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WO1997019161A1 - Preparation enzymatique contenant un polymere facilitant le lavage - Google Patents

Preparation enzymatique contenant un polymere facilitant le lavage Download PDF

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Publication number
WO1997019161A1
WO1997019161A1 PCT/EP1996/004921 EP9604921W WO9719161A1 WO 1997019161 A1 WO1997019161 A1 WO 1997019161A1 EP 9604921 W EP9604921 W EP 9604921W WO 9719161 A1 WO9719161 A1 WO 9719161A1
Authority
WO
WIPO (PCT)
Prior art keywords
enzyme
dirt
detergents
repellent polymer
weight
Prior art date
Application number
PCT/EP1996/004921
Other languages
German (de)
English (en)
Inventor
Albrecht Weiss
Georg Meine
Original Assignee
Henkel Kommanditgesellschaft Auf Aktien
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel Kommanditgesellschaft Auf Aktien filed Critical Henkel Kommanditgesellschaft Auf Aktien
Priority to EP96939004A priority Critical patent/EP0876462A1/fr
Publication of WO1997019161A1 publication Critical patent/WO1997019161A1/fr

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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
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0036—Soil deposition preventing compositions; Antiredeposition agents
    • 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
    • C11D3/37—Polymers
    • C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3715—Polyesters or polycarbonates
    • 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
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
    • C12N9/98—Preparation of granular or free-flowing enzyme compositions

Definitions

  • the invention relates to an enzyme granulate which contains dirt-repellent polymer, a process for its preparation and the use of the granulate in solid washing and cleaning agents
  • detergents In addition to the ingredients that are indispensable for the washing process, such as surfactants and builder materials, detergents generally contain further constituents which can be summarized under the term washing auxiliaries and which comprise such different active ingredient groups as foam regulators, graying inhibitors, bleaching agents, bleach activators and color transfer inhibitors. Such auxiliaries also include Substances which impart dirt-repellent properties to the washing fiber and which, if present during the washing process, support the dirt-removing ability of the other detergent components. The same applies analogously to detergents for hard surfaces. Such dirt-removing agents are often termed "sol-release" active ingredients or because of their perspectivess, the treated surface, for example the fiber, to repel dirt, referred to as "So ⁇ !
  • Enzymes in particular proteases, are also used extensively in washing, washing aids and cleaning agents.
  • the enzymes are usually not used as concentrates, but in mixtures with a thinning and carrier material. If such enzyme preparations are mixed with conventional detergents, a considerable amount can be stored Degradation of the enzyme activity occur, especially when bleach-active compounds are present.
  • the storage stability can be increased considerably if the enzymes are coated with the carrier material , or embedded in this and then converted into the desired particle shape by extrusion , pressing and Marume ⁇ sieren, as for example in the German patent DE 16 17 232, the German Offenlegungssch ⁇ ft DT 20 32 768, and the German interpretations DE 21 37 042 and DE 21 37 043 described
  • such enzyme preparations only have poor solubility properties. The undissolved particles can get caught in the goods to be cleaned and contaminate them or they are unused in the wastewater.
  • German embedding agents DT 18 03 099 known embedding agents that consist of a mixture solid acids or acidic salts and carbonates or dicarbonates exist and are obtained with the addition of water, although they improve the solvent power, but are themselves very sensitive to moisture and therefore require additional protective measures
  • enzyme granules for use in granular detergents and cleaning agents which contain 2% by weight to 20% by weight of enzyme, 10% by weight to 50% by weight of swellable starch, Contain 5 wt .-% to 50 wt .-% water-soluble organic polymer as a granulating aid, 10 wt .-% to 35 wt .-% grain flour and 3 wt .-% to 12 wt .-% water.
  • Such additives enable enzyme processing without major loss of activity and the storage stability of the enzymes in the granules is also satisfactory.
  • the international patent application WO 94/23005 describes enzyme granules for use in granular detergents and cleaning agents. These granules contain enzyme and inorganic and / or organic carrier material as well as carboxymethyl cellulose-containing granulation aids, the granulation aid system containing alkali-carboxymethyl cellulose with degrees of substitution of 0.1 to 1 and polyethylene glycol and / or alkyl or alkenyl polyethoxylate with the proviso that , in each case based on the finished granulate, at least 0.5% by weight of polyethylene glycol with an average molecular weight below 1000 and / or alkyl or alkenyl polyethoxylate with at least 20 ethoxy groups is present if more than 2% by weight of alkali metal carboxymethyl cellulose is present.
  • solubility of the enzyme granulate described in international patent application WO 94/23005 is increased by the special granulation aid system, which contains solubilizing or dust-binding components and grain-solidifying components in optimized ratios.
  • the enzyme granules described in the publications cited above have a satisfactory result by optimizing the granulation aids Storage stability of both the enzymes and the granules containing them
  • Storage stability is, however, only achieved by adding components which do not contribute to the washing performance of the agents into which the granules are incorporated.
  • the object was therefore to develop an enzyme granulate which is suitable for incorporation into particulate detergents and cleaning agents and which, in addition to the enzyme, contains a further component which is suitable for the washing and cleaning process, namely a dirt-repellent polymer, and which is satisfactory Has inventory stability and solubility
  • the invention accordingly relates to enzyme granules suitable for incorporation into particulate detergents and cleaning agents, containing enzyme and inorganic and / or organic carrier material and optionally granule auxiliaries, which is characterized in that the granules contain a dirt-repellent polymer suitable for the detergents and cleaning agents
  • the known dirt-repelling polymers include, in particular, copolyesters which contain dicarboxylic acid units, alkylene glycol units and polyalkylene glycol units.
  • Such dirt-repellant copolyesters and their use in detergents have been known for a long time.
  • the German patent application DT 16 17 141 describes a washing process using of polyethylene terephthalate-polyoxyethylene glycol copolymers
  • the German Offenlegungssch ⁇ ft DT 22 00 911 relates to detergents which contain nonionic surfactant and a copolymer of polyoxyethylene glycol and polyethylene terephthalate.
  • Polymers with a molecular weight of 15,000 to 50,000 made of ethylene terephthalate and polyethylene oxide terephthalate, the polyethylene glycol units having molecular weights of 1000 to 10,000 and the molar ratio of ethylene terephthalate to polyethylene oxide terephthalate 2 being 1 to 6 1, can be according to the German published patent application DE 33 24 258 can be used in detergents.
  • the European patent EP 066 944 relates to textile treatment agents which contain a copolyester of ethylene glycol, polyethylene glycol, aromatic dicarboxylic acid and sulfonated aromatic dicarboxylic acid in certain molar ratios.
  • European or European patent EP 185 427 includes methyl- or ethyl group-end-capped polyesters with ethylene and / or Propylene terephthalate and polyethylene oxide terephthalate units and detergents containing such a soil release polymer are known.
  • European patent EP 241 984 relates to a polyester which, in addition to oxyethylene groups and terephthalic acid units, also contains substituted ethylene units and glycine units
  • European patent EP 241 985 discloses polyesters which, in addition to oxyethylene groups and terephthalic acid units, contain 1, 2-propylene, 1, 2-butylene and / or 3-methoxy-1, 2-propylene groups and glycene units and are linked with C r to C 4 -alkyl groups are closed
  • Patent EP 253 567 relates to soil release polymers with a molecular weight of 900 to 9000 made of ethylene terephthalate and polyethylene oxide terephthalate, the polyethylene glycol units having molecular weights of 300 to 3000 and the molar ratio of ethylene terephthalate to polyethylene oxide terephthalate 0.6 is up to 0.95
  • the European patent application EP 272 033 discloses polyesters with poly-propylene terephthalate and polyoxyethylene ter
  • European patent EP 274 907 describes sulfoethyl end-capped terephthalate-containing soil-release polyesters.
  • European patent application EP 357 280 describes sulfonation of unsaturated end groups by means of soii-release polyesters with terephthalate, alkylene glycol and poly-C 2-4 glycol units manufactured.
  • Dirt-releasing polymers which are preferably used are, in particular, polymers which contain ethylene terephthalate groups of the formula (I)
  • n is an integer from 17 to 110, the molar ratio of ethylene terephthalate to polyethylene oxide terephthalate in the polymer being from about 50:50 to about 90-10
  • the molecular weight of the linking polyethylene oxide units is preferably in the range from 750 to 5000.
  • mers can have an average molecular weight of from about 5000 to about 200,000.
  • Ethylene terephthalate and polyethylene oxide terephthalate can be distributed arbitrarily in the polymer.
  • Particularly preferred polymers are those with molar ratios of ethylene terephthalate polyethylene oxide terephthalate from about 65 35 to about 90 10, preferably from about 65 35 to about 80 20, where the linking polyethylene oxide units have a molecular weight of 750-5000, preferably about 1000 to about 3000 and the polymer has a molecular weight of about 10000 to about 50,000.
  • Examples of commercially available polymers of this type are, for example, Milease® T "from ICI United States, Inc., Velvetol® by Rh ⁇ ne-Poulenc and Zelcon® 8037 by DuPont
  • the above-mentioned dirt-repellent polymers can be prepared by known polymerization processes, the starting materials being used in amounts such as to obtain the above-mentioned ratios of ethylene terephthalate to polyethylene oxide terephthalate.
  • the processes described in US Pat. No. 3,479,212 can be used for the preparation suitable polymers can be used
  • the amount of soil-repellent polymers in the granules depends on the total concentration of soil-repellent polymers required in the detergent and cleaning agent and the concentration of the granules contained in the agents, which is usually between 0.1 and 10% by weight, based on the finished agent Dirt-repellent polymers are preferably contained in the enzyme granulate according to the invention in an amount of 1 to 50% by weight , in particular 5% to 25% by weight and particularly preferably 5% to 15% by weight
  • Suitable enzymes for the enzyme granules according to the invention are primarily the proteases, lipases, amylases and / or cellulases obtained from microorganisms such as bacteria or fungi, and so-called bleaching enzymes such as oxidases, laccases and peroxidases, proteases produced by bacillus species and genetically modified proteases and their mixtures with other enzymes are preferred.
  • Preferred enzyme mixtures are, for example, mixtures of protease, lipase and cellulase from protease and cellulase or from protease and Lipase They can be obtained in a known manner by fermentation processes from suitable microorganisms, which are described, for example, in German Offenlegungsschrift DE 19 40 488, DE 20 44 161, DE 21 01 803 and DE 21 21 397, and US Pat. Nos.
  • the amounts of dirt-repellent polymers and enzymes contained in the granules according to the invention are usually matched to the properties of the finished washing and cleaning agent and can vary within wide ranges In principle, all organic or inorganic powdery substances which do not destroy or deactivate the enzymes to be granulated or only tolerably little or deactivate and are stable under granulation conditions can be used as carrier materials.
  • Such substances include, for example, starch, cereal flour, cellulose powder, cellulose derivatives such as methyl or carboxymethyl - Or ethyl cellulose, alkali alumosilicate, in particular zeolite, layered silicate, for example bentonite or smectite, synthetic, crystalline layered silicate, for example SKS-6® (commercial product from Hoechst AG, BR Germany) and water-soluble inorganic or organic salts and acids, for example alkali chloride , Alkali sulfate, alkali carbonate or alkali acetate, sodium or potassium being the preferred alkali metals, citric acid, tartaric acid, adipic acid, NaHS0 4, etc.
  • a carrier material mixture of starchy cereal flour swellable in water and optionally cellu is preferred loose powder and alkali carbonate used
  • the starch which is swellable in water is preferably corn starch, rice starch, potato starch or mixtures thereof, the use of corn starch being particularly preferred.
  • swellable starch is preferably in amounts of 5 to 50% by weight, in particular 10 up to 35% by weight, the sum of the amounts of the swellable starch and the flour is preferably not more than 80% by weight, in particular 25% by weight to 65% by weight
  • the cereal flour is, in particular, a product which can be produced from wheat, rye, barley or oats or a mixture of these flours, wholemeal flours being preferred.
  • Whole-grain flour is understood to mean a flour which is not fully ground and which consists of whole, unpeeled grains has been produced or at least predominantly consists of a product of this type, the rest consisting of fully ground flour or starch.
  • Commercial wheat flour qualities such as type 450 or type 550 are preferably used.
  • such cereal flour is preferably present in amounts of 10% to 35% by weight, in particular 15% by weight. up to 25% by weight
  • the preparations according to the invention can, as a further component of the carrier material, preferably 1% by weight to 50% by weight, particularly preferably 5% by weight to 25% by weight, based on the total granulate, of a granulation auxiliary system which contains alkali carboxymethyl cellulose with degrees of substitution of 0.5 to 1 and polyethylglycose and / or alkyl polyethoxylate contained in this granulation aid system, based in each case on finished enzyme granules, preferably 0.5% by weight to 5% by weight of alkali carboxymethyl cellulose with degrees of substitution from 0.5 to 1 and to to 3% by weight of polyethylene glycol and / or alkyl polyethoxylate, it being particularly preferred if at least 0.5% by weight, in particular 0.8% by weight to 2% by weight of polyethylene glycol with an average molecular weight of less than 1000 and / or alkyl polyethoxylate at least 30 ethoxy groups are present if more than 2% by weight of alkali carb
  • additional cellulose or starch ethers such as carboxymethyl starch, methyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose and corresponding cellulose ether, gelatin, casem, tragacanth, maltodextrose, sucrose, invert sugar, glucose syrup or other water-soluble ohmic or well-dispersible water-soluble or well-dispersible agents can optionally be used as additional constituents of the granulation aid system or polymers of natural or synthetic origin are used.
  • additional cellulose or starch ethers such as carboxymethyl starch, methyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose and corresponding cellulose ether, gelatin, casem, tragacanth, maltodextrose, sucrose, invert sugar, glucose syrup or other water-soluble ohmic or well-dispersible water-soluble or well-dispersible agents can optionally be used as additional constituents of the granulation aid system or polymers of natural or synthetic origin are used.
  • Suitable synthetic water-soluble polymers are polyacrylates, polymethacrylates, copolymers of acrylic acid with maleic acid or compounds containing methyl groups, furthermore polyvinyl alcohol, partially saponified polyvinyl acetate and polyvinylpyrrolidone.
  • Enzyme granules in amounts of up to 10% by weight, in particular from 0.5% by weight to 8% by weight, contain high molecular weight polyethylene glycols, ie those with an average molecular weight above 1000, can be used as synthetic water-soluble polymers with a dusting effect, however the high molecular weight polyethylene glycols cause an undesirable increase in the time required for the granules to dissolve, so that these substances are preferably not present in the enzyme granules according to the invention
  • Another object of the invention is a method for producing an enzyme granulate suitable for incorporation in detergents and cleaning agents
  • an enzyme granulate is produced by extruding a fermentation broth formed by mixing an aqueous enzyme preparation, which may or may not be insoluble constituents, which may have been previously removed by microfiltration, with dirt-repellent polymer and inorganic and / or organic carrier material as an additive and dirt-repellent polymer, optionally spheronization of the extrudate in a rounding machine and optionally drying and application of an outer covering layer
  • the dirt-repellent polymer is mixed uniformly with enzyme and other constituents in the granulate
  • the enzyme granulate can be obtained by extruding an enzyme premix obtained by admixing an aqueous enzyme preparation, which may or may not have been insoluble constituents previously freed from insoluble constituents by microfiltration, and inorganic and / or organic carrier material as an additive, optionally spheronization the extrudate in a rounding machine and optionally drying and applying an outer coating layer in which an outer coating layer is applied in a fluidized bed made of extrudate and dirt-repellent polymer and optionally other substances for coating, wherein at least 1% by weight to about 95% by weight of dirt-repellent polymer is contained in the coating system
  • the granules obtained by this process consist of a core and an outer shell, the core containing the enzyme and the outer shell containing the dirt-repellent polymer
  • a third possible process variant is a combination of the two processes described above.
  • the enzyme granulate obtained consists of a core and an outer shell, the enzyme being in the core and the dirt-repellent polymer being contained both in the core and in the shell
  • the enzyme granules For the production of the enzyme granules according to the invention, one preferably starts from fermentation broths, which are freed of insoluble accompanying substances, for example by microfiltration.
  • the microfiltration is preferably carried out as cross-flow microfiltration using porous tubes with micropores larger than 0.1 ⁇ m, flow rates of the concentrate solution of more than 2 m / s and a pressure difference to the permeate side of less than 5 bar, as described, for example, in European patent application EP 200 032.
  • the microfiltration pneate is then preferably concentrated by ultrafiltration, if appropriate with subsequent vacuum evaporation.
  • the concentration can, as in the international patent application WO 92 / 11347, can be carried out in such a way that only relatively low dry matter contents of preferably 5 to 50% by weight, in particular 10% to 40% by weight, are obtained if fermentation contains proteases brewing are used, the protease content at this level of the concentrate is preferably 500,000 PE / g to 1,500,000 PE / g, in particular 600,000 PE / g to 1,000,000 PE / g.
  • the concentrate is advantageously made of a dry, powdery form previously prepared to granular mixture of the above additives metered in. This mixture also contains, depending on the method of manufacture, the dirt-repellent polymer.
  • the water content of the mixture should be chosen so that it is suitable for processing with Ruhr and Transfer impact tools into granular, non-sticky particles at room temperature and plastically deform and extrude them when using higher pressures
  • the ⁇ eselfahiges premix obtained is then processed in a known manner in principle in a kneader and a connected extruder to a plastic, as homogeneous mass as possible, the result of mechanical processing, the mass to temperatures between 40 ° C and 60 ° C, especially 45 ° C. can heat up to 55 ° C.
  • the material leaving the extruder is passed through a perforated disk with a subsequent knock-off knife and thereby shredded into cylindrical particles of defined size.
  • the diameter of the holes in a perforated disk is expediently 0.7 to 1.6 mm. preferably 0.8 to 1.2 mm.
  • the particles present in this form can then be dried and coated with a coating system or fed directly to their later use.
  • a device can be used for this, which consists of a cylindrical container with stationary, fixed rare walls and a friction plate rotatably mounted on the bottom.
  • Devices of this type are known in the art under the Marume ⁇ zer® product name and are described, for example, in the German designation DE 21 37 042 and DE 21 37 043 are described below. Any dusty particles with a grain size below 0 1 mm, in particular below 0 4 mm and any coarse particles with a grain size above 2 mm, in particular above 1.6 mm, can be removed by sieving or wind screening and, if necessary are returned to the manufacturing process.
  • the beads are continuously or batchwise, preferably using a fluidized bed drying unit, at supply air temperatures of preferably 35 ° C to 50 ° C and in particular at a product temperature of not more than 42 ° C dried to the desired residual moisture content of, for example, 4% by weight to 10% by weight, in particular 5% by weight to 8% by weight, based on the entire granulate
  • additional substances can be applied to coat and coat the particles.
  • the dirt-repellent polymer is optionally applied together with other suitable coating substances.
  • Suitable coating substances are, in particular, the film formers among the abovementioned water-soluble organic polymers
  • dyes or pigments are also applied to the particles, so as to mask or change any inherent color that usually stems from the enzyme concentrate.
  • Titanium dioxide which is preferably introduced in an aqueous dispersion, is particularly suitable as an inert and physiologically harmless pigment Dispersion from the shell substances or water supplied via a polymer solution which may be present is removed during the drying which is carried out at the same time or is subsequently required again
  • an enzyme core produced by extrusion which is obtainable by extruding a fermentation broth concentrated by mixing an aqueous enzyme preparation, which may be an insoluble constituent which may have been previously freed from microfiltration, and inorganic and / or organic Carrier material as an additive enzyme premix, mixed with a particulate assembled second enzyme under agglomeration conditions, and the coating containing the dirt-repellent polymer is then applied or simultaneously, the mean particle size of the extrudate core containing the first enzyme preferably the 1, 1- to 3- times, in particular, 1.3 to 2 times that of the second or further particulate enzyme is in a preferred embodiment of this embodiment, the enzyme in the extrudate core is protease un d the enzyme amylase, lipase, cellulase, oxidase and / or peroxidase contained in the separately produced, smaller particles, which are aglomeric to the extrudate
  • the enzyme granulate according to the invention is preferably used for the production of solid, in particular particulate detergents or cleaning agents which can be obtained by simple means Mixing of the enzyme granules containing the dirt-repellent polymers with further powder components customary in such agents can be obtained.
  • the enzyme granules preferably have average grain sizes in the range from 0.1 mm to 3 mm, in particular 0.4 mm to 1 , 6 mm
  • the enzyme preparation obtained according to the invention normally consists of largely rounded, dust-free particles, which as a rule have a debris weight of about 500 to 900 grams per liter, in particular 650 to 880 grams per liter, their enzyme activity can be caused by the flexible drying substance content of the broths before Mixing, with the additives, when using protease-containing fermenter broths, values in the range of preferably 150,000 to 350,000 protease units per gram (PE / g), in particular 160,000 PE / g to 300,000 PE / g, are set.
  • Draw the granules according to the invention are characterized by a very high storage stability, in particular at temperatures above room temperature and high air humidity, and a rapid solution behavior in the wash liquor.
  • the granules according to the invention preferably add 100% of their enzyme activity in water within 3 minutes, in particular within 90 seconds to 2 minutes 25 ° C free
  • the fermenter broth concentrated in this way was mixed in a mixer equipped with a rotating impact tool with the additives listed below and dirt-repellent polymer (Velvetol®, a commercial product from Rhönen-Poulenc) and homogenized in a kneader provided with external cooling.
  • the plastic mass was extruded using an extruder equipped with a perforated disc (hole diameter 0.9 mm) and a rotating knife. Extrudates each having lengths of 0.7 mm to 1 mm were obtained, which were deformed and deburred in a spheronization device (Marumerizer®) for a processing time of about 1 minute while simultaneously dusting with powdered calcium carbonate (3% by weight).
  • the material leaving the spheronizer was dried in a fluidized bed dryer at temperatures from 40 ° C. to 45 ° C. within 15 minutes to a water content of 6% by weight. Subsequent sieving gave particles with particle sizes below 0.4 mm and above 1. 6 mm largely removed, which were fed back to the process at the stage of mixing with the additives.
  • the extrudates were coated by spraying an aqueous titanium dioxide pigment suspension during the fluidized bed drying.
  • An enzyme granulate according to the invention was obtained in this way.
  • composition of the extrudate is composition of the extrudate:
  • the granules thus obtained contained protease with an activity of 200,000 PE / g
  • An enzyme granulate was produced as described in Example 1, in which fermenter broth with a protease content of 140,000 PE / g was used.
  • the granulate had the following composition
  • the granules obtained were coated by spraying on a dispersion of 95% by weight, based on the dispersion, dirt-repellent polymer in 5% by weight, based on the dispersion, of C 12 -C 18 fatty alcohol ethoxylate with 7 ethylene oxide groups Granules in an amount of 30 g coating applied to 70 g granules
  • the granules contained soil-repellent polymer in an amount of 28.5% by weight, based on the granules and protease with an activity of 29400 PU / g

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Abstract

L'invention concerne des granulés enzymatiques pouvant être incorporés à des agents de lavage et de nettoyage. Les granulés contiennent l'enzyme, un matériau support inorganique et/ou organique et éventuellement un auxiliaire de granulation. La préparation est caractérisée en ce qu'elle contient non seulement l'enzyme mais aussi un autre composant adapté au lavage et au nettoyage, notamment un polymère facilitant le lavage.
PCT/EP1996/004921 1995-11-20 1996-11-11 Preparation enzymatique contenant un polymere facilitant le lavage WO1997019161A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP96939004A EP0876462A1 (fr) 1995-11-20 1996-11-11 Preparation enzymatique contenant un polymere facilitant le lavage

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19543196.0 1995-11-20
DE1995143196 DE19543196A1 (de) 1995-11-20 1995-11-20 Schmutzabweisendes Polymer enthaltende Enzymzubereitung

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WO1997019161A1 true WO1997019161A1 (fr) 1997-05-29

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7285523B1 (en) * 1999-01-19 2007-10-23 Seydel Companies, Inc. Enzyme-containing granule and detergent composition

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102006018780A1 (de) * 2006-04-20 2007-10-25 Henkel Kgaa Granulat eines sensitiven Wasch- oder Reinigungsmittelinhaltsstoffs

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3344104A1 (de) * 1983-12-07 1985-06-13 Henkel KGaA, 4000 Düsseldorf Zur verwendung in pulverfoermigen waschmitteln geeignete enzymzubereitung
WO1993021294A1 (fr) * 1992-04-13 1993-10-28 The Procter & Gamble Company Utilisation de polyesters modifies pour le lavage de textiles contenant du coton
DE4344490A1 (de) * 1993-12-24 1995-06-29 Henkel Kgaa Pulverförmiges Wasch- und Reinigungsmittel

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3344104A1 (de) * 1983-12-07 1985-06-13 Henkel KGaA, 4000 Düsseldorf Zur verwendung in pulverfoermigen waschmitteln geeignete enzymzubereitung
EP0168526A1 (fr) * 1983-12-07 1986-01-22 Henkel Kommanditgesellschaft auf Aktien Préparation d'enzymes utilisables dans des détergents en poudre
WO1993021294A1 (fr) * 1992-04-13 1993-10-28 The Procter & Gamble Company Utilisation de polyesters modifies pour le lavage de textiles contenant du coton
DE4344490A1 (de) * 1993-12-24 1995-06-29 Henkel Kgaa Pulverförmiges Wasch- und Reinigungsmittel

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7285523B1 (en) * 1999-01-19 2007-10-23 Seydel Companies, Inc. Enzyme-containing granule and detergent composition

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EP0876462A1 (fr) 1998-11-11
DE19543196A1 (de) 1997-05-22

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