WO2012101149A1 - Granules d'enzyme stables au stockage - Google Patents
Granules d'enzyme stables au stockage Download PDFInfo
- Publication number
- WO2012101149A1 WO2012101149A1 PCT/EP2012/051097 EP2012051097W WO2012101149A1 WO 2012101149 A1 WO2012101149 A1 WO 2012101149A1 EP 2012051097 W EP2012051097 W EP 2012051097W WO 2012101149 A1 WO2012101149 A1 WO 2012101149A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- coating
- granule
- weight
- malic acid
- bleach
- Prior art date
Links
Classifications
-
- 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
- C12N9/96—Stabilising an enzyme by forming an adduct or a composition; Forming enzyme conjugates
-
- 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
-
- 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
Definitions
- the present invention relates to an enzyme-containing granule and to a bleach- containing granular composition comprising the granules.
- Enzyme-containing granules are commonly added to bleach-containing granular compositions such as detergents or detergent additives.
- the bleach tends to lower the stability of the enzyme during storage, so there is a need to improve the storage stability of enzyme granules in this environment.
- WO 00/63336 discloses enzyme composite particles having an acidic barrier and a physical barrier coating.
- WO 2004/067739 discloses that the stability of coated enzyme granules in hostile alkaline powder detergents can be improved by adding acidic buffer components to the granules; optionally the coating of the granule may also contain an acidic buffer.
- WO 00/01793 discloses a new improved enzyme coating granule.
- WO 87/07292 discloses coated detergent enzymes.
- the inventors have found that the storage stability of enzyme granules in bleach- containing powders such as detergents or detergent additives can be improved by applying a coating which includes malic acid.
- the invention provides a granule comprising a core surrounded by a protective coating, wherein:
- the core comprises an enzyme
- the coating comprises malic acid.
- the invention also provides a granular composition comprising (a) the above particles and (b) particles comprising a bleach.
- the granule of the invention comprises a core surrounded by a protective coating.
- the core comprises an enzyme
- the protective coating comprises malic acid, typically in an amount of 2-20 % by weight of the coating.
- the malic acid coating may comprise malic acid in an amount of more than 80% by weight, e.g. more than 90% or more than 95%.
- the malic acid coating may include a salt, typically in an amount above 60%, particularly 80-98 %, by weight of the coating.
- the salt is preferably water soluble, with a solubility at 20°C of at least 0.1 g per 100 g of water, particu- larly at least 10 g per 100 g.
- the salt may be sodium sulfate (particularly in anhydrous form) or another salt described in WO 00/01793.
- the malic acid is typically present in an amount of 0.2-10 % by weight of the core, particularly 0.3-5% or 0.5-3%.
- the malic acid coating typically constitutes 10-40 % by weight of the core.
- the malic acid coating may be surrounded by one or more additional coatings, e.g. comprising a wax, particularly polyethylene glycol (PEG) or polyvinyl alcohol (PVA).
- PEG polyethylene glycol
- PVA polyvinyl alcohol
- the PEG typically has a molecular weight of 3000-6000.
- the malic acid coating and/or the optional second coating may comprise a filler or pigment, particularly kaolin, titanium dioxide or talc.
- the total amount of fillers and pigments typically constitutes 5-20 % by weight of the total amount of the coatings.
- the invention may be used to improve the storage stability of any enzyme, particularly a bleach-sensitive detergent enzyme.
- enzymes particularly a bleach-sensitive detergent enzyme.
- examples are proteases, amylases, lipases, carboydras- es and cellulases.
- the protease may be a subtilisin, particularly an alkaline microbial serine protease.
- subtilisins derived from Bacillus, e.g., subtilisin Novo, subtilisin Carlsberg, subtilisin ⁇ ', subtilisin 309, subtilisin 147 and subtilisin 168 (described in WO 89/06279).
- the content of enzyme (calculated as pure enzyme protein) in the granule will typically be in the range of from about 0.5% to 20% by weight of the core.
- the core may be prepared by various known methods, e.g. as described in US 4, 106,991 , WO 97/23606 or WO 97/391 16.
- the core may consist of an inert particle with the blend absorbed into it, or with the blend applied on to the surface e.g. via fluid bed coating.
- the core particle may have a diameter of 20-2000 ⁇ , particularly 50-1500 ⁇ , 100-1500 ⁇ or 250-1200 m.
- the malic acid coating (optionally comprising salt) may be applied onto the enzyme core by atomization of a solution of the compounds onto the core granules in a fluid bed, the malic acid coating may further be applied in vacuum mixers, dragee type coaters (pan-drum coaters), equipment for coating of seeds, equip-ment comprising rotating bottoms (eks. Roto Glatt, CF granulators (Freund), torbed processors (Gauda) or in rotating fluid bed processors such as Omnitex (Nara).
- vacuum mixers dragee type coaters (pan-drum coaters), equipment for coating of seeds, equip-ment comprising rotating bottoms (eks. Roto Glatt, CF granulators (Freund), torbed processors (Gauda) or in rotating fluid bed processors such as Omnitex (Nara).
- the granule may optionally be dried.
- the drying of the malic acid coated granule can be achieved by any drying method available to the skilled person, such as spray-drying, freeze drying, vacuum drying, fluid bed drying, pan drum coating and microwave drying. Drying of the malic acid coated granule can also be combined with granulation methods which comprise e.g. the use of a fluid bed, a fluid bed spray dryer (FSD) or a Multi-stage dryer (MSD).
- FSD fluid bed spray dryer
- MSD Multi-stage dryer
- the coating should encapsulate the core unit by forming a substantially continuous layer.
- a substantially continuous layer is to be understood in the present invention as a coating having few or none holes, so that the core unit it is encapsulating has few or none uncoated areas.
- the layer or coating should in particular be homogenous in thickness.
- the granules are particularly suited for incorporation in a granular detergent composi- tion comprising a surfactant.
- Enzyme granules according to the invention result in improved storage stability of the enzyme when the granules are incorporated in a detergent, even a detergent comprising aggressive components such as a bleaching system.
- the detergent composition may for example be formulated as a laundry detergent composition for hand or machine washings including a cleaning additive composition suitable for pre-treatment of stained fabrics or a fabric softener composition, or a detergent composition for use in general household hard surface cleaning operations, or a composition for hand or machine dishwashing operations.
- the detergent composition of the invention may be in any convenient dry form, e.g., a bar, a tablet, a powder, a granulate or a paste.
- the granules show improved storage stability when added to a bleach-containing powder (or granular) composition.
- the bleach is typically a peroxide-based bleaching system such as a percarbonate or a perborate, which may be combined with a peracid-forming bleach activator such as tetraacetylethylenediamine (TAED) or nonanoyloxybenzenesulfonate (NOBS).
- TAED tetraacetylethylenediamine
- NOBS nonanoyloxybenzenesulfonate
- the bleach-containing powder or granular composition may be a detergent additive comprising at least 50 % by weight of the bleach, or it may be a detergent comprising 5-25 % by weight of surfactant and 10-25 % by weight of the bleach.
- Suitable bleaching system components include bleach activators, sources of hydrogen peroxide such as sodium percarbonate and sodium perborates, preformed peracids and mixtures thereof.
- Suitable preformed peracids include peroxycarboxylic acids and salts, percarbonic acids and salts, perimidic acids and salts, peroxymonosulfuric acids and salts, for example, Oxone®.
- bleaching systems include peroxide-based bleaching systems, which may comprise, for example, an inorganic salt, including alkali metal salts such as sodium salts of per-borate (usually mono- or tetra-hydrate), percarbonate, persulfate, perphosphate, persili- cate salts, in combination with a peracid-forming bleach activator.
- Suitable bleach activators in- el u d e 4-(dodecanoyloxy)benzenesulfonate (LOBS), 4-(decanoyloxy)benzenesulfonate, 4- (decanoyloxy)benzoate (DOBS), 4-(3,5,5-trimethylhexanoyloxy)benzenesulfonate (ISONOBS), tetraacetylethylenediamine (TAED) and 4-(nonanoyloxy)benzenesulfonate (NOBS), and/or those disclosed in W098/17767.
- the bleaching system may comprise peroxyacids of, for example, the amide, imide, or sulfone type.
- the bleaching system may also comprise pe- racids such as 6-(phthaloylamino)percapronic acid (PAP).
- PAP 6-(phthaloylamino)percapronic acid
- the bleaching system may also include a bleach
- the bleach-containing composition may be formulated as described in EP2380481 , WO201 1133380, US201 1212874, US201 1207646, WO2011060109, WO2011005623, WO201 1005630, WO2011005827, WO201 1005833, WO2011005905, WO201 1005910, WO201 1002759, WO2011005813, WO201 1002640, WO2010090915, WO2010006861 , WO2009092699, WO2009030600, WO2009016123, WO201 1036146, WO201 1009887, WO2010142538, WO2010108787, WO2010108783, WO2010108782, WO2010108784, WO2010105961 , WO2010105962, WO2010084203, WO2010063688, DE102009033248, or WO2010049187.
- the enzyme concentrate was an aqueous solution of the protease (Everlase) also containing a carbohydrate (dextrin) binder
- the uncoated granulate was sieved between 300 and 1200 microns:
- Granulate A (comparative granulate):
- Granulate B (granulate of the invention):
- Inlet air temperature 90°C during salt coating, 60°C during film coating
- Product temperature 42-46°C during salt coating, 40-42°C during film coating 1.2 mm nozzle
- the granulate was dried to a temperature of approx. 60°C, after film coating the granulate was dried to a temperature of approx. 50°C and subsequently cooled to approx. 40°C before discharge.
- Granulate A and B were mixed with a commercial bleach-containing powder detergent additive (4% granulate+96% powder additive) without enzyme (Vanish from Reckitt Benckiser). Glasses with 5 g of the enzyme containing detergent additive were stored for 2 weeks at 37°C and 70% relative humidity (%RH) in open glasses. The residual activity of the protease was analyzed using standard protease assays (compared to unstored samples):
- Granulate A comparative granulate: 71 % Granulate B (granulate of the invention) 89%
Abstract
Selon la présente invention, la stabilité au stockage de granules d'enzyme dans des granulats contenant un agent de blanchiment tels que des détergents ou des additifs pour détergents peut être améliorée par l'application d'un enrobage contenant de l'acide malique.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP11152214 | 2011-01-26 | ||
EP11152214.0 | 2011-01-26 |
Publications (1)
Publication Number | Publication Date |
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WO2012101149A1 true WO2012101149A1 (fr) | 2012-08-02 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2012/051097 WO2012101149A1 (fr) | 2011-01-26 | 2012-01-25 | Granules d'enzyme stables au stockage |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015028567A1 (fr) * | 2013-08-28 | 2015-03-05 | Novozymes A/S | Granulé enzymatique contenant un agent de blanchiment fluorescent |
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WO1987007292A1 (fr) | 1986-05-21 | 1987-12-03 | Novo Industri A/S | Enzymes detergents enrobes |
WO1989006279A1 (fr) | 1988-01-07 | 1989-07-13 | Novo-Nordisk A/S | Genes de subtilisine mutes |
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WO1997039116A1 (fr) | 1996-04-12 | 1997-10-23 | Novo Nordisk A/S | Granules contenant une enzyme et technique de production |
WO1998017767A1 (fr) | 1996-10-18 | 1998-04-30 | The Procter & Gamble Company | Compositions detergentes |
WO2000001793A1 (fr) | 1998-06-30 | 2000-01-13 | Novozymes A/S | Nouveau granule ameliore contenant des enzymes |
WO2000063336A1 (fr) | 1999-04-19 | 2000-10-26 | The Procter & Gamble Company | Particules composites enzymatiques avec barrière acide et couche d'enduction barrière physique |
WO2004067739A2 (fr) | 2003-01-27 | 2004-08-12 | Novozymes A/S | Stabilisation de granules |
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WO2011005827A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Compositions contenant des co-particules dagent de blanchiment |
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WO2011005813A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Procédé pour laver des textiles à l'aide d'une composition détergente de lavage sous forme de tablettes |
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WO2011005833A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Particules stratifiées et compositions les comprenant |
WO2011005910A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Procédé de lessive d'un tissu utilisant une composition détergente de lessive compactée |
WO2011009887A1 (fr) | 2009-07-24 | 2011-01-27 | Henkel Ag & Co. Kgaa | Ensemble tissu/adjuvant de lavage avec agents de blanchiment |
WO2011036146A1 (fr) | 2009-09-28 | 2011-03-31 | Henkel Ag & Co. Kgaa | Agent de prétraitement des taches |
WO2011060109A1 (fr) | 2009-11-11 | 2011-05-19 | The Procter & Gamble Company | Procédé de nettoyage |
US20110207646A1 (en) | 2010-02-25 | 2011-08-25 | Jose David Baez Chavez | Detergent Composition |
US20110212874A1 (en) | 2010-03-01 | 2011-09-01 | Michelle Meek | Composition Comprising Co-Bleach Particle and Amylase |
EP2380481A2 (fr) | 2010-04-23 | 2011-10-26 | The Procter & Gamble Company | Produit de lave-vaisselle automatique |
WO2011133380A1 (fr) | 2010-04-19 | 2011-10-27 | The Procter & Gamble Company | Composition détergente pour le linge comprenant des particules d'agent de blanchiment en suspension dans une phase liquide continue |
-
2012
- 2012-01-25 WO PCT/EP2012/051097 patent/WO2012101149A1/fr active Application Filing
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WO1987007292A1 (fr) | 1986-05-21 | 1987-12-03 | Novo Industri A/S | Enzymes detergents enrobes |
WO1989006279A1 (fr) | 1988-01-07 | 1989-07-13 | Novo-Nordisk A/S | Genes de subtilisine mutes |
WO1997023606A1 (fr) | 1995-12-22 | 1997-07-03 | Genencor International, Inc. | Granules enrobees contenant des enzymes |
WO1997039116A1 (fr) | 1996-04-12 | 1997-10-23 | Novo Nordisk A/S | Granules contenant une enzyme et technique de production |
WO1998017767A1 (fr) | 1996-10-18 | 1998-04-30 | The Procter & Gamble Company | Compositions detergentes |
WO2000001793A1 (fr) | 1998-06-30 | 2000-01-13 | Novozymes A/S | Nouveau granule ameliore contenant des enzymes |
WO2000063336A1 (fr) | 1999-04-19 | 2000-10-26 | The Procter & Gamble Company | Particules composites enzymatiques avec barrière acide et couche d'enduction barrière physique |
WO2004067739A2 (fr) | 2003-01-27 | 2004-08-12 | Novozymes A/S | Stabilisation de granules |
WO2009016123A1 (fr) | 2007-07-27 | 2009-02-05 | Unilever Plc | Perfectionnements aux parfums |
WO2009030600A1 (fr) | 2007-09-08 | 2009-03-12 | Unilever Plc | Perfectionnements se rapportant à des assouplissants pour tissus |
WO2009092699A1 (fr) | 2008-01-24 | 2009-07-30 | Unilever Nv | Compositions de détergent pour machine à laver la vaisselle |
WO2010006861A1 (fr) | 2008-07-14 | 2010-01-21 | Unilever Plc | Procédé pour le traitement de taches sur un tissu |
WO2010049187A1 (fr) | 2008-10-31 | 2010-05-06 | Henkel Ag & Co. Kgaa | Agent de lavage pour lave-vaisselle |
WO2010063688A1 (fr) | 2008-12-05 | 2010-06-10 | Henkel Ag & Co. Kgaa | Détergents |
WO2010084203A1 (fr) | 2009-01-26 | 2010-07-29 | Henkel Ag & Co. Kgaa | Article servant d'additif pour le lavage |
WO2010090915A1 (fr) | 2009-02-09 | 2010-08-12 | The Procter & Gamble Company | Composition détergente |
WO2010105961A1 (fr) | 2009-03-20 | 2010-09-23 | Henkel Ag & Co. Kgaa | Agent de lavage ou de nettoyage comportant éventuellement un complexe de métaux de transition généré in situ à pouvoir blanchissant renforcé |
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WO2011005813A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Procédé pour laver des textiles à l'aide d'une composition détergente de lavage sous forme de tablettes |
WO2011005910A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Procédé de lessive d'un tissu utilisant une composition détergente de lessive compactée |
WO2011005827A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Compositions contenant des co-particules dagent de blanchiment |
WO2011005623A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Composition détergente pour lessive comprenant de faibles taux d'agent de blanchiment |
WO2011005630A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Procédé de lessive d'un tissu utilisant une composition détergente de lessive compactée |
WO2011005905A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Composition solide de détergent pour le traitement des tissus légèrement alcaline, comprenant de l'acide phtalimido peroxy caproïque |
WO2011005833A1 (fr) | 2009-07-09 | 2011-01-13 | The Procter & Gamble Company | Particules stratifiées et compositions les comprenant |
DE102009033248A1 (de) | 2009-07-14 | 2010-05-06 | Henkel Ag & Co. Kgaa | Waschmittel für die Niedrigtemperaturwäsche von hochfunktionellen Materialien |
WO2011009887A1 (fr) | 2009-07-24 | 2011-01-27 | Henkel Ag & Co. Kgaa | Ensemble tissu/adjuvant de lavage avec agents de blanchiment |
WO2011036146A1 (fr) | 2009-09-28 | 2011-03-31 | Henkel Ag & Co. Kgaa | Agent de prétraitement des taches |
WO2011060109A1 (fr) | 2009-11-11 | 2011-05-19 | The Procter & Gamble Company | Procédé de nettoyage |
US20110207646A1 (en) | 2010-02-25 | 2011-08-25 | Jose David Baez Chavez | Detergent Composition |
US20110212874A1 (en) | 2010-03-01 | 2011-09-01 | Michelle Meek | Composition Comprising Co-Bleach Particle and Amylase |
WO2011133380A1 (fr) | 2010-04-19 | 2011-10-27 | The Procter & Gamble Company | Composition détergente pour le linge comprenant des particules d'agent de blanchiment en suspension dans une phase liquide continue |
EP2380481A2 (fr) | 2010-04-23 | 2011-10-26 | The Procter & Gamble Company | Produit de lave-vaisselle automatique |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015028567A1 (fr) * | 2013-08-28 | 2015-03-05 | Novozymes A/S | Granulé enzymatique contenant un agent de blanchiment fluorescent |
CN105473699A (zh) * | 2013-08-28 | 2016-04-06 | 诺维信公司 | 具有荧光增白剂的酶颗粒 |
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