EP0404806B1 - Composition particulaire stabilisee - Google Patents

Composition particulaire stabilisee Download PDF

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Publication number
EP0404806B1
EP0404806B1 EP19890903702 EP89903702A EP0404806B1 EP 0404806 B1 EP0404806 B1 EP 0404806B1 EP 19890903702 EP19890903702 EP 19890903702 EP 89903702 A EP89903702 A EP 89903702A EP 0404806 B1 EP0404806 B1 EP 0404806B1
Authority
EP
European Patent Office
Prior art keywords
composition
coating
particles
component
clay
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
Application number
EP19890903702
Other languages
German (de)
English (en)
Other versions
EP0404806A1 (fr
Inventor
Erik Kjaer Markussen
Per Falholt
Howard Goodman
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.)
Novozymes AS
Original Assignee
Novo Nordisk AS
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
Priority claimed from DK137888A external-priority patent/DK137888D0/da
Priority claimed from DK137788A external-priority patent/DK137788D0/da
Application filed by Novo Nordisk AS filed Critical Novo Nordisk AS
Priority to AT89903702T priority Critical patent/ATE73484T1/de
Publication of EP0404806A1 publication Critical patent/EP0404806A1/fr
Application granted granted Critical
Publication of EP0404806B1 publication Critical patent/EP0404806B1/fr
Expired 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
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0084—Antioxidants; Free-radical scavengers
    • 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
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • C11D3/126—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite in solid compositions
    • 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
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3937—Stabilising 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
    • C11D3/40—Dyes ; Pigments
    • C11D3/42—Brightening agents ; Blueing agents

Definitions

  • the invention relates to a particulate composition
  • a particulate composition comprising:
  • the invention relates to such a composition with improved stability during storage of component (1).
  • the invention also relate to particles of an enzyme or an optical brightener for use in said composition and to a method of producing said composition or particles.
  • Particulate detergents containing particles of an enzyme mixed with separate particles of a bleaching agent or a detergent builder are commonly used. It is know that the latter components may negatively affect the storage stability of the enzyme.
  • the prior art suggests coating of the particles of the enzyme. It is know that the coating material needs to be carefully selected since it must one hand protect the enzyme and on the other hand release the component rapidly when the detergent is dissolved.
  • WO 87/07292 (Novo) teaches that the use of an enteric coating on enzyme particles improves the stability in detergent with bleach; the enteric coating material dissolves at the pH of the detergent solution. However, we have found that this does not always give sufficient storage stability.
  • an enzyme in a particulate composition can be stabilized in the above-mentioned mixed composition by applying a clay coating to one or both components.
  • Clay coating has previously been applied to other components, e.g. bleach activator (EP 51,987), but the use of this coating to the components considered here is novel.
  • the invention provides a particulate composition comprising:
  • the invention also provides a particulate product comprising an enzyme for use in the above composition, characterized by having a coating containing clay.
  • the invention further provides a method for producing said composition or said particulate product, wherein the particles to be coated and an aqueous dispersion of the coating agent are introduced into a fluid bed drying apparatus, whereafter the material leaving the apparatus is collected as the product.
  • the invention provides a method for producing said composition or said particulate product, comprising introducing the particles to be coated and the coating agent together with water and a binder into a mixer, followed by drying.
  • Typical examples of particulate compositions according to the invention are cleaning compositions, such as detergents and laundry bleaches.
  • composition of the invention contains separate particles of component (1) and (2) as defined above.
  • the latter end to destabilize the former during storage.
  • one or both is/are coated with clay.
  • the particulate composition of the invention may obviously contain more than one type of particles of component (1) and/or component (2), in which cas one or more may be coated according to the invention.
  • Component (1) is an enzyme, which is commonly used in detergents.
  • Detergent enzymes are generally microbial, e.g. proteases, amylases, cellulases and lipases.
  • Typical examples of detergent enzymes are: proteases derived from Bacillus (e.g. from B. licheniformis , from alkalophilic strains according to US 3,723,250 or subtilisin Novo) or Fusarium (e.g. F.oxysporum ); amylase derived from Bacillus , especially B. amyloliquefaciens ( B. subtilis or B. licheniformis ; cellulase derived from Humicola , especially H. insolens ; lipase derived from Pseudomonas (e.g. Ps.
  • compositions of the invention typically contain 0.005-5%, e.g. 0.01-2% and especially 0.1-1.5% by weight of particles containing component (1).
  • Component (2) is a bleaching agent of the peroxy type, or a detergent builder.
  • Typical bleaching agents of the peroxy type are organic and inorganic peracids and salts thereof, e.g sodium perborate, sodium percarbonate, potassium persulphate, magnesium peroxy phthalate and diperoxy dodecane dioic acid.
  • Typical detergent builders are sodium or potassium salts of tripolyphosphoric acid, citric acid, zeolite, ethylenediamine tetraacetic acid (EDTA), diethylene triamine pentaacetic acid (DTPA), and nitrilo triacetic acid (NTA).
  • EDTA ethylenediamine tetraacetic acid
  • DTPA diethylene triamine pentaacetic acid
  • NTA nitrilo triacetic acid
  • the particles containing component (2) will typically be present in amounts above 0.5%, e.g. above 1% and especially above 2% by weight.
  • the amount of component (2) may be more than 50%, and even more than 80%, e.g. in laundry bleaches.
  • the clay used in the coating is preferably a layered clay of the smectite type, such as montmorillonite or bentonite.
  • ASB e.g. ASB 350 Powder and ASB 350S Powder (ECC International Ltd., St. Austell, Cornwall, England).
  • the coating material used in the invention may consist essentially of clay, or it may comprise binders, colouring agents (such as TiO2), etc.
  • Conventional binders may be used, e.g. polyvinyl pyrrolidone, polyvinyl alcohol, cellulose derivatives (such as hydroxypropyl-, carboxymethyl- or methyl-cellulose) or carbohydrates (such as dextrin, starch hydrolysates, mono- and di-saccharides and sugar alcohols). If a binder is used, the amount will typically be in the range 1-30% of the coating material.
  • the amount of coating material should generally be above 0.1%, preferably above 0.5% and most preferably above 2% by weight of the coated particles.
  • the clay types used in the invention may be useful detergent ingredients in their own right, acting as antiredeposition agents. To obtain this effect, it is generally preferred that the amount of clay makes up 0.1-20% of the total weight of the composition of the invention.
  • the clay coating applied to the enzyme according to the invention may additionally comprise an antioxidant.
  • the antioxidant may be a thiosulphate, a sulphite, a bisulphite, ascorbic acid or an ascorbate, the salts being preferably sodium or ammonium salts.
  • the enzyme may have an additional protective coating, e.g. consisting of or containing a low-melting wax (such as polyethyleneglycol), enteric coating according to WO 87/02979, a mono-or diglyceride or a sorbitan ester.
  • a low-melting wax such as polyethyleneglycol
  • enteric coating according to WO 87/02979
  • a mono-or diglyceride or a sorbitan ester may both be applied to the same particles of enzyme, with either coating as the top coating.
  • the additional coating may be applied to the enzyme and the clay coating to component (2).
  • the particles to be coated according to the invention are preferably granulated. Granulation may be done according to methods known in the art, e.g. NL-C 167,993 (Novo), US 4,106,991 (Novo) or US 4,661,452 (Novo).
  • the particle size is preferably such that at least 90% lie in the range 3-2000 ⁇ m.
  • at least 90% will usually lie in the range 250-2000 tzar (standard granulate) or in the range 100-400 ⁇ m (microgranulate).
  • the coating according to the invention can be applied by means of any fluid bed method, e.g. a usual fluid bed process, a Wurster bed process or a rotor bed (Glatt) process ( vide e.g. David M. Jones, "Factors to consider in fluid-bed processing", Pharmaceutical Technology, April 1985).
  • the fluid bed method can be carried out batch wise or continuously.
  • the coating can be applied by introducing the particles and the coating agent together with water and a binder into a mixer, followed by drying (e.g. fluid-bed drying).
  • the mixer may be a Lodige mixer or any type of granulator described in US 4,106,991 at col. 4.
  • the coating agent is introduced as a dry powder, and the binder as an aqueous solution or dispersion.
  • the amount of water should be adjusted so as to avoid agglomeration on one hand, and avoid excessive dust on the other hand.
  • the particles may be introduced first, and the coating agent and binder later, either continuously or intermittently.
  • a base (uncoated) granulate of alkaline protease was prepared with the following composition:
  • the granulate was prepared as described in Example 1 of US 4,106,991, using pure water as granulating agent. After drying, the granulate was sieved, and the fraction between 300 and 900 ⁇ m was collected.
  • Part of the above base granulate was coated with bentonite which was sealed to the granulate surface with carbohydrate binder, as follows: 15 kg of the base granulate was introduced into a Lodige mixer FM 50. 5 kg of bentonite ASB 350 ECC was dosed continuously by the use of a self-regulating loss-in-weight feeding system into the mixer which ran at 95 rpm during the whole layering process. The feeding rate of the bentonite was 50 kg/h.
  • part of the base granulate was coated with PEG as described above, to represent a prior-art coated granulate.
  • Storage stability tests were carried out by adding granulate to a powder detergent with 25% perborate, storing this at 37°C and 70% relative humidity, and determining the residual protease activity. Results are expressed in percentage of initial activity. The storage tests were run in 2 series.
  • results show a marked improvement of storage stability in samples coated according to the invention.
  • the prior-art coating shows no improvement over the uncoated granulate.
  • a base granulate oF alkaline protease was prepared and sieved as in Example 1, except that the following composition was used:
  • 15 kg of the base granulate was coated with 5 kg of bentonite ASB 350 and sealed with 0.45 kg of carbohydrate binder in the following manner.
  • the base granulate was introduced into a Lodige mixer FM 50.
  • the coating/layering was applied with continuous mixing and alternately applying bentonite and binder solution ( 25% carbohydrate in water) in such a balanced way that the charge was neither too sticky nor contained a substantial amount of free bentonite powder.
  • the actual sequences and amounts of material were:
  • the granulate was finally dried to a water content below 1% and sieved to between 300 ⁇ m and 100 ⁇ m.
  • a base granulate of alkaline protease prepared as in Example 1 was coated with a layer of bentonite ASB 350 and sodium thiosulphate by a conventional fluid-bed process.
  • 350 g of bentonite and 350 g of sodium thiosulphate were dispersed/dissolved in water and sprayed onto 7 kg of base granulate in a Glatt WSG 5 fluid-bed with continuous layering and drying (Air inlet temperature 50°C, air outlet temperature 35°C). The process was completed by a 5 min. drying period with air inlet temperature 50°C.
  • the granulate was hereafter coated with 5% glyceryl stearate/palmitate (Grindtek MSP 90, Grindsted Product) (TM) and 12.5% TiO2:kaolin as described in Example 1 for PEG.
  • Example 1 Comparison of the above results with Example 1 shows that incorporation of thiosulphate and monoglyceride gives a further improvement of the storage stability obtained with bentonite coating.
  • Lipase was produced according to EP 305,216 and concentrated by ultrafiltration and evaporation.
  • the resulting liquid lipase concentrate had an activity of 520,000 LU/g (see EP 305,216).
  • the bentonite coated lipase granulate showed 2% loss of activity after 4 days storage and 11% loss after 10 days storage.
  • the base granulate showed 9% loss of activity after 4 days storage and 23% after 10 days storage.

Abstract

On stabilise pendant le stockage des particules contenant une enzyme ou un agent d'azurage optique dans un mélange avec des particules contenant un agent de blanchiment péroxy, un tensio-actif ou un adjuvant, en recouvrant d'argile par exemple d'argile smectique décolorante le formateur et/ou lesdites particules.

Claims (20)

1. Composition particulaire comprenant :
(1) des particules contenant une enzyme, mélangées avec
(2) des particules séparées contenant un agent de blanchiment du type peroxy ou un adjuvant de détergent
   la composition étant caractérisée en ce que les particules du premier/ou du second composant ont un revêtement contenant de l'argile.
2. Composition de nettoyage selon la revendication 1, de préférence un agent de blanchiment de laverie ou une composition de détergent.
3. Composition selon la revendication 1 ou 2, dans laquelle le composant (1) est une enzyme microbienne, de préférence une protéase, une amylase, une lipase ou une cellulase.
4. Composition selon les revendications 1 - 3, dans laquelle le composant (2) est un agent de blanchiment choisi dans le groupe d'un peracide organique ou minéral ou de son sel.
5. Composition selon la revendication 4, dans laquelle l'agent de blanchiment est du perborate de sodium, du percarbonate de sodium, du persulfate de potassium, du peroxy-phtalate de magnésium ou un acide diperoxy dodécane dioïque.
6. Composition selon les revendications 1 - 3, dans laquelle le composant (2) est un adjuvant de détergent choisi dans le groupe d'un sel de métal alcalin de l'acide tripolyphosphorique, de l'acide citrique, une zéolithe, un acide éthylène-diamine tétraacétique, un acide diéthylène-triamine pentaacétique ou un acide nitrilotriacétique.
7. Composition selon les revendications 1 - 6, dans laquelle les particules du composant (1) constituent 0,005-5 % en poids, de préférence 0,01-2 % et de façon plus préférentielle 0,1-1,5 % en poids du poids total de la composition.
8. Composition selon les revendications 1 - 7, dans laquelle les particules du composant (2) constituent plus de 0, 5 %, de préférence plus de 1 % et de façon plus préférentielle plus de 2 % du poids total de la composition.
9. Composition selon les revendications 1 - 8, dans laquelle le matériau de revêtement contient plus de 70 % et de préférence plus de 90 % d'argile.
10. Composition selon les revendications 1 - 9, dans laquelle le revêtement comprend de plus un liant, de préférence un hydrate de carbone, et de préférence dans une quantité de 1-30 % du poids du revêtement.
11. Composition selon les revendications 1 - 10, dans laquelle l'argile est une argile en couche, de préférence de la montmorillonite ou de la bentonite.
12. Composition selon les revendications 1 - 11, dans laquelle la quantité du revêtement constitue plus de 0,1 %, de préférence plus de 0,5 % et de façon plus préférentielle plus de 2 % du poids des particules revêtues.
13. Composition selon les revendications 1 - 12, dans laquelle l'argile contenue dans le revêtement constitue 0,1-2 % en poids de la composition totale.
14. Composition selon les revendications 1 - 13, dans laquelle les particules du composant (1) comprennent de plus un revêtement protecteur, de préférence contenant ou consistant en une cire (avec un point de fusion de préférence supérieur à 35°C), une substance entérique, un mono- ou diglycéride ou un ester de sorbitan.
15. Composition selon les revendications 1 - 14, dans laquelle le revêtement d'argile est appliqué sur le composant (1) et ce revêtement contient également un agent de réduction, de préférence un sulfite ou un thiosufate.
16. Composition selon les revendications 1 - 15, dans laquelle plus de 90 % des particules revêtues se situent dans la plage de 2-3 000 µm et de façon plus préférentielle dans la plage de 250-2 000 µm.
17. Produit particulaire comprenant une enzyme pour l'utilisation dans la composition selon les revendications 1 - 16, caractérisé en ce qu'il possède un revêtement contenant de l'argile.
18. Produit particulaire selon la revendication 17, caractérisé de plus selon les revendications 3 ou 9 - 16.
19. Procédé pour la production de la composition selon les revendications 1 - 16 du produit particulaire des revendications 17 ou 18, dans lequel les particules sont revêtues et une dispersion aqueuse de l'agent de revêtement sont introduites dans un appareil de séchage à lit fluidisé après quoi, le matériau quittant l'appareil est recueilli sous la forme du produit.
20. Procédé pour la production de la composition des revendications 1 - 16 ou du produit particulaire selon les revendications 17 ou 18, comprenant l'étape consistant à introduire les particules à revêtir et l'agent de revêtement conjointement avec l'eau et un liant dans un mélangeur, opération suivie du séchage.
EP19890903702 1988-03-14 1989-03-13 Composition particulaire stabilisee Expired EP0404806B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT89903702T ATE73484T1 (de) 1988-03-14 1989-03-13 Stabilisierte teilchenzusammensetzung.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DK1378/88 1988-03-14
DK137888A DK137888D0 (da) 1988-03-14 1988-03-14 Stabiliseret partikelformet komposition
DK1377/88 1988-03-14
DK137788A DK137788D0 (da) 1988-03-14 1988-03-14 Som granulat foreliggende dertergentenzymprodukt, fremgangsmaade til fremstilling deraf, anvendelse deraf og detergent indeholdende et saadant produkt

Publications (2)

Publication Number Publication Date
EP0404806A1 EP0404806A1 (fr) 1991-01-02
EP0404806B1 true EP0404806B1 (fr) 1992-03-11

Family

ID=26065676

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19890903702 Expired EP0404806B1 (fr) 1988-03-14 1989-03-13 Composition particulaire stabilisee

Country Status (3)

Country Link
EP (1) EP0404806B1 (fr)
JP (1) JP2624860B2 (fr)
WO (2) WO1989008694A1 (fr)

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EP0862623A2 (fr) 1995-10-06 1998-09-09 Genencor International, Inc. Microgranule destine a des applications de l'industrie alimentaire
US7803604B2 (en) 2000-07-28 2010-09-28 Henkel Ag & Co. Kgaa Amylolytic enzyme extracted from Bacillus sp. A 7-7 (DSM 12368) and washing and cleaning agents containing this novel amylolytic enzyme

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US5376288A (en) * 1989-06-21 1994-12-27 Noro Nordisk A/S Detergent additive granulate and detergent
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EP0773984B1 (fr) * 1995-05-29 1999-11-03 Kao Corporation Substance granulee contenant une enzyme et son procede de preparation
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WO1989008694A1 (fr) 1989-09-21
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EP0404806A1 (fr) 1991-01-02

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