sulfosuccinic acid esters and the monoesters and / or diesters of sulfosuccinic acid with alcohols, preferably fatty alcohols and in particular ethoxylated fatty alcohols.
• alcohols preferably fatty alcohols and in particular ethoxylated fatty alcohols.
• Preferred sulfosuccinates contain C 8-18 fatty alcohol residues or mixtures of these.
• Particularly preferred sulfosuccinates contain a fatty alcohol residue derived from ethoxylated fatty alcohols, which in themselves constitute nonionic surfactants (see description below).
• Sulfosuccinates whose fatty alcohol residues are derived from ethoxylated fatty alcohols with a narrow homolog distribution, are again particularly preferred.
• alk (en) yl-succinic acid having preferably 8 to 18 carbon atoms in the alk (en) yl chain or salts thereof.
• Particularly preferred anionic surfactants are soaps.
• Suitable are saturated and unsaturated fatty acid soaps, such as the salts of lauric acid, myristic acid, palmitic acid, stearic acid, (hydrogenated) erucic acid and behenic acid and, in particular, soap mixtures derived from natural fatty acids, for example coconut, palm kernel, olive oil or tallow fatty acids.
• the anionic surfactants may be in the form of their sodium, potassium or ammonium salts and as soluble salts of organic bases, such as mono-, di- or triethanolamine.
• the anionic surfactants are preferably present in the form of their sodium or potassium salts, in particular in the form of the sodium salts.
• the content of preferred liquid detergents and cleaners to anionic surfactants is 2 to 30 wt .-%, preferably 4 to 25 wt .-% and in particular 5 to 22 wt .-%, each based on the total agent.
• the viscosity of the liquid detergents and cleaning agents can be measured by conventional standard methods (for example Brookfield LVT-II viscosimeter at 20 rpm and 20 ° C., spindle 3) and is preferably in the range from 500 to 5000 mPas.
• Preferred agents have viscosities from 700 to 4000 mPas, with values between 1000 and 3000 mPas being particularly preferred.
• the liquid detergents and cleaning agents may contain further ingredients which further improve the performance and / or aesthetic properties of the liquid detergent and cleaning agent.
• preferred agents additionally comprise the capsules and to the surfactant (s) one or more substances from the group of builders, bleaches, bleach activators, enzymes, electrolytes, nonaqueous solvents, pH adjusters, fragrances, perfume carriers, fluorescers, dyes , Hydrotropes, foam inhibitors, silicone oils, anti redeposition agents, optical brighteners, grayness inhibitors, anti-shrinkage agents, anti-crease agents, color transfer inhibitors, antimicrobial agents, germicides, fungicides, antioxidants, corrosion inhibitors, antistatic agents, ironing aids, repellents and impregnating agents, swelling and anti-slip agents and UV absorbers.
• Suitable builders which may be present in the liquid detergents and cleaners are, in particular, silicates, aluminum silicates (in particular zeolites), carbonates, salts of organic di- and polycarboxylic acids and mixtures of these substances.
• Suitable crystalline layered sodium silicates have the general formula NaMSi x O 2x + 1 .H 2 O, where M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20 and preferred values for x 2, 3 or 4 are.
• Such crystalline sheet silicates are described, for example, in the European patent application EP-A-0 164 514 described.
• Preferred crystalline layered silicates of the formula given are those in which M is sodium and x assumes the values 2 or 3.
• both .beta.- and ⁇ -sodium Na 2 Si 2 O 5 ⁇ yH 2 O are preferred, with ⁇ -sodium disilicate being obtainable, for example, by the method described in the international patent application WO-A-91/08171 is described.
• amorphous sodium silicates with a Na 2 O: SiO 2 modulus of from 1: 2 to 1: 3.3, preferably from 1: 2 to 1: 2.8 and in particular from 1: 2 to 1: 2.6, which Delayed and have secondary washing properties.
• the dissolution delay compared to conventional amorphous sodium silicates may have been caused in various ways, for example by surface treatment, compounding, compaction / densification or by overdrying.
• the term "amorphous” is also understood to mean "X-ray amorphous”.
• the silicates do not yield sharp X-ray reflections typical of crystalline substances in X-ray diffraction experiments, but at most one or more maxima of the scattered X-rays which have a width of several degrees of diffraction angle. However, it may well even lead to particularly good builder properties if the silicate particles provide blurred or even sharp diffraction maxima in electron diffraction experiments. This is to be interpreted as meaning that the products have microcrystalline regions of size 10 to a few hundred nm, with values of up to a maximum of 50 nm and in particular up to a maximum of 20 nm being preferred.
• Such so-called X-ray amorphous silicates which likewise have a dissolution delay compared to the conventional water glasses, are described, for example, in the German patent application DE-A-44 00 024 described.
• Particularly preferred are compacted / compacted amorphous silicates, compounded amorphous silicates and overdried X-ray amorphous silicates.
• the finely crystalline, synthetic and bound water-containing zeolite used is preferably zeolite A and / or P.
• zeolite P zeolite MAP® (commercial product from Crosfield) is particularly preferred.
• zeolite X and mixtures of A, X and / or P are particularly preferred.
• the zeolite can be used as a spray-dried powder or else as undried, still moist, stabilized suspension of its preparation.
• the zeolite may contain minor additions of nonionic surfactants as stabilizers, for example 1 to 3 wt .-%, based on zeolite, of ethoxylated C 12 -C 18 fatty alcohols having 2 to 5 ethylene oxide groups .
• Suitable zeolites have an average particle size of less than 10 ⁇ m (volume distribution, measuring method: Coulter Counter) and preferably contain 18 to 22% by weight, in particular 20 to 22% by weight, of bound water.
• phosphates as builders are possible, unless such use should not be avoided for environmental reasons.
• sodium perborate tetrahydrate and sodium perborate monohydrate are of particular importance.
• Other useful bleaching agents are, for example, sodium percarbonate, peroxypyrophosphates, citrate perhydrates and H 2 O 2 -producing peracidic salts or peracids, such as perbenzoates, peroxophthalates, diperazelaic acid, phthaloiminoperacid or diperdodecanedioic acid.
• bleach activators can be incorporated into the detergents and cleaners.
• bleach activators it is possible to use compounds which, under perhydrolysis conditions, give aliphatic peroxycarboxylic acids having preferably 1 to 10 C atoms, in particular 2 to 4 C atoms, and / or optionally substituted perbenzoic acid.
• Suitable substances are those which carry O- and / or N-acyl groups of the stated C atom number and / or optionally substituted benzoyl groups.
• polyacylated alkylenediamines in particular tetraacetylethylenediamine (TAED), acylated triazine derivatives, in particular 1,5-diacetyl-2,4-dioxohexahydro-1,3,5-triazine (DADHT), acylated glycolurils, in particular tetraacetylglycoluril (TAGU), N- Acylimides, in particular N-nonanoylsuccinimide (NOSI), acylated phenolsulfonates, in particular n-nonanoyl or isononanoyloxybenzenesulfonate (n- or iso-NOBS), carboxylic anhydrides, in particular phthalic anhydride, acylated polyhydric alcohols, in particular triacetin, ethylene glycol diacetate and 2, 5-diacetoxy- 2,5-dihydrofuran.
• TAED tetraacety
• bleach catalysts can also be incorporated into the liquid detergents and cleaners.
• These substances are bleach-enhancing transition metal salts or transition metal complexes such as Mn, Fe, Co, Ru or Mo saline complexes or carbonyl complexes.
• Mn, Fe, Co, Ru, Mo, Ti, V and Cu complexes with nitrogen-containing tripod ligands and Co, Fe, Cu and Ru ammine complexes can also be used as bleach catalysts.
• the liquid detergent and cleaning agent preferably contains a thickener.
• the thickener may include, for example, a polyacrylate thickener, xanthan gum, gellan gum, guar gum, alginate, carrageenan, carboxymethyl cellulose, bentonites, wellan gum, locust bean gum, agar-agar, tragacanth, gum arabic, pectins, polyoses, starch, dextrins, gelatin and casein include.
• modified natural substances such as modified starches and celluloses, examples which may be mentioned here include carboxymethylcellulose and other cellulose ethers, hydroxyethyl and -propylcellulose and core flour ethers, can be used as thickeners.
• the polyacrylic and polymethacrylic thickeners include, for example, the high molecular weight homopolymers of acrylic acid crosslinked with a polyalkenyl polyether, in particular an allyl ether of sucrose, pentaerythritol or propylene (INCI name according to "International Dictionary of Cosmetic Ingingients” of "The Cosmetic, Toiletry and Fragrance Association (CTFA) ": carbomer), also referred to as carboxyvinyl polymers.
• CTF Cosmetic, Toiletry and Fragrance Association
• Such polyacrylic acids are available, inter alia, from 3V Sigma under the trade name Polygel®, for example Polygel DA, and from BF Goodrich under the trade name Carbopol®, for example Carbopol 940 (molecular weight about 4,000,000), Carbopol 941 (molecular weight about 250,000) or Carbopol 934 (molecular weight about 3,000,000).
• acrylic acid copolymers are included: (i) Copolymers of two or more monomers from the group of acrylic acid, methacrylic acid and their simple ester, preferably formed with C 1-4 -alkanols (INCI acrylates copolymer), such as the copolymers of methacrylic acid, butyl acrylate and methyl methacrylate (CAS designation according to Chemical Abstracts Service: 25035-69-2 ) or of butyl acrylate and methyl methacrylate ( CAS 25852-37-3 ) and which are available, for example, from Rohm & Haas under the trade names Aculyn® and Acusol® and from Degussa (Goldschmidt) under the trade name Tego® Polymer, for example the anionic non-associative polymers Aculyn 22, Aculyn 28, Aculyn 33 (cross-linked), Acusol 810, Acusol 820, Acusol 823 and Acusol 830 ( CAS 25852-37-3
• Carbopol® eg the hydrophobic Carbopol ETD 2623 and Carbopol 1382 (INCI Acrylates / C 10 -30 alkyl acrylate crosspolymer) and Carbopol Aqua 30 (former Carbopol EX 473).
• xanthan gum a microbial anionic heteropolysaccharide produced by Xanthomonas campestris and some other species under aerobic conditions and having a molecular weight of from 2 to 15 million daltons.
• Xanthan is formed from a chain of ⁇ -1,4-linked glucose (cellulose) with side chains.
• the structure of the subgroups consists of glucose, mannose, glucuronic acid, acetate and pyruvate, the number of pyruvate units determining the viscosity of the xanthan gum.
• Xanthan gum can be described by the following formula (1):
• Xanthan gum is available, for example, from Kelco under the trade names Keltrol® and Kelzan® or also from Rhodia under the trade name Rhodopol®.
• Preferred aqueous liquid detergents and cleaners contain, based on the total agent, from 0.01 to 1% by weight and preferably from 0.1 to 0.5% by weight of thickener.
• the aqueous liquid detergents and cleaners contain enzymes in encapsulated form and may also contain them directly in the detergent composition.
• enzymes are in particular those from the classes of hydrolases such as proteases, esterases, lipases or lipolytic enzymes, amylases, cellulases or other Glykosylhydrolasen and mixtures of said enzymes in question. All of these hydrolases in the wash contribute to the removal of stains such as proteinaceous, greasy or starchy stains and graying.
• cellulases and other glycosyl hydrolases may contribute to color retention and to enhancing the softness of the fabric by removing pilling and microfibrils. Oxireductases can also be used for bleaching or inhibiting color transfer.
• Bacillus subtilis Bacillus licheniformis, Streptomyceus griseus and Humicola insolens derived enzymatic agents.
• Bacillus subtilis Bacillus subtilis
• Bacillus licheniformis Bacillus licheniformis
• Streptomyceus griseus and Humicola insolens derived enzymatic agents.
• subtilisin-type proteases and in particular proteases derived from Bacillus lentus are used.
• enzyme mixtures for example from protease and amylase or protease and lipase or lipolytic enzymes or protease and cellulase or from cellulase and lipase or lipolytic enzymes or from protease, amylase and lipase or lipolytic enzymes or protease, lipase or lipolytic enzymes and cellulase, but in particular protease and / or lipase-containing mixtures or mixtures with lipolytic enzymes of particular interest.
• lipolytic enzymes are the known cutinases. Peroxidases or oxidases have also proved suitable in some cases.
• Suitable amylases include in particular ⁇ -amylases, iso-amylases, pullulanases and pectinases.
• Cellulases used are preferably cellobiohydrolases, endeglucanases and .beta.-glucosidases, which are also known as gellobias, or mixtures thereof. Since different cellulase types differ by their CMCase and avicelase activities, the desired activities can be set by targeted mixtures of the cellulases.
• the enzymes may be adsorbed to carriers to protect against premature degradation.
• the proportion of enzymes, enzyme mixtures or enzyme granules directly in the detergent composition may be, for example, about 0.1 to 5% by weight, preferably 0.12 to about 2.5% by weight.
• electrolytes from the group of inorganic salts a wide number of different salts can be used.
• Preferred cations are the alkali and alkaline earth metals, preferred anions are the halides and sulfates. From a manufacturing point of view, the use of NaCl or MgCl 2 in the compositions is preferred.
• the proportion of electrolytes in the agents is usually 0.5 to 5 wt .-%.
• Non-aqueous solvents that can be used in the liquid detergents and cleaners, for example, from the group of monohydric or polyhydric alcohols, Alkanalamine or glycol ethers, provided they are miscible in the specified concentration range with water.
• the solvents are preferably selected from ethanol, n- or i-propanol, butanols, glycol, propane or butanediol, glycerol, diglycol, propyl- or butyldiglycol, Hexylene glycol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol propyl ether, ethylene glycol mono-n-butyl ether, diethylene glycol methyl ether, diethylene glycol ethyl ether, propylene glycol methyl, ethyl or propyl ether, dipropylene glycol monomethyl or ethyl ether, di-isopropylene glycol monomethyl or ethy
• pH adjusters In order to bring the pH of the liquid detergents and cleaners into the desired range, the use of pH adjusters may be indicated. Can be used here are all known acids or alkalis, unless their use is not for technical application or environmental reasons or for reasons of consumer protection prohibited. Usually, the amount of these adjusting agents does not exceed 7% by weight of the total formulation.
• dyes In order to improve the aesthetic impression of the liquid washing and cleaning agents, they can be dyed with suitable dyes.
• Preferred dyes the selection of which presents no difficulty to the skilled person, have a high storage stability and insensitivity to the other ingredients of the agents and to light and no pronounced substantivity to textile fibers so as not to stain them.
• Suitable foam inhibitors which can be used in the liquid detergents and cleaners are, for example, soaps, paraffins or silicone oils, which may optionally be applied to support materials.
• Suitable anti-redeposition agents which are also referred to as "soil repellents" are, for example, nonionic cellulose ethers such as methylcellulose and methylhydroxypropylcellulose with a proportion of methoxy groups of 15 to 30% by weight and of hydroxypropyl groups of 1 to 15% by weight, based in each case on nonionic cellulose ethers and the known from the prior art polymers of phthalic acid and / or terephthalic acid or derivatives thereof, in particular polymers of ethylene terephthalates and / or polyethylene glycol terephthalates or anionic and / or nonionic modified derivatives thereof.
• Especially preferred of these are the sulfonated derivatives of the phthalic and terephthalic acid polymers.
• Optical brighteners can be added to the liquid detergents and cleaning agents in order to eliminate graying and yellowing of the treated textile fabrics. These fabrics impinge on the fiber and cause whitening and bleaching by transforming invisible ultraviolet radiation into visible longer wavelength light, emitting the ultraviolet light absorbed from the sunlight as faint bluish fluorescence, and pure with the yellowness of the grayed or yellowed wash White results.
• Suitable compounds are derived, for example, from the substance classes of 4,4'-diamino-2,2'-stilbenedisulfonic acids (flavonic acids), 4,4'-distyrylbiphenyls, methylumbelliferones, coumarins, dihydroquinolinones, 1,3-diarylpyrazolines, naphthalimides, benzoxazole , Benzisoxazole and benzimidazole systems as well as heterocyclic substituted pyrene derivatives.
• the optical brighteners are usually used in amounts of between 0.03 and 0.3 wt .-%, based on the finished composition.
• Grayness inhibitors have the task of keeping the dirt detached from the fiber suspended in the liquor and thus preventing the dirt from being rebuilt.
• Water-soluble colloids of mostly organic nature are suitable for this purpose, for example glue, gelatine, salts of ether sulfonic acids or cellulose or salts of acidic sulfuric acid esters of cellulose or starch.
• water-soluble polyamides containing acidic groups are suitable for this purpose. It is also possible to use soluble starch preparations and starch products other than those mentioned above, for example degraded starch, aldehyde starches, etc. Polyvinylpyrrolidone is also useful.
• cellulose ethers such as carboxymethylcellulose (Na salt), methylcellulose, hydroxyalkylcellulose and mixed ethers such as methylhydroxyethylcellulose, methylhydroxypropylcellulose, methylcarboxymethylcellulose and mixtures thereof in amounts of from 0.1 to 5% by weight, based on the compositions.
• the compositions may contain synthetic crease inhibitors.
• the liquid detergents and cleaning agents may contain antimicrobial agents.
• antimicrobial agents Depending on the antimicrobial spectrum and mechanism of action, a distinction is made between bacteriostats and bactericides, fungistatics and fungicides, etc.
• Important substances from these groups are, for example, benzalkonium chlorides, alkylarylsulfonates, halophenols and phenolmercuric acetate, and the compounds according to the invention can be completely dispensed with.
• the agents may contain antioxidants.
• This class of compounds includes, for example, substituted phenols, hydroquinones, catechols and aromatic amines, as well as organic sulfides, polysulfides, dithiocarbamates, phosphites and phosphonates.
• Antistatic agents increase the surface conductivity and thus allow an improved drainage of formed charges.
• External antistatic agents are generally substances with at least one hydrophilic molecule ligand and give a more or less hygroscopic film on the surfaces. These mostly surface-active antistatic agents can be subdivided into nitrogen-containing (amines, amides, quaternary ammonium compounds), phosphorus-containing (phosphoric acid esters) and sulfur-containing (alkyl sulfonates, alkyl sulfates) antistatic agents.
• External antistatics are for example in the patent applications FR 1,156,513 . GB 873 214 and GB 839,407 described.
• the lauryl (or stearyl) -dimethylbenzylammonium chlorides disclosed herein are useful as antistatics for textile fabrics or as an additive to laundry detergents, with a softening effect being additionally achieved.
• silicone derivatives can be used in the liquid detergents and cleaners. These additionally improve the rinsing behavior of the agents by their foam-inhibiting properties.
• Preferred silicone derivatives are, for example, polydialkyl or alkylaryl siloxanes in which the alkyl groups have one to five carbon atoms and are completely or partially fluorinated.
• Preferred silicones are polydimethylsiloxanes, which may optionally be derivatized and are then amino-functional or quaternized or have Si-OH, Si-H and / or Si-Cl bonds.
• the viscosities of the preferred silicones are in the range between 100 and 100,000 mPas at 25 ° C, wherein the silicones in amounts between 0.2 and 5 wt .-%, based on the total agent can be used.
• the liquid detergents and cleaners may also contain UV absorbers that wick onto the treated fabrics and improve the lightfastness of the fibers.
• Compounds having these desired properties include, for example, the non-radiative deactivating compounds and derivatives of benzophenone having substituents in the 2- and / or 4-position. Also suitable are substituted benzotriazoles, phenyl-substituted acrylates (cinnamic acid derivatives) in the 3-position, optionally with cyano groups in the 2-position, salicylates, organic Ni complexes and natural substances such as umbelliferone and the body's own urocanic acid.
• Suitable heavy metal complexing agents are, for example, the alkali metal salts of ethylenediaminetetraacetic acid (EDTA) or nitrilotriacetic acid (NTA) and alkali metal salts of anionic polyelectrolytes such as polymaleates and polysulfonates.
• EDTA ethylenediaminetetraacetic acid
• NTA nitrilotriacetic acid
• anionic polyelectrolytes such as polymaleates and polysulfonates.
• a preferred class of complexing agents are the phosphonates, which in preferred liquid detergents and cleaners in amounts of from 0.01 to 2.5 wt .-%, preferably 0.02 to 2 wt .-% and in particular from 0.03 to 1 , 5 wt .-% are included.
• These preferred compounds include in particular organophosphonates such as 1-hydroxyethane-1,1-diphosphonic acid (HEDP), aminotri (methylenephosphonic acid) (ATMP), diethylenetriamine penta (methylenephosphonic acid) (DTPMP or DETPMP) and 2-phosphonobutane-1,2 , 4-tricarboxylic acid (PBS-AM), which are used mostly in the form of their ammonium or alkali metal salts.
• organophosphonates such as 1-hydroxyethane-1,1-diphosphonic acid (HEDP), aminotri (methylenephosphonic acid) (ATMP), diethylenetriamine penta (methylenephosphonic acid) (DTPMP or DETPMP) and 2-phospho
• the resulting aqueous liquid detergents and cleaners are preferably clear, ie they have no sediment and are particularly preferably transparent or at least translucent.
• the detergents and cleaning agents according to the invention can be used for cleaning textile surface fabrics.
• gellan gum is first added to water and allowed to swell at 80.degree. Subsequently, a small amount of a saline solution, preferably with trivalent or divalent metal cations such as Al 3+ or Ca 2+ , is added. In the next step, the acidic components such as the linear alkyl sulfonates, citric acid, boric acid, phosphonic acid, the fatty alcohol ether sulfates, etc., and the nonionic surfactants are added. Subsequently, a base such as NaOH, KOH, triethanolamine or monoethanolamine is added followed by the fatty acid, if any.
• a base such as NaOH, KOH, triethanolamine or monoethanolamine is added followed by the fatty acid, if any.
• the remaining ingredients and the solvents of the aqueous liquid detergent and cleaning agent and, if present, the polyacrylate thickener are added to the mixture and the pH adjusted to about 8.5.
• the particles to be dispersed can be added and distributed homogeneously in the aqueous liquid washing and cleaning agent by stirring and / or mixing.
• liquid detergents and cleaners without gellan gum by conventional methods and methods in which, for example, the ingredients are simply mixed in stirred tanks, water, non-aqueous solvent and surfactant (s) are conveniently presented and the other ingredients are added in portions , Separate heating in the preparation is not required, if desired, the temperature of the mixture should not exceed 80 ° C.
• the capsules can be stably dispersed in the aqueous liquid detergent and cleaner, for example.
• Stable means that the compositions are stable at room temperature and at 40 ° C for a period of at least 4 weeks, and preferably at least 6 weeks, without the medium creaming or sedimenting.
• the respective alginate solutions had the compositions given in Table 1 (in% by weight).
• the hardening bath used contained 2.5% by weight CaCl 2 0.2% by weight of polydiallyldimethylammonium chloride 0.05% by weight preservative and to 100% by weight of water.
• the obtained capsules K1 to K6 were washed several times with water and a complexing agent such as Dequest®.
• capsules K1 and K2 were then stored for 2 weeks at room temperature in water. Subsequent enzyme analysis of capsules K1 and K2 and the surrounding solution gave the following values: sample Cellulase activity [mU / g] Content of cellulase [%] Capsule K1 105.0 0.39 Capsule K2 89.5 0.33 Storage solution of K1 3.5 0.01 Storage solution from K2 2.9 0.01
• capsules were prepared analogously with the compositions according to Table 1 but without cellulose and stored in water at room temperature. After a short storage time, there was just as much enzyme in the storage solution as in the capsule itself.
• the capsules according to the invention can be stably dispersed in aqueous liquid detergents and cleaners of various compositions.
• Stable means that the compositions are stable at room temperature and at 40 ° C for a period of at least 4 weeks, and preferably at least 6 weeks, without the medium creaming or sedimenting.
• Table 2 shows washing and cleaning agents E1 to E4 according to the invention.
• the washing and cleaning agents E1 to E4 obtained had a viscosity of around 1,000 mPas.
• the pH of the liquid detergents and cleaners was 8.5.
• Capsules K7 were prepared with alginate as a matrix material in a hardening bath (composition as in Example 1) by means of a Rieter drip system or vetropft.
• the alginate solution had the composition given in Table 3 (in% by weight).
• Table 3 K7 Na alginate 1 Aerosil 200 - Sipernat 22S 3 Hollow microspheres 1 3 preservative 0.05 dye 0.1 Termamyl 300 LDX 1 corn starch 2.5 water
• the resulting capsules K7 were washed several times with water and a complexing agent such as Dequest®.
• capsules K7 were then stored for 4 weeks at room temperature in water or in liquid detergent E3 . Subsequent enzyme analysis of capsules K7 and the surrounding solution gave the following values: sample Content of amylase [%] Capsule K7 in water 2.9 Capsule K7 in E3 2.9 Storage solution water 0.03 Storage solution E3 0.03
• capsules were prepared analogously with the compositions according to Table 3 but without corn starch and stored in water at room temperature. After a short storage time, there was just as much enzyme in the storage solution as in the capsule itself.

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• 2004
  • 2004-09-29 DE DE102004047097A patent/DE102004047097A1/de not_active Ceased
• 2005
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