EP0629692A1 - Préparations enzymatiques liquides - Google Patents

Préparations enzymatiques liquides Download PDF

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Publication number
EP0629692A1
EP0629692A1 EP94108755A EP94108755A EP0629692A1 EP 0629692 A1 EP0629692 A1 EP 0629692A1 EP 94108755 A EP94108755 A EP 94108755A EP 94108755 A EP94108755 A EP 94108755A EP 0629692 A1 EP0629692 A1 EP 0629692A1
Authority
EP
European Patent Office
Prior art keywords
liquid
enzyme
weight
enzyme preparation
preparation according
Prior art date
Legal status (The legal status 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 status listed.)
Granted
Application number
EP94108755A
Other languages
German (de)
English (en)
Other versions
EP0629692B1 (fr
Inventor
Wilfried Hahn
Hubert Herrmann
Torsten Dr. Kiesser
Vera Sander
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chr Hansen GmbH
Danisco US Inc
Original Assignee
Solvay Enzymes GmbH and Co KG
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Filing date
Publication date
Application filed by Solvay Enzymes GmbH and Co KG filed Critical Solvay Enzymes GmbH and Co KG
Publication of EP0629692A1 publication Critical patent/EP0629692A1/fr
Application granted granted Critical
Publication of EP0629692B1 publication Critical patent/EP0629692B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38663—Stabilised liquid enzyme compositions

Definitions

  • the present invention relates to liquid enzyme preparations, a process for their preparation and their use in liquid detergent and cleaning agent compositions.
  • liquid detergent and cleaning agent compositions e.g. B. for cleaning textiles or dishes
  • enzymes are used to increase the washing effectiveness.
  • Proteases, lipases, amylases or cellulases are usually used as enzymes.
  • the enzyme stability can be severely impaired by the other detergent components present.
  • Another problem with these enzyme-containing liquid compositions is often their sedimentation stability.
  • the object was therefore to provide liquid enzyme preparations which are stable to sedimentation and have high enzyme stability and are therefore well suited for use in liquid detergent and cleaning agent compositions.
  • Liquid enzyme preparations have now been found which show the required properties.
  • the invention therefore relates to a liquid enzyme preparation which comprises 3 to 25% by weight of an enzyme particle suspension, optionally 0.5 to 30% by weight of water, 1 to 10% by weight of a highly disperse filler and 65 to 95.5% by weight. -% of a liquid alkylene oxide polymer based on ethylenediamine having a molecular weight in the range from 500 to 8,200.
  • All the enzymes customary in detergent and cleaning agent compositions for example proteases, lipases, amylases, glucanases such as cellulases, hemicellulases, oxidases or oxygenases, can be present as enzymes in the liquid enzyme preparations according to the invention.
  • the enzymes can be present individually or as an enzyme mixture, for example as a protease / amylase mixture or protease / lipase mixture.
  • the liquid enzyme preparations according to the invention preferably contain proteases and / or amylases.
  • the liquid enzyme preparations according to the invention advantageously contain a heat-stable amylase such as, for. B. Optitherm R.
  • the liquid enzyme preparations according to the invention contain proteases, in particular alkaline proteases.
  • the so-called subtilisins are particularly advantageous as alkaline proteases.
  • Subtilisins are alkaline proteases with a pH optimum in the alkaline pH range and an essential serine residue in the active center.
  • Optimized proteases which have improved properties such as increased washing performance or improved stability due to known biotechnological mutagenesis can also be used in an advantageous manner.
  • Proteases can be obtained in a manner known per se from Gram-positive bacteria or fungi.
  • proteases obtained from Bacillus strains, for example subtilisins such as Subtilisin BPN ', Subtilisin Carlsberg and proteases derived from Bacillus subtilis, Bacillus amyloliquefaciens, Bacillus licheniformis, Bacillus lentus, Bacillus mesentericus or Bacillus alcalophilus can be isolated.
  • proteases which have a pH optimum in the range from 7 to 13 and which, for. B. as Savinase R , Maxacal R , Durazym R , Maxapem R or Opticlean R are commercially available.
  • the enzymes suitable for the liquid enzyme preparations according to the invention can be obtained in a manner known per se by fermentation processes from suitable microorganisms, in particular from bacteria or fungi.
  • the fermentation broths obtained during the fermentation are made of insoluble accompanying substances, e.g. B. by filtration, and then freed in a conventional manner, for. B. by membrane filtration processes or by thin-layer evaporation, whereby so-called enzyme concentrates are obtained, which usually contain the enzyme or enzyme mixture in an amount of 2 to 50 wt .-%, based on the dry matter.
  • the enzymes are in the form of a so-called aqueous enzyme particle suspension (enzyme slurry).
  • aqueous enzyme particle suspension is obtained by, for example, from the aforementioned enzyme concentrates in a manner known per se. B. by precipitation processes, spray drying or crystallization, the enzymes precipitated and the precipitate thus obtained again in a known manner in liquid, for. B. the mother liquor or a suitable buffer solution, saline or amino acid solution.
  • Suitable precipitation processes according to which the enzymes can be precipitated from the enzyme concentrates are e.g. B. the known methods according to which the enzymes by means of the addition of salts, for. B.
  • a concentrated sodium or ammonium sulfate solution or by the addition of an organic solvent such as.
  • an organic solvent such as ethanol, acetone, octanol or decanol can be precipitated from the enzyme concentrates obtained after the fermentation.
  • An enzyme crystal suspension (enzyme crystal slurry) is preferably used as the enzyme particle suspension in the liquid enzyme preparations according to the invention. This is obtained by adding an aqueous, e.g. B. 5 to 20% solution of an alkali or alkaline earth metal halide salt, optionally heated to 20 to 35 ° C and awaiting crystallization of the enzyme.
  • An aqueous 10% alkali metal chloride solution in particular a 10% sodium chloride solution, is preferably added.
  • the enzyme crystal suspension of a protease in particular an alkaline protease such as, for example, is preferably processed in the liquid enzyme preparations according to the invention.
  • the main constituent of the liquid enzyme preparations according to the invention contains 65 to 95.5% by weight, preferably 80 to 90% by weight, of a liquid alkylene oxide polymer based on ethylenediamine with a molecular weight in the range from 500 to 8,200.
  • a liquid alkylene oxide polymer based on ethylenediamine with a molecular weight in the range from 500 to 8,200.
  • Such compounds are obtained in a manner known per se by the addition of alkylene oxide units, for. B. ethylene oxide or propylene oxide units, on ethylenediamine.
  • alkylene oxide block or mixed polymers are obtained. Both the alkylene block and the copolymers based on ethylenediamine can be used in the liquid enzyme preparations according to the invention.
  • the block polymers are preferably used.
  • alkylene oxide polymers based on a lower alkylenediamine other than ethylenediamine e.g. B. based on propylenediamine.
  • the alkylene oxide polymers are used in liquid form in the enzyme preparations according to the invention. Since the flowability of the alkylene oxide polymers depends on the number of alkylene oxide units present in the polymer changed, "liquid" in the sense of the invention should be understood to mean both low viscosity and viscous to pasty alkylene oxide polymers.
  • the liquid enzyme preparations according to the invention preferably contain an ethylene oxide-propylene oxide polymer based on ethylenediamine.
  • the molecular weight of this polymer should preferably be in the range from 1,500 to 7,500.
  • the ethylene oxide content in such a preferred polymer should advantageously be about 40% by weight.
  • Such polymers that contain ethylene oxide and propylene oxide units as block polymers added to ethylenediamine are, for. B. commercially available under the trade name Synperonic T R (from ICI).
  • the liquid enzyme preparations according to the invention contain a highly disperse filler in an amount of 1 to 10% by weight, preferably 1 to 5% by weight.
  • a highly disperse filler in an amount of 1 to 10% by weight, preferably 1 to 5% by weight.
  • highly disperse inorganic compounds from the group consisting of silicas, aluminosilicates, aluminum oxides and titanium dioxide are suitable as highly disperse fillers.
  • Such highly disperse products are generally known and commercially available. Preference is given to using highly disperse silicas such.
  • B. the products available from Degussa under the trade name Aerosil R , e.g. B. Aerosil 200 R.
  • a liquid enzyme preparation according to the invention contains 3 to 10% by weight of an enzyme crystal suspension of a highly alkaline protease, 5 to 10% by weight of water, 1 to 5% by weight of Aerosil R 200 and 80 to 90% by weight of Synperonic T304 R.
  • 1,000 DU correspond to a proteolytic activity which, with a volume of 1 ml of a 2% enzyme solution (w / w) after degradation of casein, results in an extinction difference (1 cm light path; 275 nm; determination against blind sample test) of 0.400.
  • the invention further comprises a process for the preparation of liquid enzyme preparations, in which 3 to 25% by weight of an enzyme particle suspension, optionally 0.5 to 30% by weight of water, 1 to 10% by weight of a highly disperse filler and 65 to 95.5% by weight of a liquid alkylene oxide polymer based on ethylenediamine with a molecular weight in the range from 500 to 8,200 are mixed with one another, the percentages by weight relating to the finished overall preparation.
  • the process is expediently carried out by placing the liquid alkylene oxide polymer based on ethylenediamine in a vessel and then slowly adding the highly disperse filler with vigorous stirring, and then adding the corresponding enzyme particle suspension homogenized by stirring.
  • An ethylene oxide-propylene oxide polymer based on ethylene diamine is preferably used. This polymer should preferably have a molecular weight in the range from 1,500 to 7,500.
  • Synperonic R e.g. B. Use Synperonic T304 R with a molecular weight of approx. 1,650.
  • the enzyme particle suspension the appropriate amount of water is usually also added due to the water content of the enzyme particle suspension added.
  • An enzyme crystal suspension of a highly alkaline protease is preferably used as the enzyme particle suspension, the enzyme activity of which has been concentrated to 2 million to 6 million DU / ml in a manner known per se.
  • the invention further relates to liquid washing and cleaning agents which contain the liquid enzyme preparations according to the invention.
  • the liquid enzyme preparations according to the invention are preferably used in liquid detergents for cleaning textiles or in liquid dishwashing detergents. Except for the liquid enzyme preparations
  • the detergent or cleaning agent formulations can contain all the ingredients and auxiliaries which are customary in the prior art for the formulation of liquid washing and cleaning agents, for. B. surfactants, builders (builder) and optionally bleach or bleach precursors in conventional amounts.
  • the auxiliaries include e.g. B. enzyme stabilizers, complexing and chelating agents, foam regulators and additives such as corrosion inhibitors, antistatic agents, dyes, fragrances, bactericides, fungicides and activators.
  • the liquid enzyme preparations according to the invention show surprisingly good properties which are particularly suitable for use in liquid detergent and cleaning agent formulations.
  • the liquid enzyme preparations according to the invention have a very high storage stability, the enzyme activity of the enzymes processed in these liquid enzyme preparations remaining virtually unchanged even over a relatively long period.
  • the liquid enzyme preparations according to the invention are very stable to sedimentation. Due to their low viscosity, the liquid enzyme preparations according to the invention can be easily metered and are therefore very well suited for processing in liquid washing or cleaning agents.
  • the activity of the protease processed in the liquid enzyme preparations was determined in Delft Units (DU).
  • 1,000 DU correspond to the proteolytic activity, which results in an extinction difference (1 cm light path; 275 nm; determination against blind sample test) of 0.400 with a volume of 1 ml of a 2% enzyme solution (w / w) after degradation of casein.
  • a Bacillus alcalophilus (DSM No. 5466) was fermented in a manner known per se. Insoluble accompanying substances were separated from the fermenter broth by filtration using filter aids and flocculants. The pH in the filtrate was adjusted to 5.2 and concentrated by ultrafiltration by a factor of about 4 to a protease activity of about 750,000 DU / ml. After ultrafiltration, a 10% saline solution was added, the mixture was warmed to about 30 ° C. and the crystallization of the enzyme was awaited. An enzyme crystal suspension was obtained which, in a manner known per se, was concentrated to a protease activity of about 3.6 million DU / ml while removing the mother liquor.
  • the enzyme crystal suspension of the highly alkaline protease was then processed into the liquid enzyme preparations according to the invention using the following recipe: 5% by weight enzyme crystal suspension 7.0% by weight of water (also introduced via the enzyme crystal suspension) 2.6% by weight Aerosil 200 R (highly disperse silica) 85.4% by weight Synperonic T304 R (liquid ethylene oxide-propylene oxide polymer based on ethylenediamine, MW: approx.1,650).
  • the liquid enzyme preparations according to the invention were prepared by placing the specified amount of Synperonic T304 R in a vessel to which the specified amount of Aerosil 200 R was slowly added with vigorous stirring. Then the enzyme crystal suspension previously homogenized by stirring was added with stirring. You got a sedimentation-stable liquid enzyme preparation of the highly alkaline protease with a protease activity of approx. 678,000 DU / g.
  • An enzyme crystal suspension of a protease obtained in the same way as in Example 1 was processed in the same manner according to the following recipe: 10% by weight enzyme crystal suspension 7% by weight of water (also introduced via the enzyme crystal suspension) 5.2% by weight Aerosil 200 R 77.8% by weight Synperonic T304 R A sedimentation-stable liquid enzyme preparation with a protease activity of approx. 960,000 DU / g was obtained.
  • a liquid enzyme preparation of a protease was produced according to the following recipe: 25% by weight enzyme crystal suspension 7.4% by weight of water (also introduced via the enzyme crystal suspension) 2.6% by weight of Aerosil 200 R. 65% by weight Synperonic T 304 R A sedimentation-stable liquid enzyme preparation with a protease activity of approximately 1.8 million DU / g was obtained.

Landscapes

  • 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)
  • Detergent Compositions (AREA)
  • Enzymes And Modification Thereof (AREA)
  • Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
EP94108755A 1993-06-16 1994-06-08 Préparations enzymatiques liquides Expired - Lifetime EP0629692B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4319908 1993-06-16
DE4319908A DE4319908A1 (de) 1993-06-16 1993-06-16 Flüssige Enzymzubereitungen

Publications (2)

Publication Number Publication Date
EP0629692A1 true EP0629692A1 (fr) 1994-12-21
EP0629692B1 EP0629692B1 (fr) 2001-11-28

Family

ID=6490438

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94108755A Expired - Lifetime EP0629692B1 (fr) 1993-06-16 1994-06-08 Préparations enzymatiques liquides

Country Status (13)

Country Link
US (1) US5558812A (fr)
EP (1) EP0629692B1 (fr)
JP (1) JPH078277A (fr)
CN (1) CN1102436A (fr)
AT (1) ATE209675T1 (fr)
AU (1) AU688312B2 (fr)
BR (1) BR9402425A (fr)
CA (1) CA2125945A1 (fr)
DE (2) DE4319908A1 (fr)
DK (1) DK0629692T3 (fr)
ES (1) ES2169052T3 (fr)
FI (1) FI942847A (fr)
PT (1) PT629692E (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995015371A1 (fr) * 1993-12-03 1995-06-08 Buckman Laboratories International, Inc. Stabilisation d'enzymes par des copolymeres sequences
WO2014087011A1 (fr) * 2012-12-07 2014-06-12 Novozymes A/S Prévention de l'adhésion de bactéries

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69720043T2 (de) * 1996-12-20 2003-10-16 Unilever N.V., Rotterdam Enzymatische bleichmittelzusammensetzung
AU3664097A (en) * 1997-07-09 1999-02-08 Procter & Gamble Company, The Detergent compositions comprising a specific oxygenase
ATE259875T1 (de) * 1997-07-09 2004-03-15 Procter & Gamble Reinigungszusammensetzungen enthaltend eine spezifische oxygenase
US6251845B1 (en) 1997-07-09 2001-06-26 The Procter & Gamble Company Detergent compositions comprising an oxygenase enzyme and cofactor to remove body soils
US6541606B2 (en) * 1997-12-31 2003-04-01 Altus Biologics Inc. Stabilized protein crystals formulations containing them and methods of making them
GB2477914B (en) 2010-02-12 2012-01-04 Univ Newcastle Compounds and methods for biofilm disruption and prevention
WO2013148492A1 (fr) 2012-03-29 2013-10-03 Novozymes A/S Utilisation d'enzymes pour préparer des films hydrosolubles
JP6186821B2 (ja) * 2013-04-10 2017-08-30 日油株式会社 水系分散剤、および水系分散体組成物
AU2014346511B2 (en) 2013-11-11 2016-12-22 Ecolab Usa Inc. Multiuse, enzymatic detergent and methods of stabilizing a use solution
CN105829516A (zh) 2013-11-11 2016-08-03 艺康美国股份有限公司 具有强化的污垢控制和污物分散的高碱性餐具清洗洗涤剂
JP6615758B2 (ja) * 2013-12-11 2019-12-04 ノボザイムス アクティーゼルスカブ 水可溶性フィルム中の酵素粒子の使用
CN107197877B (zh) * 2017-07-12 2020-04-21 宿迁研美生物科技有限公司 生物复合酶病毒清除剂（消毒剂）
CN115322846A (zh) * 2022-08-23 2022-11-11 广西电网有限责任公司钦州供电局 一种含有多酶的用于清洗生物膜的清洗剂及其生产方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD286181A5 (de) * 1988-12-28 1991-01-17 Adw Der Ddr,Zi Fuer Organische Chemie,De Fluessiges, enzymhaltiges waschmittel
JPH0465494A (ja) * 1990-07-04 1992-03-02 Kao Corp 自動食器洗浄機用洗浄剤組成物

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3553139A (en) * 1966-04-25 1971-01-05 Procter & Gamble Enzyme containing detergent composition and a process for conglutination of enzymes and detergent composition
US3717550A (en) * 1970-09-25 1973-02-20 Pabst Brewing Co Liquid compositions of bacterial protease and/or amylase and preparation thereof
US3950277A (en) * 1973-07-25 1976-04-13 The Procter & Gamble Company Laundry pre-soak compositions
US4889652A (en) * 1988-05-02 1989-12-26 Colgate-Palmolive Company Non-aqueous, nonionic heavy duty laundry detergent with improved stability using microsperes and/or vicinal-hydroxy compounds
WO1991009941A1 (fr) * 1989-12-21 1991-07-11 Novo Nordisk A/S Preparation contenant des enzymes et detergent contenant une telle preparation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD286181A5 (de) * 1988-12-28 1991-01-17 Adw Der Ddr,Zi Fuer Organische Chemie,De Fluessiges, enzymhaltiges waschmittel
JPH0465494A (ja) * 1990-07-04 1992-03-02 Kao Corp 自動食器洗浄機用洗浄剤組成物

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 9215, Derwent World Patents Index; Class A97, AN 92-120579 *
DATABASE WPI Section Ch Week 9224, Derwent World Patents Index; Class A97, AN 92-197681, NOVO-NORDISK AS: "Liq. detergent compsns. - comprising slurries of crystalline enzymes, esp. proteases" *
RESEARCH DISCLOSURE, vol. 337, no. 091, 10 May 1992 (1992-05-10), EMSWORTH, GB *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995015371A1 (fr) * 1993-12-03 1995-06-08 Buckman Laboratories International, Inc. Stabilisation d'enzymes par des copolymeres sequences
US5780283A (en) * 1993-12-03 1998-07-14 Buckman Laboratories International, Inc. Enzyme stabilization by oxygen-containing block copolymers
WO2014087011A1 (fr) * 2012-12-07 2014-06-12 Novozymes A/S Prévention de l'adhésion de bactéries
CN110628528A (zh) * 2012-12-07 2019-12-31 诺维信公司 预防细菌的粘附
CN110628528B (zh) * 2012-12-07 2021-09-14 诺维信公司 预防细菌的粘附

Also Published As

Publication number Publication date
DE4319908A1 (de) 1994-12-22
FI942847A (fi) 1994-12-17
AU6473494A (en) 1994-12-22
EP0629692B1 (fr) 2001-11-28
FI942847A0 (fi) 1994-06-15
CA2125945A1 (fr) 1994-12-17
DK0629692T3 (da) 2002-04-02
US5558812A (en) 1996-09-24
ATE209675T1 (de) 2001-12-15
DE59409972D1 (de) 2002-01-10
PT629692E (pt) 2002-03-28
ES2169052T3 (es) 2002-07-01
JPH078277A (ja) 1995-01-13
CN1102436A (zh) 1995-05-10
AU688312B2 (en) 1998-03-12
BR9402425A (pt) 1995-01-17

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