JPH05502584A - Enzyme-containing preparations and detergents containing the preparations - Google Patents

Abstract

The enzyme containing preparation contains at least one enzyme, whereby at least 50 % of the enzymatic activity of at least one enzyme is present in the preparation as enzyme crystals, preferably together with a stabilizing agent for the enzyme(s). The detergent contains this preparation. Both the preparation and the detergent can be a granulate or a slurry. Both the preparation and the detergent exhibit good stability and no discoloration.

Description

[Detailed description of the invention] Enzyme-containing preparations and detergents containing said preparations The present invention provides enzyme-containing preparations containing at least one enzyme. Enzyme-containing preparations containing the same and detergents containing the preparations. scope of claims As used herein as well as in the description, the term "preparation" refers to a granulate or a liquid slurry. It means either. The slurry may be anhydrous or substantially anhydrous or aqueous. Either is fine.

These enzyme-containing preparations are useful in various fields, including those involving digestion aids. They can be used in the field of detergents, but their main use can be found in the field of detergents. I can do that.

In this specification, along with the claims, the term "particulate matter" is used in its broadest sense. From small particles with dimensions on the order of magnitude of about loμm, about ICl11 It is to be understood to include tablets of dimensions having orders of magnitude.

Enzyme-containing granules are widely used in industry, mainly as dust-free additives for detergents. It is. For example, U.S. Patent 4,106,991, U.S. Patent 4,66L452, Reference is made to Japanese Publication No. 2.060.095 and British Patent L362,365. I can do it.

One of the major problems with enzyme-containing granules is that enzyme-containing granules cannot be mixed with other detergent ingredients. The storage stability of the enzyme is affected when mixed with Some aspects regarding the stability of enzyme activity Although a method has been proposed, the stability of enzyme activity in detergents containing enzyme granules is unknown. There is still room for improvement. Another problem with enzyme-containing granules is color. Na For example, if not coated with titanium oxide, most enzyme-containing granules It will change color.

A third problem with enzyme-containing granules is their odor. Enzyme-containing powder Even after fairly good purification of the fermentation broth, the final product is often undesirably strong. Indicates odor.

Anhydrous or substantially anhydrous slurries are primarily used as additives to liquid detergents. Widely used in industry. Aqueous slurries are used in the starch and food industries. It can be used as an additive to liquid detergents. If the slurry is water-based If the activity or ionic strength of the water in the slurry is Crystallization must be controlled so that the enzyme is maintained in crystalline form.

A major problem with liquid detergents is the stability of the enzymes added to them. how many Such stable systems have been used in attempts to overcome these problems. low Calcium formate and calcium borate stabilization are both useful in the field of pH preparation. It has been used and is still in use today. In the higher pn range, some Suppression methods have also been used. However, especially in assembled liquids, Aqueous encapsulation has been used (see British Published Patent No. 2.186,884A).

However, there is room for improvement in these stable systems. Large information regarding liquid enzyme-containing preparations The problem lies in the colors. Most liquid enzyme-containing preparations are colored due to impurities. It is usually a cloudy, pale brown color and the color varies somewhat from batch to batch. this thing means the following contents. i.e. a manufacturer of liquid detergent, if he sells, for example, a blue liquid detergent. If you want to manufacture a color, you will have to guarantee the color, and also Warranties can vary from corpus to corpus of liquid enzyme-containing preparations, and this is clearly a disadvantage. This is a point.

Odor is a problem both with spillage and also with liquid detergents.

Alternatively, some preparations may contain allergenic impurities and therefore a purer preparation may Required.

It is thus an object of the present invention to provide improved stability and also to be colorless or almost colorless. In addition, preparations using enzymes that are highly pure and have no odor problems, and such enzymes. The object of the present invention is to provide detergents containing preparations with agents.

The enzyme-containing preparation according to the invention which contains at least one enzyme At least 50% of the enzyme activity of the seed enzyme is present in the preparation as enzyme crystals. It is characterized by.

Surprisingly, the following was discovered. That is, the enzyme-containing preparation according to the present invention is have similar good enzyme stability when present in detergents or another similar However, it has better enzyme stability than enzyme-containing preparations that are somewhat less pure. More than normal It is estimated as below. That is, certain impurities from the fermentation broth stabilize the enzyme, Purifying the enzyme too much would therefore be detrimental to enzyme stabilization.

This assumption is correct.

However, if the pure enzyme can be maintained as crystals in the preparation according to the invention, The stability is almost equal or better than that of the less pure preparation. Something was discovered. Furthermore, the following contents were discovered. After enzyme crystallization, impurities If carried out without the introduction of enzymes, the enzyme-containing preparation according to the invention It has different color and odor properties.

It should be understood as follows. i.e. if the normal enzyme starting material, i.e. the normal ratio Enzymes in the form of amorphous powders with relatively large amounts of impurities, or enzyme solutions or slurries. The enzyme is in the form of an enzyme starting material (where at least 50% of the enzyme activity is present as enzyme crystals), the enzyme-containing preparation according to the invention The product can be manufactured using normal methods. If the preparation is a granular material, such use A non-limiting list of available granulation methods can be found in the aforementioned U.S. Pat. No. 4,106,991; U.S. Patent 4,661. ．． 452, German Publication No. 2,060,095 and British Pat. It is 1.362,365.

Preferred forms of enzyme crystals are disclosed in pending patent application no. 847, filed on the same date as the present application. /90 and 84.8/90 (applicant reference number 3411.010-DK and 3 411.020). Other types of enzymes in enzyme-containing preparations Crystals are known per se. Danish patent 872/86, US patent 4.699.8 82 and Nordlov, J. H., et al. (Crystallin Enzymes, 2 nd edition, New York, 1948). Also, Sig Machical Co., Ltd. (P, O, Box 14508.SL).

See recent catalogs available from Louis, MO, LISA).

Another advantage associated with the preparation according to the invention is that, together with the chlorine in the tap water, the cleaning flow It can be found in the cleaning process at home. For a cleaning float like this In this case, the enzyme will be consumed at the beginning of the wash cycle, and the crystallized enzyme will pass through. This enzyme dissolves more slowly in the wash float than commonly used enzymes. The enzyme in the preparation according to the invention is present in dissolved form before some of the chlorine is consumed. will not be present and the enzyme will therefore be protected from inactivation by chlorine.

This will be shown later in the specification.

In a preferred embodiment of the preparation according to the invention, the preparation contains stabilizers for enzymes. contains. In this way, further improvements in the stability of the enzyme can be obtained. Granular matter PV When P (polyvinylpyrrolidone) is used; slurry against microbial growth In the case of preservatives, sucrose and Ca'' can be used as stabilizers.

According to a preferred embodiment of the preparation according to the invention, the preparation contains protease and at least Both contain one type of other enzyme, in which virtually 100% of the proteolytic activity is present in the crystals. It exists as.

Only small amounts of crystalline protease will be dissolved in the preparation according to the invention, or Nor will anything dissolve. Therefore, other enzymes or The stability of other enzymes will be improved in this manner. Moshi protease is Savinase (registered trademark), and the preparation is When containing Lipolase (registered trademark) as another enzyme In addition, if the preparation is a slurry, the preparation (containing crystalline savinase) ), the lipase was found to exhibit superior stability.

The present invention contains a protease and at least one protease-sensitive enzyme. In preferred embodiments of such preparations, substantially 100% protease-sensitive fermentation The protease-sensitive enzyme is present as crystals. just a small amount of protea enzyme-sensitive enzymes may be dissolved in the preparation according to the invention, or alternatively some of them may be Even the amount of water will not dissolve. Therefore, the protease content in the preparation according to the invention The stability of the competent enzyme will be improved in this manner. Moshi protea The enzyme is Savinase (registered trademark), and the preparation is lipophilic. - Contains Lipolase (registered trademark) as other enzymes, Furthermore, if the preparation is a granular material, the preparation (with crystalline lipase) In response, lipases were found to exhibit superior stability.

In a preferred embodiment of the preparation according to the present invention, 90% or more of the crystals are 0. 1am -500um, preferably Ipm-100um. Like this The crystals are co-pending patent application number 847/90 filed on the same day as this application and 848/90 (applicant reference numbers 3411.010-DK and 3411.020 -DK), but they can also be produced by other crystallization methods. .

In a preferred embodiment of the preparation according to the invention, the enzyme is protease, lipase, amylase, cellulase, hemicellulase, pectinase, amidase or oxidases or protein-processed variants thereof. These enzymes are additives in detergents. It is an enzyme commonly used as

In a preferred embodiment of the preparation according to the invention, the enzyme is a protease; Rotease is a subtilisin type protease. An example of this is Sabina Savinase (registered trademark), Esperase (registered trademark), Alcalase (registered trademark), subtilisi Subtilisin N0VO or protein-treated variants thereof. child These enzymes are the preferred proteases in detergents.

In a preferred embodiment of the preparation according to the invention, the enzyme is a lipase; Lipolase (registered trademark).

In a preferred embodiment of the preparation according to the invention, at least one of the enzymes The enzyme activity is preferably at least 75%, preferably at least 90% of all enzymes. Present in granules as enzyme crystals. The stability of such preparations is excellent. Ru.

In a preferred embodiment of the preparation according to the invention, the preparation is a granulate. This preparation The product is well suited as an additive to detergents in the form of particles Th.

In a preferred embodiment of the preparation according to the invention, the preparation is a slurry.

In a preferred embodiment of the preparation as a slurry, the slurry is anhydrous or Virtually anhydrous.

In a preferred embodiment of the preparation as a slurry, the slurry is aqueous.

In a preferred embodiment of the preparation according to the invention, the preparation is used as a detergent additive. It will be done. This is the main use of the preparation according to the invention.

It also comprises a detergent containing the preparation according to the invention.

In a preferred embodiment of the detergent according to the present invention, the detergent is solid and further according to the present invention 0.00110 μ of enzyme protein per gram of detergent, preferably per gram of detergent. 0.005-5 μ of enzyme protein, most preferably 0.01-1 μ per gram of detergent. Contains enzyme protein. These concentrations depend on the strength of the enzyme in the granulate according to the present invention. degree can usually be obtained by adding 0.0 to 10% w/w granules to the detergent. Probably.

In a preferred embodiment of the detergent according to the present invention, the detergent is liquid and further according to the present invention Anhydrous or substantially anhydrous slurry containing 0.001-10 μg of enzyme per gram of detergent. Protein, preferably 0.005-5 μg of enzyme protein per gram of detergent, most preferably is contained in an amount of 0.01-1 μg of enzyme protein per gram of detergent. liquid detergent like this indicates a satisfactory stability of the enzyme.

The use of binders with respect to the granulate preparations according to the invention is necessary and furthermore optional. Binders such as Riko are carbohydrate binders such as dextrin or cellulose. Rose derivatives such as hydroxypropylcellulose, methylcellulose or C I'm an MC.

Example Example 1 0.5 kg of crystalline Savinase (SAVINA) with an activity of 244 KNPU/g. SE) (registered trademark), 1.5kg Hentonite ASB350 (ECCI) , 2.2 kg of fibrous cellulose, ARBOCEL BC200, and 9.1 kg 13.3 kg of a powder composition having a formulation of finely divided sodium sulfate of 3.0 k g water, 0.15 kg polyvinylpyrrolid 7 to 30 and 1.35 kg (7) charcoal Ludige mixer with 4-5 kg of binder solution consisting of hydrate binder. - Granulate in FM50. Granulation is described in Example 1 of U.S. Pat. No. 4,106,991. It is done in the same way when it is loaded.

Savinase (registered trademark) is US Pat. No. 3,723,25 Alkali Baccilius pro- duced similarly as shown in 0. It's Tease. Also, Savinase (registered trademark), B54 Product sheet for 5 b-CB, March 1988 (Novo Nordis (available on request from Company K).

The KNPU protein lytic activity unit is presented in AFIOl, 10, which requires available from Nova Nordisk (Denmark).

The granulate is dried in a fluidized bed to less than 1%, after which the light colored granulate is reduced to a particle size of 2 obtained with cloth 11% > 1180μm 17%　＞　100100 0a%〉〉850μm 40%〉710μm 56%〉〉600μm 77%〉〉〉500μm 86%〉〉420μm 93%〉〉355μm 2.4%〈300IJm It has an activity of 7.3KNPU/g and is also a Hunter Power Larcodite ( It has L:a:b)=(79,6:1.3+11.3).

Finally, the granules are sieved to obtain a product having a particle size of 300 μm to 1000 μm, Then a 1:1 mixture of 7% PEG4000 and 12% TiO□ and kaolin was added. using the method described in Example 22 of U.S. Pat. No. 4,106,991. Ta.

Example 2 Livolase (L) containing crystalline Lipolase (registered trademark) ipoJase) (Registered commercial product) Preparation of 100T granular material. Introducing into mixer FM50: 2, Okg Hentonite ASB 3503, O kg of fiber cellulose, Arbocel BC2002, 1 kg of carbohydrate bis Under 0.63kg Crystalline Lipolase (Registered Trademark 1) (EP2 Lipolase (registered trademark) manufactured according to 38023 ) 12.3 kg of crushed NazSOa Spray the mixed dry ingredients using 3.6 kg of water. wet mixture, us Similar to the description in Example 1 of patent 4,106.991, from a multi-cent knife Subject to compression and granulation effects.

Once the granulation is complete, the granulate is dried in a fluidized bed and then the defined product is (in this case 300-900 μm) are separated for quality testing. Less than specified dimensions parts (which will not be processed) and parts with dimensions exceeding the specifications (which will be crushed) ) to recirculate.

Color is measured according to the Hunter Love Scale (AF78): L=70.1, a= o, 4, b-12,0° The above product part was tested according to U.S. Patent 4.10 for storage stability test Coat according to Example 22 of 6.991.

Example 3 Amorphous ribolase (registered trademark) was included as a control for comparison. Preparation of Lipolase® LOOT Granules with.

Produced according to Example 2 with the following formulation: 2.0 kg of Hentonite ASB 35 03.0kg fibrous cellulose, Arbocel BC2002, 1kg carbon water chemical binder 0.63 kg amorphous ribolase (Lipolase) (registered trademark) 9, 7 kg of crushed Naz SO4 Spray the mixed dry ingredients using 3.0 kg of water.

Color coordination Tony L=68.0. a=0.7, b-15,0° The color of the preparation of Example 2 (Crystalline Lipolase®) is From the color of the preparation of No. 3 (Amorphous Lipolase (registered trademark)) It's also brighter.

Product parts are coated for storage stability testing.

The storage stability of the coated granules obtained according to Examples 2 and 3 was tested using accelerated conditions. Experience: Add 2% of the particulate matter to a European heavy duty detergent and then store it in a sealed container at 50°C. save. Activity was measured after 0, 1, 3 and 7 days and then calculated as a percentage. do.

Residual activity (%) 1st 3rd 7th Example 2: Crystalline lipolase (Ljpolase) (Registered Trademark> 99 85 69 Example 3: Amorphous Livolor Ze (Ljpolase) (registered trademark) 90 82 59 example 4 Amorphous Savinase (registered trademark) and crystalline ribolase (L Savinase (registered trademark) containing ipolase (registered trademark) (registered trademark)/ribolase (Ljpolase) (registered trademark) 3.0150T Preparation of grains.

Produced according to Example 2 using the following formulation: 2.0 kg of bentonite ASB 35 03.0kg fibrous cellulose, Arbocel BC2002, 1kg carbon water chemical binder 0.32kg crystalline Lipolase (registered trademark) 1.84k Grinding of 10.7 kg of amorphous Savinase (registered trademark) NazSO4 Spray the mixed dry ingredients using 3.3 kg of water.

Product parts are coated for storage stability testing.

Example 5 Amorphous Savinase (registered trademark) and amorphous ribolase ( Savinase containing Lipolase (registered trademark) (Registered Trademark)/Lipolase (Registered Trademark) 3. .

Preparation of 150T cogranulate.

Produced according to Example 2 using the following formulation: 2.0 kg of Hentonite ASB 3 502.1kg carbohydrate binder 1.6kg of amorphous ribolase (Lipolase) (registered trademark) 1.84k g amorphous Savinase (registered trademark) 9, 7kg (7) Spray the crushed Naz so4 mixed dry ingredients using 3.3 kg of water.

Product parts are coated for storage stability testing.

Example 6 Crystalline Savinase (registered trademark) and amorphous ribolase (L Savinase (registered trademark) containing ipolase (registered trademark) (registered trademark)/Lipolase (registered trademark) 3.0150T Preparation of granules.

Produced according to Example 2 using the following formulation: 2.0 kg of Hentonite 8SB 3 503.0 Heron fiber cellulose, Arbocel BC2002, 1kg of carbon water chemical binder 1. 6 kg of amorphous ribolase (Lipolase) (registered trademark) 1.1. 0kg crushed Naz SO4 The mixed dry ingredients were suspended in 2.9 kg of water. 7kg crystal Sabina Savinase (registered trademark) filter cake (Denmark patent application) 847/90)).

Code product parts for storage stability testing.

Example 7 Crystalline Savinase (registered trademark) and Crystalline Lipolase (Li Savinase (registered trademark) containing (registered trademark)/Lipolase (registered trademark) 3.0150T co-granule Preparation of parables.

Produced according to Example 2 using the following formulation: 2.0 kg of Hentonite ASB 3 503.0kg fibrous cellulose, Arbocel BC2002, 1kg charcoal hydrate binder 0.32kg crystalline lipolase (registered trademark) 12.2k g of pulverized pJ az S Oa mixed dry ingredients were suspended in 3.0 kg of water. ,0. 7kg crystalline Savinase (registered trademark) filter - Spraying using Cake (manufactured according to Danish patent application 847/90) Ru.

Product parts are coated for storage stability testing.

Regarding the protease-sensitive enzyme Ripolase (registered trademark) The storage stability of the coated granules obtained according to Example 4-7 was determined under accelerated conditions. 24% of the granulate to be tested at 50°C was added to a European heavy duty detergent and Store in an airtight container. Activity was measured after 0, 1, 3 and 7 days and then Calculate as a percentage.

Residual activity of ribolase (%) 1st 3rd 7th In another example, the granulate obtained according to Examples 4-7 (protease-sensitive enzyme lysate) borase (Lipolase®)) under other promoting conditions. The 24% granulate tested below was added to a European heavy duty detergent and then washed at 37°C. Store in a closed container at C and 70% relative humidity. activity on days 0, 3, 7 and It is measured after 14 days and then calculated as a percentage.

Residual activity of ribolase (%) 3rd, 7th, 14th From the above table the best results are obtained for crystalline lipase.

Example 8 Savinase (S) containing crystalline Savinase (registered trademark) avinase) (registered trademark) 4. Preparation of OT granules.

Produced according to Example 2 using the following formulation: 2.0 kg of bentonite ASB 3 503.0 kg of fibrous cellulose, 8 rboceIBG, 2002.4 kg of charcoal hydrate binder 11.7kg crushed Naz SO4 The mixed dry ingredients were 2.2 kg of water and 0.11 kg of Naz.

1 or 2 kg of crystalline Savinase suspended in 4 and 0.2 kg of PVP K2O (5avinase) (registered trademark) Filter cake (Denmark patent issue 1' 847/90)).

Color cope innate: L=79.9, a=0.8, b=7.8° Example 9 Savinase containing amorphous Savinase (registered trademark) Preparation of Savinase® 4.0T Granules.

Produced according to Example 2 using the following formulation: 0.8 kg kaolin, 5 pesi+ hite3.0kg fiber cellulose, Arbocel 8C2003,0kg Amorphous Savinase (registered trademark) concentrate Dissolve 11.2 kg of crushed N az S O4 mixed dry ingredients in 3.0 kg of water. Understand 1. Using 8kg carbohydrate binder, 0.2kg PVP K2O and spray.

Color co-op inate: L=48.2, a=6.0. b-17,7゜ Apparently the preparation of Example 8 (Crystalline Savinase®) The color of the preparation of Example 9 (amorphous Savinase®) The color is brighter and for the purpose TiO2 is not needed in the preparation of Example 8. .

Example 10 Durazym containing crystalline Durazym (registered trademark) (1) Preparation of urazym (registered trademark) 6.0T granules.

Produced according to Example 2 using the following formulation: 0.7 kg of Hentonite ASB 3 501.0kg fibrous cellulose, Arbocel BC2000, 4kg charcoal hydrate binder 4. 3kg crushed Naz SO4 Mix the dry ingredients into 1. 5kg water, 0.07kg PVP K2O and 0.4 0°354 kg of crystalline Dourazyme suspended in kg of carbohydrate binder (Durazym) (registered trademark) Filter cake (Denmark patent application 8 47/90).

Color Cope Inate: L=82.5, a=1.0, b-amorphous Durazyme ( Durazym (Durazym) containing (registered trademark) Preparation of 6.0T Granules.

Produced according to Example 2 using the following formulation: 1.5 kg of bentonite ASB 3 503.25kg of fibrous cellulose, Arbocel BC2000, 9kg carbohydrate binder 7.7 kg of crushed N az S Oa 2.0 kg of amorphous Durazyme (Du razym> (registered trademark) mixed dry ingredients, 2.5 kg of water, 0.15 kg of Spray with PVP K2O and 0.5 kg carbohydrate binder.

Color cope innate: L=52.8, a=5.2, b=17.4° Apparently the preparation of Example 10 (crystalline Durazym®) The color of the preparation of Example 11 (amorphous Durazym®) )), and for the purpose, TiO2 is not necessary in the preparation of Example 10. Not necessary.

Example I2 Savinase (S) containing crystalline Savinase (registered trademark) avinase) (registered trademark) 4.0T granulate.

Manufactured using the following recipe according to Bone 2: 2.0 kg of bentonite 8SB 3 503.0 kg of fibrous cellulose, Arbocel BC2001, 2 kg of charcoal hydrate binder LL, 9 kg of crushed Na2S O40, 46 kg of dry crystalline Sabinase (S avinase) (registered trademark) mixed dry ingredients, 0.2 kg of PVP K2O and 1. Spray using 2-3 kg of water containing 2 kg of carbohydrate binder. Savinase containing crystallized Savinase (registered trademark) Preparation of Savinase® 4.0T Granules.

Produced according to Example 2 using the following recipe.

2.0kg Hetonite ASB 3503.0kg fiber cellulose, Arb ocel BC2002, 4kg carbohydrate binder 11.6 kg of crushed Na, So.

The mixed dry ingredients were mixed with O, 1 kg NazSO4 and 0.2 kg in 2.5 kg water. PVP K2O was suspended, 1. 5kg of crystalline Savinase ase) (registered trademark) Filter Cake (Danish patent application 847/90) Therefore, spray using

Example 14 Savinase containing amorphous Savinase (registered trademark) Preparation of Savinase® 6.0T Granules.

Produced according to Example 2 using the following formulation: o, skg kaolin, Speswh itel, 8kg fiber cellulose, Arbocel BC2002, 8kg Amorphous Savinase (registered trademark) 12.6 kg of crushed Na z　S○4 Dissolve the mixed dry ingredients in 3.6 kg of water and add 1.8 kg of carbohydrate binder; Spray with 0.2 kg of PVP K2O.

Example 1.2, measured for Savinase® The storage stability of the coated granules produced according to -14 is tested under accelerated conditions: 1% of the granulate was added to a European heavy duty detergent and then placed in a closed container at 50°C. Save to. Activity was measured after 0, 1, 3 and 7 days and then calculated as a percentage. Calculate.

Residual activity of savinase (%) 1st 3rd 7th Example 12: Dry crystal savinase (Savinase) (registered trademark) 60 58 52 Example 13: Crystal Savinase Ze (Savinase) (registered trademark) 68 57 49 Example 14: Amorphous Sabinase -ze (Savinase) (registered trademark) 60 51 42 Obviously crystal Sabinase The stability of Savinase (registered trademark) is similar to that of amorphous Savinase (Savinase). better than (registered trademark).

Example 15 This example shows further advantages with respect to chlorine-containing wash floats.

release rate expressed in seconds, i.e. to dissolve 50%, 90% and 95% of the enzyme. The required time interval is shown below.

Release rate (sec) 50% 90% 95% Example 12: Dry crystal savinase (Savinase) (registered trademark) 57 85 92 Example 13: Crystal Savinase Ze (Savinase) (registered trademark) 69 116 122 Example 11 Amorphous rust Nase (Savinase) (registered trademark) 43 62 59 Obviously crystal Sabinase Savinase (registered trademark) is an amorphous Savinase e) Dissolves more quickly than (registered trademark).

Example 16 1% amount of liquid preparation Lipolase (registered trademark) 100L, Crystalline Savinase® in an amount of 0.2% and 0.6 A 25% amount of Savinase® was added to the following formulation. Added to NoVO standard liquid detergent with builder according to: Verol 160 15% Nansa 1169/P 33.3% Coconut fatty acid 9% Oleic acid 1% Triethanolamine 9% Glycerol 12% Ethanol 1.5% Trisodium citrate 2H208% CaCIz 2Hz O0,1% The table below shows the amount of lipolase dissolved in liquid detergent after 3 days at 4°C-35°C. se) (registered trademark).

Residual activity after 3 days Sample 4°C35°C Ripolase (registered trademark) + Crystal Savinase (Savin) ase) (registered trademark) 66% 23% Lipolase ( registered trademark) + liquid Savinase (registered trademark) 16% 0 ．． 9% Clearly, the stability of Lipolase® is The crystallization rate is lower than in the presence of Savinase (registered trademark). Due to the presence of Savinase (registered trademark), this example and storage stability of anhydrous Savinase (registered trademark) slurry shows.

The aqueous slurry base was 54% (NH4)2304 dissolved in deionized water. Ta.

The anhydrous slurry base contains 305g surfactant T9, 140g Na, SO4 and and 15 g of Aerosil 200, which were mixed well enough to Homogenized in a Turlux mixer.

8.7g crystalline Savinase® or 17g free Mix regular Savinase (registered trademark) with each base. Ta. The slurry was homogenized with an Ultra-Turlux mixer.

The slurry was incubated at 60°C for 5 days and then the residual activity was determined.

storage stability crystal amorphous Aqueous Anhydrous Aqueous Anhydrous KNPU/g (χ) KNPtl/g Cχ) KNPU/g (χ) KNPU/g (X) 0 days 63.0 (100) 15.8 (100) 9 ．． 18 (100) 7.63 (100) 1 day 65.6 (104) 17.5 ( 111) 7.45 (81) 7.05 (92) 5th 57.7 (92) 14 ．． 7 (93) 7.6H83) 6.48 (85) As is clear from the table above, The stability of crystalline preparations is superior to that of amorphous preparations.

Summary book The enzyme-containing preparation contains at least one enzyme, thereby providing at least one The enzyme activity of at least 50% of the enzymes is preferably It is present in the preparation as enzyme crystals, together with a stabilizing agent. Detergents contain this preparation do. Both the preparation and the detergent may be granules or slurries. the key The product and the detergent exhibit good stability and no fading.

Submission of translation of written amendment (Article 184-8 of the Patent Act) 1992 month/day

Claims (17)

[Claims] 1. An enzyme-containing preparation containing at least one enzyme, the enzyme-containing preparation comprising at least one enzyme. at least 50% of the enzyme activity of the enzyme is present in the preparation as enzyme crystals. Said enzyme-containing preparation. 2. Preparation according to claim 1, wherein the preparation contains a stabilizer for enzymes. . 3. Contains protease and at least one other enzyme, substantially 100% The preparation according to claim 1 or 2, wherein the proteolytic activity is present as crystals. . 4. Contains protease and at least one protease-sensitive enzyme; Generally, 100% of protease-sensitive enzymes or multiple protease-sensitive enzymes are bound. 3. A preparation according to claim 1 or 2, which is present as a crystal. 5.90% or more of the crystals are 0.01 μm-500 μm, preferably 0.1 μm- Any one of claims 1 to 4, having a maximum crystal size of 100 μm. Preparation as described. 6. Enzymes include protease, lipase, amylase, cellulase, and hemicellulase. , pectinase, amidase or oxidase, or protein processing variants thereof A preparation according to any one of claims 1 to 5. 7. The enzyme is a protease, and the protease is a subtilin type protein. 7. Preparation according to claim 6, which is Aase. 8. The enzyme is lipase, and lipase is lipolase (registered). 6. The preparation according to claim 6, which is a registered trade mark. 9. at least 75%, preferably at least 90% of at least one enzyme The claim is that the enzyme activity is present in the preparation as enzyme crystals, preferably of all the enzymes. The preparation according to any one of Items 1 to 8. 10. The preparation according to any one of claims 1 to 9, wherein the preparation is a granule. product. 11. Claims 1 to 9, wherein the preparation is a slurry. Preparation products. 12. Claim 11, wherein the slurry is anhydrous or substantially anhydrous. preparations of. 13. 12. A preparation according to claim 11, wherein the slurry is aqueous. 14. Claims 1 to 13, wherein the preparation is used as a detergent additive. Preparation products listed in any of the above. 15. Characterized by containing the preparation according to any one of claims 1 to 14. detergent. 16. The detergent is solid and further contains 1 g of the enzyme-containing granular material described in claim 10. 0.001-10 mg enzyme protein per detergent, preferably 0.0 per gram detergent 0.05-5 mg enzyme protein, most preferably 0.01-1 mg per gram of detergent. 16. The detergent according to claim 15, containing the enzyme protein at a concentration of the enzyme protein. 17. The detergent is a liquid, and further contains 1 g of the enzyme-containing slurry described in claim 11. of enzyme protein per gram of detergent, preferably 0.101-10 mg of enzyme protein per gram of detergent. 005-5 mg of enzyme protein, most preferably 0.01-1 mg per gram of detergent 16. The detergent according to claim 15, containing an amount of enzyme protein.