EP0478684B1 - Granule d'addition au detergent et detergent - Google Patents

Granule d'addition au detergent et detergent Download PDF

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Publication number
EP0478684B1
EP0478684B1 EP90910607A EP90910607A EP0478684B1 EP 0478684 B1 EP0478684 B1 EP 0478684B1 EP 90910607 A EP90910607 A EP 90910607A EP 90910607 A EP90910607 A EP 90910607A EP 0478684 B1 EP0478684 B1 EP 0478684B1
Authority
EP
European Patent Office
Prior art keywords
granulate
detergent
enzyme
detergent additive
photobleaching
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.)
Expired - Lifetime
Application number
EP90910607A
Other languages
German (de)
English (en)
Other versions
EP0478684A1 (fr
Inventor
Per Falholt
Erik Kjaer Markussen
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.)
Novo Nordisk AS
Original Assignee
Novo Nordisk AS
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Filing date
Publication date
Application filed by Novo Nordisk AS filed Critical Novo Nordisk AS
Publication of EP0478684A1 publication Critical patent/EP0478684A1/fr
Application granted granted Critical
Publication of EP0478684B1 publication Critical patent/EP0478684B1/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
    • C11D3/38672—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
    • 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
    • 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
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0063—Photo- activating compounds

Definitions

  • the concept of incorporation of a photobleaching agent in a detergent is known, reference being made to e.g. DE-A-3430773, EP-A-119746, and EP-A-87833.
  • the photobleaching agent is inactive if not exposed to UV light, and thus, under normal conditions, the photobleaching agent will first be activated and function as a bleaching agent when the clean laundry is dried in the open. This is a clear advantage over the detergents with a normal bleach, which will function as a bleaching agent already in the washing solution and thus damage sensitive detergent additives, especially enzymes.
  • photobleaching agents in detergents in solid form are not without problems, though.
  • particles of pure photobleaching agent or particles of detergent additives, which contains photobleaching agents at the surface thereof will tend to adhere to the laundry due to a selective adhesion ability of the photobleaching agent to the laundry, and also such photobleaching agent will tend to stay with the laundry without being dissolved during the washing process.
  • Most photobleaching agents possess a very intense color, and such photobleaching agents will create a most undesirable staining of the laundry.
  • the photobleaching agent is colorless, the above indicated attachment thereof to the laundry during the washing process will create an uneven concentration of photobleaching agent on the laundry, and in that case an uneven overbleaching action will take place when the laundry is dried in the open.
  • the detergent additive granulate according to the invention is a co-granulate containing at least one enzyme and at least one photobleaching agent, the co-granulate being coated.
  • the photobleaching agent can be any photobleaching agent, e.g. Tinolux BBS, vide the following examples, zinc phthalocyanine sulfonate (ZPS), and aluminum phthalocyanine sulfonate (APS).
  • Tinolux BBS zinc phthalocyanine sulfonate
  • ZPS zinc phthalocyanine sulfonate
  • APS aluminum phthalocyanine sulfonate
  • Tinolux and the later indicated materials Arbocel, Speswhite, and Glascol are trade marks.
  • the detergent additive granulate according to the invention will fulfil the above objective in an especially advantageous manner, if produced by means of a drum granulator, as will later be described in more detail.
  • the detergent additive granulate can and will usually contain other components besides the components listed above, provided that these components do not damage the enzyme and/or the photobleaching agent.
  • aqueous fabric washing detergent which can contain both enzymes and a photobleaching agent.
  • this detergent is aqueous, and the above problem, which is solved according to the invention, does not appear at all in relation to aqueous detergents, which exhibit other problems, e.g. stability problems.
  • EP-A-119.746 describes a detergent powder which contains both photobleach and enzyme.
  • the first step during the production of this washing powder is the formation of the aqueous crutcher slurry, consisting of surfactants, builders, fillers, and a solution of the photobleach.
  • This crutcher slurry is spray-dried, whereby the so-called base powder is formed.
  • the enzyme which may optionally be added vide page 4, line 29 in EP-A-119.746) has to be added as enzyme containing particles separate from the base powder, due to the fact that the enzyme activity in the base powder would be reduced severely or lost completely, if the enzyme was added to the crutcher solution.
  • the EP-A-119.746 contains enzyme free, photobleaching agent containing particles and photobleaching agent free enzyme containing particles. It has been found that the problem of staining and overbleaching is not completely solved in relation to this prior art washing powder.
  • DE-A-28 13 198 describes a bleaching agent which contains a special photoactivator.
  • This bleaching agent is produced by co-granulation of all constituents of the bleaching agent to a co-granulate or by granulation of a single constituent on a basis detergent component, whereas according to the invention two sensitive constituents of the detergent are selected, i.e. the enzyme and the photobleaching agent, and co-granulated.
  • the detergent additive granulate according to the invention can be produced by co-granulation in many ways, e.g. as indicated in the following.
  • the photobleaching agent is added as an aqueous solution, preferably as part of the granulation water.
  • the usual coating agents may be used, e.g. the coating agents described in DK-A-0121/88, DK-A-1377/88, and DK-A-378/88.
  • the enzyme is one or more of the enzymes protease, amylase, lipase, cellulase, oxidase, and amidase. These are the most common enzymes used in the detergent additive.
  • detergent additive granulate according to the invention between 2 and 40% w/w of cellulose fibres are incorporated into the granulate.
  • a granulate of this kind can be produced according to US-A-4,106,991 (Novo Nordisk A/S, Denmark). In this manner a dust free granulate is obtained which can easily be produced in an industrial scale.
  • the invention comprises a detergent which contains the detergent additive granulate according to the invention.
  • the concentration of the detergent additive is between 0.05 and 5% w/w. In this manner the object of the invention is fulfilled, and also, the photobleaching effect is fully satisfactory.
  • Example 1 In the following the production of the detergent additive granulate according to the invention is illustrated in Examples 1, 4, 5, 7, 9, and 10, and the use of the detergent additive granulate is illustrated in Example 11.
  • a powder mixture containing a proteolytic enzyme and with the following composition 8.0 kg of SAVINASE® with an activity of 36.1 KNPU/g 6.0 kg of fibrous cellulose Arbocel BC 200 1.6 kg of kaolin, Speswhite ECCI 2.4 kg of carbohydrate binder 20.6 kg of finely ground sodium sulphate is transferred to a 130 liter Lodige mixer FM 130 and granulated with 9.7 kg of a granulation liquid made up by mixing of 2.0 kg of Tinolux BBS (liquid), Ciba-Geigy 0.9 kg of carbohydrate binder 7.0 kg of water all other conditions during the granulation being identical to Example 1 in US-A-4.106.991 (Novo Nordisk A/S, Denmark).
  • KNPU is an activity unit for proteolytic activity, described in the document AF 220/1-GB
  • KLU is an activity unit for lipolytic activity, described in the document AF 95/5
  • CSU is an activity unit for cellulolytic activity, described in the document AF 187/3
  • KNU is an activity unit for amylolytic activity, described in the document AF 207/1, whereby all the cited documents are available on request from Novo Nordisk, Novo Allé, DK-2880 Bagsvaerd, Denmark.
  • Tinolux BBS is a photobleaching agent, which is a derivative of tetrabenzo-tetraazaporphine.
  • the moist granulate is dried on a fluid bed to a water content below 1%, and the sieve fraction of the granulate between 300 ⁇ m and 900 ⁇ m is taken out as a product.
  • This product is coated with 6.2% of polyethylene glycol (PEG 4000) and 10% of kaolin (Speswhite, ECC) by means of the method described in Example 22 in US-A-4.106.991 (Novo Nordisk A/S, Denmark).
  • the granulate is further provided with a film coating consisting of 170 ppm of duasynic acid green and 0.25% of hydroxypropyl cellulose.
  • the final preparation exhibited a proteolytic activity of 5.7 KNPU/g.
  • a powder mixture containing a lipolytic enzyme and with the following composition 0.75 kg of LIPOLASE® with an activity of 860 KLU/g 2.25 kg of fibrous cellulose Arbocel BC 200 1.50 kg of bentonite ECCI ASB350 0.90 kg of carbohydrate binder 8,90 kg of finely ground sodium sulphate is transferred to a 50 liter Lödige mixer FM 50 and granulated with 3.4 kg of a granulation liquid made up by mixing of 0.7 kg of Tinolux BBS 0.7 kg of carbohydrate binder 2.0 kg of water
  • the granulation is carried out as described in Example 1, except for the size of the mixer.
  • the granulate is dried and sifted as described in Example 1, whereby a granulate with an activity of 31.2 KLU/g is obtained.
  • a powder mixture containing a cellulolytic enzyme and with the following composition 3.00 kg of cellulase with an activity of 5340 CSU/g 2.25 kg of fibrous cellulose Arbocel BC 200 0.60 kg of kaolin ECCI Speswhite 0.60 kg of carbohydrate binder 8,85 kg of finely ground sodium sulphate is transferred to a 50 liter Lödige mixer FM 50 and granulated with 3.4 kg of a granulation liquid made up by mixing of 0.83 kg of Tinolux BBS 0.30 kg of carbohydrate binder 3.00 kg of water
  • the granulation is carried out as described in Example 1, except for the size of the mixer.
  • the granulate is dried and sifted as described in Example 1.
  • Example 2 1 kg of dry sifted (300-1000 ⁇ m) granulate produced as described in Example 2 is coated in a 5 liter Lödige mixer according to the method described in US-A-4,106,991 (Novo Nordisk A/S, Denmark), example 22.
  • Example 4 1 kg of dry sifted (300-1000 ⁇ m) granulate produced as described in Example 3 is coated as described in Example 4.
  • Example 6 5 kg of a Tinolux/bentonite coated granulate produced as described in Example 6 is further coated with 100 g of bentonite and 45 g of Glascol LS22P (dry matter) by spraying with an emulsion/suspension consisting of 100 g of bentonite ASB 350 100 g of Glascol LS22P (45% microemulsion) 500 g of water by means of the same fluidized bed coating technique as described in Example 6.
  • Example 8 5 kg of a Tinolux coated granulate produced as described in Example 8 is further coated with 200 g of bentonite and 135 g of Glascol LS22P (dry matter) by spraying with an emulsion/suspension consisting of 200 g of bentonite ASB 350 300 g of Glascol LS22P (45% microemulsion) 1000 g of water by means of the same fluidized bed coating technique as described in Example 6.
  • a powder composition containing an amylolytic enzyme and with the following composition is prepared for extrusion according to Example 4 in US-A-4,661,452 (Novo Nordisk A/S, Denmark).
  • 0.500 kg of BAN with an activity of 4900 KNU/g 0.100 kg of titanium dioxide 0.275 kg of a carbohydrate binder 0.500 kg of calcium carbonate, Sturcal L 0.350 kg of anhydrous calcium sulphate 0.125 kg of sodium carboxymethyl cellulose, Hercules 7H 2.725 kg of finely ground sodium sulphate by spraying with 600 g Tinolux BBS containing 100 g of PVP K30 and finally spraying the moist mixture with 200 g of coconut monoethanol amide.
  • the hot (55°C) moist mixture is extruded using a pellet press type extruder (Simon-Heesen type Monoroll Labor).
  • a pellet press type extruder Simon-Heesen type Monoroll Labor.
  • the original Simon-Heesen pellet die with 8 mm holes is equipped with a screen plate with 0.8 mm holes on the inside, which screen is supported by the die.
  • the extrudate After extrusion the extrudate is allowed to cool by blowing cold air through it. After cooling to room temperature it is transferred to the Marumerizer®, which breaks the extrudate to a short sized noodle like product, which is compact and exhibits a well rounded surface. Finally the product is dried in a fludized bed drier.
  • the product is coated with a protective coating as described in example 22 of US-A-4,106,991 (Novo Nordisk A/S, Denmark) or in WO-A-89/08694 (Novo Nordisk A/S, Denmark) or in WO-A-89/08695 (Novo Nordisk A/S, Denmark).
  • This example is a spotting example illustrating the use of the detergent additive granulate according to the invention.
  • Granules from Example 1 are added to a solution of a standard powder detergent in a jar. A piece of white cotton textile is placed on the bottom of the jar. The spotting from the granules on the white textile is evaluated after 1 minute according to the grades shown in the legend.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Enzymes And Modification Thereof (AREA)

Claims (5)

  1. Granulé additif de détergent qui est un co-granulé contenant au moins une enzyme et au moins un agent de photoblanchiment, le co-granulé étant enrobé.
  2. Granulé additif de détergent selon la revendication 1, dans lequel l'enzyme est une ou plusieurs des enzymes protéase, amylase, lipase, cellulase, oxydase et amidase.
  3. Granulé additif de détergent selon les revendications 1 à 2, dans lequel sont incorporés entre 2 et 40 en masse/masse de fibres de cellulose.
  4. Détergent qui contient le granulé additif de détergent selon les revendications 1-3.
  5. Détergent selon la revendication 4, dans lequel la concentration du granulé additif de détergent est comprise entre 0,05 et 5 % en masse/masse.
EP90910607A 1989-06-21 1990-06-14 Granule d'addition au detergent et detergent Expired - Lifetime EP0478684B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DK3062/89 1989-06-21
DK306289A DK306289D0 (da) 1989-06-21 1989-06-21 Detergentadditiv i granulatform

Publications (2)

Publication Number Publication Date
EP0478684A1 EP0478684A1 (fr) 1992-04-08
EP0478684B1 true EP0478684B1 (fr) 1993-12-08

Family

ID=8118654

Family Applications (1)

Application Number Title Priority Date Filing Date
EP90910607A Expired - Lifetime EP0478684B1 (fr) 1989-06-21 1990-06-14 Granule d'addition au detergent et detergent

Country Status (16)

Country Link
EP (1) EP0478684B1 (fr)
JP (1) JPH04506229A (fr)
KR (1) KR920701410A (fr)
AT (1) ATE98295T1 (fr)
AU (1) AU641672B2 (fr)
BR (1) BR9007470A (fr)
DE (1) DE69005112T2 (fr)
DK (2) DK306289D0 (fr)
EG (1) EG19045A (fr)
ES (1) ES2046788T3 (fr)
MX (1) MX21242A (fr)
MY (1) MY105995A (fr)
NZ (1) NZ234159A (fr)
PT (1) PT94439B (fr)
TR (1) TR27368A (fr)
WO (1) WO1990015856A1 (fr)

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5167854A (en) * 1985-08-21 1992-12-01 The Clorox Company Encapsulated enzyme in dry bleach composition
US5376288A (en) * 1989-06-21 1994-12-27 Noro Nordisk A/S Detergent additive granulate and detergent
GB9220669D0 (en) * 1992-09-30 1992-11-11 Unilever Plc Detergent composition
DK5593D0 (da) * 1993-01-18 1993-01-18 Novo Nordisk As Granulat
WO1995033039A1 (fr) * 1994-05-31 1995-12-07 Novo Nordisk A/S Preparation inhibant le transfert des couleurs et composition detergente contenant une telle preparation
CN1156571C (zh) 1998-10-09 2004-07-07 花王株式会社 酶颗粒
DE19855677A1 (de) * 1998-12-02 2000-06-08 Henkel Kgaa Herstellung Aufheller-haltiger Waschmittel-Granulate
US6767882B1 (en) 1999-06-21 2004-07-27 The Procter & Gamble Company Process for producing coated detergent particles
BR0011800A (pt) * 1999-06-21 2002-03-26 Procter & Gamble Processo para a produção de partìculas de detergente revestidas
IT1319655B1 (it) 2000-11-15 2003-10-23 Eurand Int Microsfere di enzimi pancreatici con elevata stabilita' e relativometodo di preparazione.
GB2374082A (en) * 2001-04-04 2002-10-09 Procter & Gamble Particles for a detergent product
GB0314210D0 (en) 2003-06-18 2003-07-23 Unilever Plc Laundry treatment compositions
TR201808840T4 (tr) 2007-02-20 2018-07-23 Allergan Pharmaceuticals Int Ltd Stabil sindirim enzimi bileşimleri.
WO2009109856A2 (fr) 2008-03-07 2009-09-11 Axcan Pharma Inc. Procédé pour détecter un parvovirus infectieux dans des préparations pharmaceutiques
AU2011309763B2 (en) † 2010-10-01 2015-08-13 Allergan Therapeutics LLC Enteric coated, low- strength pancrelipase formulations
WO2013021359A1 (fr) 2011-08-08 2013-02-14 Aptalis Pharma Ltd. Procédé de test de dissolution de compositions solides contenant des enzymes digestives
EP3030257B1 (fr) 2013-08-09 2020-02-19 Allergan Pharmaceuticals International Limited Composition d'enzymes digestives appropriée pour une administration entérale
JP2017519490A (ja) 2014-06-19 2017-07-20 アプタリス ファルマ リミテッド 膵臓抽出物からのウイルス汚染の除去方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1075405A (fr) * 1977-03-28 1980-04-15 John F. Goodman Agent de blanchiment photosensible, composition et procede connexes
GR78065B (fr) * 1982-02-19 1984-09-26 Unilever Nv
GB8304631D0 (en) * 1983-02-18 1983-03-23 Unilever Plc Detergent powder

Also Published As

Publication number Publication date
NZ234159A (en) 1992-01-29
EP0478684A1 (fr) 1992-04-08
DE69005112D1 (de) 1994-01-20
ATE98295T1 (de) 1993-12-15
WO1990015856A1 (fr) 1990-12-27
DK306289D0 (da) 1989-06-21
MY105995A (en) 1995-02-28
MX21242A (es) 1993-11-01
AU5960190A (en) 1991-01-08
BR9007470A (pt) 1992-06-16
ES2046788T3 (es) 1994-02-01
AU641672B2 (en) 1993-09-30
DE69005112T2 (de) 1994-04-14
TR27368A (tr) 1995-01-17
PT94439A (pt) 1991-02-08
EG19045A (en) 1994-12-30
PT94439B (pt) 1997-02-28
JPH04506229A (ja) 1992-10-29
KR920701410A (ko) 1992-08-11
DK0478684T3 (da) 1994-04-18

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