DK152057B - ENZYMOUS PARTICLES, PROCEDURES FOR THEIR PREPARATION AND THEIR USE IN DETERGENTS - Google Patents

Description

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DK 152057B

The invention relates to flexible and non-dusty enzyme-containing particles characterized by the characterizing part of claim 1. Furthermore, the invention relates to a process for the preparation of the particles and the use of the particles as a component in detergents.

In particular, the enzymes in question are those enzymes commonly used in detergents, and also enzymes used for other purposes, e.g. in pharmaceutical preparations.

Enzymes have been used in detergents for several years.

However, one of the problems with the formation of enzymatically active detergents is the fact that during the preparation of the enzymatic detergent enzyme dust is formed. This is uncomfortable for the people who work with the enzyme material, and sometimes there are skin irritations and allergic reactions.

Dust of the enzyme can be substantially avoided by bringing the enzyme into a form other than powder form, which is the form in which it is normally obtained. This is advantageously done by bringing the enzyme into a solid particle form. Danish Patent Application No. 3696/71 discloses a process for preparing an enzyme preparation consisting of spherical enzyme-containing pellets, from a mixture of 75-97% enzyme-containing powder and 25-3% water, in a spheronization process which uses of a rotational speed of up to approx. 2000 rpm in an apparatus in which centrifugal and frictional forces act on said pellets, after which the spherical solid particles thus obtained are optionally dried in a fluidization layer. It is necessary to add water to complete the extrusion process. The spherical enzyme compositions obtained can be coated, preferably with a wax type, which, however, must be water-insoluble or dispersible. Among other compounds, polyethylene glycol 1000-6000 is mentioned as an example of a suitable coating material. An organic cohesive and / or lubricant may also be added to the materials to be extruded and spheronized. Polyethylene glycols are mentioned as suitable lubricants and dextrin, polyvinylpyrrolidone and polyvinyl alcohol are mentioned as cohesive agents.

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Casein, lean milk powder and polyvinylpyrrolidone have a stabilizing effect on enzymes. According to said patent application, the enzyme preparations can also be powdered with an inorganic oxide such as titanium dioxide or an inorganic salt to prevent clumping of the granular final product. However, the low moisture content of the enzyme preparations thus produced, caused by drying or evaporation of moisture during storage, has an adverse effect on their flexibility. "The particles prove to be rather brittle in practice.

British Patent Specification No. 1,342,116 discloses a process by which a liquid mixture of the enzyme and a binder, i.e. a low-melting non-ionic emulsifier, dispersed in droplets by means of a tooth plate and guided into a cooling tower where the droplets solidify. In this way, a dust-free product is obtained which is easily formulated for detergents. Although the enzyme particles obtained according to this patent are good and can be used without the risk of dust formation, they can be improved to avoid those whose mechanical pressure is exerted on the particles, such as the pressure from the feet of a person passing over spilled particles, easily breaks down into smaller particles and powders so that enzyme powder from broken particles can be carried off by air currents.

Through the present enzyme-containing particles, flexible enzyme particles are provided which do not or substantially do not degrade to powder when mechanical pressure is exerted on them.

The present process for preparing the enzyme-containing particles of the invention is characterized by homogeneously mixing an amount (preferably up to 6% by weight, based on the total mixture of materials) of an enzyme in dry or substantially dry state to obtain the desired enzyme activity in the particles formed, ca. 2Q to approx. 6Q% by weight, based on the total mixture of materials (preferably about 30 to about 5Q%) 1 of a hydrophilic organic binder compatible with the enzyme, approx. 10 to approx. 60% by weight, based on the total material mix (preferably about 20 to about 45%). of a structural agent suitable for use in the enzyme material and, if necessary, a small amount of water sufficient to give a moisture content of the formed particles of from 5 to 15% by weight that

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3 divides the obtained mixture into particles, i.e. beads of the desired size, and coating the particles with a water repellent.

It need not be necessary to add water if the moisture content of the ingredients is sufficient to supply the required moisture content in the final product. Optionally, an amount of humidity regulator may be added which is sufficient to maintain the moisture content of the formed particles of from approx. 5 to approx. 15% by weight at ordinary temperatures and normal relative humidity values.

The percentages mentioned in this specification and claims are by weight unless otherwise indicated.

For use in detergents, the basic constituents can be selected from a large amount of raw materials as they do not need to be consumable, although they are preferably biodegradable. For use in oral pharmaceutical preparations, the ingredients should be edible and pharmaceutically acceptable.

The present enzyme-containing particles are very useful for use in detergents if the enzymes for this purpose are selected from the enzymes usually used in detergents. Examples of such enzymes are proteolytic enzymes (proteases), amylolytic enzymes (amylases). or lipolytic enzymes (lipases) and mixtures thereof. Examples of suitable proteolytic enzymes are enzymes of bacterial origin, such as proteolytic enzymes from Bacillus species, e.g. B. subtilis, B. licheniformis and B. alcalophilus. Preferably, myylolytic enzymes are also enzymes of bacterial origin, such as amylolytic enzymes produced by Bacillus species, e.g. B. subtilis. Some bacteria produce suitable proteolytic and amylolytic enzymes at the same time. Lipolytic enzymes that can be used are preferably also enzymes of microbial origin. They can be produced by Candidate species, e.g. Candida cylindraceae. Lactases are also useful. The enzymes for pharmaceutical compositions are e.g. a lactase or glucoamylase.

The hydrophilic organic binder used for the subject enzyme-containing particles can be selected from starch and cellulose derivatives, and a preferred type of starch derivative is acetylated amylopectin, called "amylopectin gum". This type of rubber

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4 is an amylopectin with an acetylation degree of approx. 5% to approx. 30%. Examples of other useful binders are gum arabic, dextrin, karaya gum, methyl cellulose, tragacanth and other types of amylopectin such as methyl amylopectin. Certain starch hydrolysates (preferably with DE (dextrose equivalent) of about 30) may also be used.

A starch hydrolyzate can be used as a binder if it has adhesive properties, i.e. if it contains amylopectin derivatives.

The structural agent used for the enzyme-containing particles is preferably a water-soluble carbohydrate, generally containing from 5 to 12 (preferably 6) carbon atoms. Suitable examples of carbohydrates with 5 carbon atoms, pentoses, are xylose, arabinose, ribose and luxose. Suitable examples of carbohydrates with 6 carbon atoms, hexoses, are glucose, mannose, galactose, fructose and sorbose. In addition, disaccharides can be used, usually with 12 carbon atoms, such as sucrose, maltose or cellobiose. The most preferred carbohydrate is glucose. Since glucose crystallizes fairly easily (and so do other carbohydrates), some or all of the glucose or other carbohydrate can be replaced by starch hydrolyzed to some degree. A starch hydrolyzate of approx. 20 DEG to 70 DEG, preferably approx. 30 to approx. 60 DE, is used advantageously. These starch hydrolysates are also called glucose syrups. Preferably, an amount of approx. 40% to approx. 70% of the total weight of the structural agent to replace glucose or other carbohydrate.

The preferred structural agents are glucose, sucrose and starch hydrolyzate.

It should be noted that starch hydrolysates with adhesive properties can exert a dual effect as adhesive and structural agent.

Lubricants can be added to the enzyme mixture to facilitate partitioning of the mixture into particles by mechanical means. Preferably, approx. 2% to approx. 7% (preferably about 3% to about 5%) of lubricant for the enzyme mixture.

Examples of lubricants which may be used are polymeric substances such as polyvinyl alcohol, paraffin oil or wax, stearic acid and polyvinylpyrrolidone. Glycerol also acts as a lubricant.

As mentioned, a humectant can be introduced into the enzyme mixture in an amount sufficient to maintain 5

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the desired moisture content. It is necessary to maintain a total moisture content of approx. 5% to approx. 15%, preferably approx. 5% to approx. 10%, to maintain the supple nature of the enzyme particles after their formation. Examples of agents useful in maintaining the moisture content are polyols having 2-6 carbon atoms and 2-4 hydroxy groups attached to various carbon atoms. Examples of this group of compounds are ethylene glycol, 1,2- and 1,3-propylene glycol, 1,2-, 1,3- and 2,2-butylene glycol, glycerol and sorbitol. Glycerol and sorbitol are preferably used. To maintain the moisture content mentioned above, approx. 0.5 to approx. 5% by weight, preferably approx. 1 to approx.

3% by weight, of the humectant, depending on the circumstances.

Further, other constituents may be added to the enzyme mixture prior to formation of particles thereof, e.g. pigments, such as titanium dioxide, or an optical lighter. The quantities normally used are approx. 1 to approx. 10% by weight, preferably approx. 3 to approx. 7% by weight of pigment, especially in the case of titanium dioxide.

In addition, fillers such as silica, penicillium mycelium, cellulosic powder or fiber, saw dust and bentonite can be added in amounts of e.g. 3-10%. The fillers can be added for structural stability of the particles, especially when the material is to be treated in large quantities.

The ingredients can be mixed together in any order at room temperature and even at elevated temperatures, the maximum temperature being dependent on the nature of the enzyme.

The mixture is a powder at ordinary temperatures but becomes plastic at elevated temperatures and by application of pressure. The lowest usable temperature may be that at which the mixture just becomes plastic and the highest temperature depends on the nature of the enzyme. Temperatures of approx. 4Q ° to approx. 70 ° C is usually suitable, but in special cases other temperatures may or may not be used. The softening of the mixture can be carried out by means of a kneader mixer and, in principle, any mixer in which the mixture is softened under mild conditions (at low shear) and from which the softened mixture can be extracted portionwise or continuously.

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Just after softening, the still plastic mixture is pressed through a pump and a string forming apparatus, e.g. a gear pump and an extruder. The strand forming apparatus may comprise a mold plate having one or more holes through which strands of the desired cross-section may be formed, e.g. cross section of approx. 0.5 to approx. 3 µm, preferably 0.7 to 1.5 µm.

The desired particles can be obtained in granulated form by cutting off the strands formed. Granulating equipment for this purpose can be placed at some distance from the plate. The granulation can also be carried out by cutting equipment, provided with one or more moving edges which cut off the extruded product on the mold plate. The cutting equipment preferably consists of a plurality of rotating blades in such a way that, depending on the location of the rotational axis relative to the mold plate, the blades move either continuously or once per second. rotation across the filler plate.

It is also possible to combine softening, pumping and granulation in a single apparatus, e.g. a screw extruder. The hopper in the extruder is filled with a powdery mixture which, when applied to the apparatus, is plasticized by heat and pressure generated by the rotary screw. The last part of the screw action is a mixture and pressure generation sufficient for extrusion through a multi-hole font plate.

The constituents of the mixture can also be fed separately to the appropriate apparatus in a desired ratio, combining mixing, softening, pumping and extrusion through a font plate. An example of such equipment is a double screw extruder fitted with mixing equipment.

Depending on the desired size of the enzyme particles, a plate down apertures of approx. 0.5 to about 3 nm, preferably 0.7 to 1.5 µm, but larger or smaller apertures may also be used in particular cases. Also, the size and shape of the enzyme particles also depend on the speed of the cutting blades, their number and the composition of the mixture.

To avoid loss of moisture, the particles formed are preferably coated with about, Q, 5 to approx. 5% by weight (depending on the nature of coating agent 1 of a water repellent, such as paraffin oil or flaxseed oil, several types of wax, e.g., ground wax, cocoa fat, candelilla wax, camauba wax, ceresin wax, lanolin, paraffin wax, beeswax and mixtures thereof. which may occur when placed in sacks for transport may be avoided by coating the particles already coated as described above with an anticliner such as corn starch or other starches, absorbent silica such as "AerosiT®, or talcum powder.

The present enzyme-containing particles do not or substantially do not give rise to enzyme dust formation. The formation of 7

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enzyme dust can be measured by a standard test method, e.g. elutriationstesten. This test is described in Belgian Patent No. 838125 and is carried out with a test of 60 grams. The activity of the dust is measured for protease in DU (Delft units, the procedure is described in British Patent Specification No. 1353317, page 4, line 114 et seq.).

The dust formation measured by the elutriation test for the subject enzyme-containing particles is below ca. 100 DU, preferably below approx. 50 DU.

Depending on the conditions under which the subject enzyme-containing particles are prepared, for use in detergents, they may have a particle size of approx. 0.2 to approx. 3 mm, preferably approx. 0.5 to approx. 1.5 mm, in cross section. For other purposes, e.g. When used in oral pharmaceutical formulations, the particle size will, as in normal practice, usually be larger. The particles are of a smooth nature and can be deformed under pressure without degrading to powder, thus causing dust formation. However, as it appears in bags packed with particles, pressure should not deform the particles too much. The agility of the particles can be adapted to different sack sizes. In small bags, the pressure on the particles in the bottom of the bags is less than in large bags, and for small bags the requirements for resistance to deformation are less stringent than for large bags.

The detergents in which the subject enzyme-containing particles can be used as a constituent may contain one or more detergents, usually used in enzymatic detergents such as nonionic and anionic detergents, e.g. sodium benzenesulphonate. The detergents usually contain ingredients that has a softening effect on the wash water, such as complex phosphates, e.g. sodium tripolyphosphate, sodium pyrophosphate, or phosphate-free water softeners, e.g. nitrilotriacetic acid or its salts or sodium citrate. Other ingredients may be added, e.g. anhydrous sodium silicate, weak alkaline components such as sodium carbonate, oxidizing agents such as sodium perborate filler such as sodium sulfate, and other ingredients such as carboxymethyl cellulose, perfumes, optical lighters and pigments such as titanium dioxide.

Usually, an amount of enzyme particles produced by the treatment, in the process of the invention, of a proteolytic

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8 enzyme to obtain a finished detergent having a proteolytic activity of approx. 1000 to approx. 3000, preferably, approx. 1500 to approx. 2500 DU / g. The amount of detergent used in detergents is usually from ca. 4% to approx. 20%, preferably approx. 6% to approx. 12%. The amount of water softener is usually approx. 35% to approx. 55%, preferably approx. 40% to approx. 50%. The amount of residual constituents is usually approx. 1% to approx. 20%, with the filler yielding 100%. The detergent is prepared in the usual manner. All of the ingredients can simply be mixed together or first a mixture is prepared containing some of the ingredients to be added in low volume.

The invention is further described by the following examples.

Example 1 (A) Preparation of particles containing "Maxatase".

The following ingredients were mixed together under heating until all ingredients were dissolved: 1 part by weight glycerol, 2 parts by weight polyvinylpyrrolidone, 2 parts by weight "Berol" ® 80 (C ^ gt fatty alcohol polyethylene oxide, etc., 80 ethylene oxide units).

This mixture was added to 26 parts by weight of "Maxatase "® concentrate with about 1.7 MDU / g and then added; 5 parts by weight of titanium dioxide, 15 parts by weight glucose syrup (starch hydrolyzate with about 43 DE) 15 parts by weight glucose, 33 parts by weight Amylogum CLS-0473 (trade name, acylated amylopectin from Avebe, The Netherlands), and about 1 part by weight of water.

The total moisture content of the resulting mixture was approx. 7%.

The whole was mixed to a homogeneous paste at a temperature of approx. 65 ° C and supplied with an extruder fitted with a perforated plate with openings of 1 mm. The extruder was further provided with 2 rotating cutting blades just behind the perforated plate and with a sheath with cooling or heating water as desired. The paste was extruded at a temperature of approx. 65 ° C and the extruded strands became 9

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immediately cut into small particles using the cutting blades. The particles were cooled on a tray.

The particles thus obtained having a cross section of approx. 2 mm and with a (calculated) proteolytic activity of 0.43 MDU / g was coated with 1 wt% paraffin oil, followed by 3% corn starch. coated with 1 wt.% paraffin oil, followed by 3% corn starch. The enzyme-containing particles thus obtained could be deformed under mechanical pressure without breaking, but under the pressure normally found in the lower portions of commonly used bags, the particles were hardly deformed more than some. few percent.The Elutration test showed a value of 18 DU. .

(B) Generating a detergent.

The particles thus obtained were used in a detergent. The following ingredients were mixed together: 54 parts by weight sodium sulfate, 24 parts by weight sodium tripolyphosphate, 6 parts by weight sodium pyrophosphate, 10 parts by weight sodium biorbonate, 2 parts by weight sodium carboxymethylcellulose and 4 parts by weight dialkylphenoxypoly (ethylene oxyethanol).

After thorough mixing of the detergent ingredients, 0.5 parts by weight of enzyme-containing particles (prepared as indicated in (A)) was added and thoroughly mixed with the detergent. The detergent thus obtained had the same detergent activity as similar detergents in which the enzyme-containing particles were replaced by an amount of enzyme particles obtained according to the process disclosed in British Patent No. 1324116 and with the same enzyme activity in the final detergent (about 2000 DU / g).

Example 2

Preparation of enzyme-containing particles with varying contents of filler and different coatings.

Starting from the recipe set forth in Example 1 (A) for the preparation of enzyme-containing particles, the following fillers and coatings were used in the amounts indicated:

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Filler :: Coating 1 Coating 2 Elutriation Test (DU) 5% C 0.5% E 3% G 45 2% A 2.5% E + 2.5% F 2% A 32 2% A 2.5% Ξ + 2.5% F 3% G 18 2% A 0.5% E + 0.5% F 1% A 10 1% A - 1% A 80/6 \ -A - "Aero s il" '972 (et "Hydropyl silica adsorbent C = Arbocel C250 (trade name, fine saw dust D = bentonite E = paraffin oil F = glycerol monostearate G = corn starch o

The table shows that all produced enzyme-containing particles have fairly low elutriation values, the best being the 4th sample. The enzyme particles were used in detergents in the manner set forth in Example 1 (B). The detergents showed the same detergent activity as a similar detergent containing enzyme particles according to British Patent Specification No. 1324116.

The elutriation test mentioned above is performed as follows:

A bed of enzyme particles is subjected to an air flow in such a way that the particles having a predetermined final velocity or less are fed with the air flow. This method is a modification of the standard elutriation fester described in BS 3406, Volume 3, 1963, and carried out in a vertically disposed elutriation tube containing a dust filter. The entrained particles are collected on the filter and weighed and their enzymatic action determined (expressed in system units or Delft units). The velocity of the main air flow is 0.8 m / sec.

Example 3

Preparation of enzyme-containing particles with varying amounts of other fillers.

Based on the recipe set forth in Example 1 (A) for preparing enzyme-containing particles, the following fillers were used: 2% Aerosir® 972, 5% and 10% bentonite, 5% penicillin mycelium (obtained from the penicillin fermentation liquid (G fermentation) The particles were coated with 1% paraffin oil, followed by 1% Aerosil (S) 972.

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All of the fillers listed proved to be useful, but the particles containing 10% bentonite tended to be slightly brittle.

The enzyme particles were used in detergents in the manner described in Example 1 (B). The detergents had the same detergent activity seen as detergent containing enzyme particles according to British Patent Specification No. 1324116.

Example 4

Variation in Example 1's recipe for the preparation of enzyme-containing particles.

Preparation of particles of Example 1 (A) was repeated with the difference that Amylogum CLS-0473 was replaced by a similar amount of Paselli MD-30 (trade name, a starch hydrolyzate with a DS of about 30 from Avebe, The Netherlands). The particles were coated with 1% paraffin; n-oil followed by 1% nAerosil1 ^ 972.

According to another experiment, the preparation of the particles was repeated according to Example 1 (A), with the exception that "BerpI" £ poly polyvinylpyrrolidone and glucose were not used and present! 10 parts by weight of bentonite was used. All of the components were blended together to a temperature of ca. 65 ° C and the resulting paste was extruded and cut into particles. The particles were coated in the same way as for particles containing Paselli MB-3G

Both types of particles prepared according to this example prove to be very useful, and detergents prepared in the same manner as described in Example 1 (B) showed essentially the same washing - = activity as similar detergents containing enzyme particles tf; · British Patent Specification No. 1324116,

Example 5

Preparation of enzyme-containing particles for pharmaceutical use.

The following specification was used to prepare a granulate according to the invention.

25% glucoamylase (about 25,000 U / g), 6.25% invertase (about 325,000 SU / g), 45% Amylogum CLS-0473, 20% glucose syrup (starch whey polysate with about 43 DE), 3.75%, glycerol.

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The powder was directly extruded through openings 1 mm in diameter and the extrudate was converted into granules. The grains were coated as described in Example 3. This type of preparation is useful for oral administration to patients suffering from carbohydrate metabolism caused by a lack of invertase, glucoamylase or iso-maltase.

Example 6

Other particles containing "Haxatase".

The following specification was used for this purpose: 50% Maxatase® (2.3 million DU / g), 35% Amylogum CLS-0473, 15% glucose syrup (starch hydrolyzate, about 43 DE).

This mixture was converted to grain as set forth in Example 5. After granulation and coating as in Example 3, the particles were coated with 5% titanium dioxide.

Example 7

Further preparation of particles containing "Maxatase®.

The following specification was used for this: 45% methylcellulose, 20% "Maxatase "® (2.4 'million DU / g}., 10% glucose syrup (starch hydrolyzate, about 43 DE)), 4% paraffin wax, 5% titanium dioxide, 2% glycerol, 14% glucose.

A granulate was prepared by the procedure described in Example 5 and found to have similar properties. (Coating of the granulate was performed as described in Example 3).

Example 8 (£)

Further preparation of particles containing:, I /; axatase, Ke> 'The following specification was used for this purpose.

in 13 DK 152057 B | in 45% rubber arabic, 20% Maxatase® (2.4 million. DU / gJ., 10% glucose syrup (starch hydrolyzate, about 43 DE)), 4% paraffin wax, 5% titanium dioxide, 2% glycerol, 14% glucose.

A granulate was prepared by the procedure described in Example 5 and found to have similar properties. (Coating of the granulate was performed as described in Example 3).

Example 9

Preparation containing amylase.

The following regulation was used for this? 25% amylase (16,400 BAU / g), 37% Amylogum CLS-0473, 16% glucose syrup (starch hydrolyzate, ca. 43 DS), 16% glucose, 5% titanium dioxide, 1% glycerol.

In addition, this regulation uses 50% amylase (16,000 BAU / g), 35% Amylogum CLS-0473, 15% glucose syrup (starch hydrolyzate, about 43 DE).

A granulate was prepared according to these instructions according to the procedure described in Example 5, and both preparations were found to have similar properties (Coating of the granules was performed as described in Example 3).

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Example 10

Several preparations containing "llaxatase®.

Sample # 1 2 3 4 5 6 7

Amylogum CLS-0473 (%) 40 40 40 40 40 40 40 "Maxatase1® (% J (11 20 20 20 20 20 20 20 sorbitol (%) -2 ----- glycerol (%) 2-22222 paraffin wax (% ) -'- 4-244 HAerosil® 972 (% I --- 21-- "Berol®80 (% I 1 1 1 1 1 - - titanium dioxide (%) 5555555 glucose (ft) 22 22 18 20 19 19 14 glucose syrup (%) (2) 10 10 10 10 10 10 10

Elutriation Test (3) 29 20 14 10 20 32 11 (1) 2.18 million DU / g

(2) starch hydrolyzate, ca. 43 DE

(3) per 60 grams of sample.

Coating of the particles was performed as described in Example 3.

Example 11

Composition containing alkaline protease.

The following specification was used for this: 34% Amylogum CLS-0473, 17% glucose, 17% glucose syrup (starch hydrolyzate, approximately 43 DE1, 7% stearic acid, 20% PB 92 (1.7 million ADU / g) (1), 5 % titanium dioxide.

(1) PB 92 is an alkaline proteolytic enzyme disclosed in U.S. Patent No. 4,002,572.

A granulate was prepared according to the procedure described in Example 5 and the granulate was found to have similar properties. Among other things. showed elutriation tests applied to a sample of 60 g, a value of 95 ADU / g. (Coating of the granulate was performed as described in Example 3).

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Example 12

Storage stability of a granule according to the invention containing "iiaxatas'e".

A commercially available washing powder (400 g) containing sodium perborate was used. An amount of enzyme granulate of Example 10 (Sample 5), previously coated with 1% of a 1: 1 mixture of glycerol monostearate and paraffin oil, to give an active; - 6000 DU / g, was added and the material was thoroughly mixed.

Weighed samples of 20 g were taken from the material immediately after mixing for use in a storage stability test "C, ·ί · was made after 0.5, 1, 2 and 3 months of storage at 37 ° C. The samples were tested after dissolution in synthetic tap water (containing 111 mg / l CaO, 27.5 mg / l MgO and 210 mg / l NaHCOg, German hardness 15%) containing sufficient sodium dithionite to neutralize the effect of the perborate, and dilution with synthetic conductinase water to a concentration suitable for testing the activity in Delphi units (cf. British Patent Specification No. 1,353,317) (series A of the following table).

A similar test was performed with a commercially available granule of the same enzyme ("Maxatase "®, from Gist-Brocades, The Netherlands, prepared according to the method described in British Patent Specification No. 1,324,116 (Series B]). achieved:

Shelf life (months) 0.5 1 2 3

Series A 100 99 89 91

Series B 94 92 82 75

The table shows that the storage stability of series A, according to the invention, is good and, in addition, better than the comparison series B, which also has a fairly good stability.

Example 13

Composition containing lactase.

The following specification was used for this purpose: 45% Amylogum CLS-0473, 30% lactase (precipitated), 25% glucose syrup (starch hydrolyzate, about 43 DE).

A granulate was prepared by the procedure described in Example 5 and coated as described in Example 3. When the temperature was maintained at or below 50 ° C during the preparation of the granulate, the activity of the granulate was 95% of the starting activity, while ir

Claims (18)

1. Flexible and non-dusty enzyme-containing particles, characterized in that they contain, in addition to an enzyme in an amount which gives the desired enzyme activity. 20 to about 60% by weight, based on the total mixture of materials, of a hydrophilic organic binder compatible with the enzyme, and about 10 to approx. 60% by weight, based on the total material mixture, of a structural agent suitable for use in enzyme preparations and having a moisture content of from 5 to 15% by weight, the particles being coated with a water repellent. Process for the preparation of enzyme-containing particles according to claim 1, characterized in that an amount of an enzyme in a dry or substantially dry state is homogeneously mixed to obtain the desired enzyme activity in the particles formed, approx. 2Q to approx. 60% by weight. Based on the total material mix, of a hydrophilic organic binder compatible with the enzyme, approx. 10 to approx. 60% by weight, based on the total material mix, of a structural agent suitable for use in the enzyme material and, if necessary, a small amount of water sufficient to give a moisture content of the formed particles of 5 to 15% by weight, mechanically dividing the obtained base into particles of the desired size and coating the particles with a water repellent. Process according to claim 2, characterized in that a humidity control agent is further admixed. Process according to claim 2 or 3, characterized in that the hydrophilic binder is selected from starch and cellulose derivatives. Process according to any one of claims 2-4, characterized in that the hydropilic binder is acetylated amylopectin with an acetylation degree of approx. 5 to 30%. Process according to any one of claims 2-5, characterized in that the amount of hydrophilic binder used is approx. 30 to approx. 50% by weight. Process according to any of claims 2-6, characterized in that the structural agent is selected from water-soluble carbohydrates containing 5-12 carbon atoms. Process according to any one of claims 2-7, characterized in that the structural agent is a mixture of glucose and 40 to 70% by weight of starch hydrolyzate with a dextrose equivalent of approx. 20 to approx. 70th Process according to claim 8, characterized in that the dextrose equivalent in the starch hydrolyzate is approx. 3Q to approx. 60th Process according to any one of claims 2-10, characterized in that the amount of structural agent used is approx. 20 to approx. 45% by weight. Process according to any of claims 3-10, characterized in that the added humidity regulator is selected from polyols having 2-6 carbon atoms and 2-4 hydroxy groups attached to different carbon atoms. Process according to claim 11, characterized in that the humectant is selected from glycerol and sorbitol. Process according to claim 11 or 12, characterized in that the amount of humidity regulating agent used is approx. 0.5 to approx. 5% by weight. / DK T52057 B Process according to claim 13, characterized in that the amount of humidity regulator is approx. 1 to approx. 3% by weight. Process according to any one of claims 2-14, characterized in that the amount of enzyme used is up to approx. 50% by weight. Process according to any one of claims 2-15, characterized in that the particles are coated with approx. 0.5 to approx. 5% by weight of the water repellent. Method according to claim 16, characterized in that the particles are additionally coated with an anti-caking agent. Use of enzyme-containing particles according to claim 1 as a component of detergents.