DK157937B - Enzyme-containing granulate, and process for preparing it - Google Patents

Description

in

DK 157937 B

The invention relates to an enzyme-containing granule and a process for its preparation.

The granulate according to the invention and the method of preparation thereof is a further development of the granulate and process thereof, which is described in US Patent No. 4,106,991, which is carried out in a drum granulator. The term drum granulator represents a broad category of granulator apparatus, e.g. extensive bowl granulators and granulation mixers.

Although the known granule possesses many advantageous properties, the physical stability of the known granule can be improved.

According to the invention, it has surprisingly been found that a granule which is built up around a core but which is essentially built up as disclosed in U.S. Patent No. 4,106,991 exhibits improved physical stability and other improved properties, which will appear from the following.

The enzyme-containing granule of the invention is peculiar to that of the characterizing part of claim 1.

Due to the introduction of the core which can be very inexpensive, the amount of (expensive) cellulose fibers (or synthetic fibers) and binder can be reduced to below the level disclosed in U.S. Patent 4,106,991. Thus, the total cost of the granulate can be reduced to a certain extent compared to the total cost of the known granule from US Patent No. 4,106,991. It has also been found that the physical stability of the granulate is improved over the prior art from U.S. Patent No. 4,106,991, due to the network structure of the oriented fibers. Probably because of the interaction between the core and the fibers filtered around the core, it has also been found that it is possible to prepare a granulate having a higher enzyme activity compared to the prior art. As will be explained later in more detail, it has further

2 DK 157937 B

It has been found that it is possible in a simple way to obtain the granulate in a very narrow particle size distribution which can be tailored to any need.

The core must have an average particle size of between 200 and 700 μιη, and it can be made of any coherent, non-crumbly material which will not cause any damage during the final use of the enzyme granulate. Thus, if the enzyme granule is to be used as a detergent additive, the core could be inorganic or organic salts which are readily soluble or heavily soluble in water, e.g. sodium chloride, sodium sulfate, sodium tripolyphosphate or sodium citrate. In this case, the nucleus may also be a particle of an already produced enzyme granule. In this way, granules with various enzymes can be prepared in the core and in the coating.

For example, if the enzyme granulate. to be used as a food additive, the core can be starch, sugar or protein.

Thus, the granulate according to the invention can be constructed in the following three ways:

I I

enzym_ | X_ | _X_

I I

no enzyme 1 X_j_ 1 2 3 4 5 6

The fibrous cellulose may be sawdust, pure fiber 2 cellulose, cotton or other forms of pure or impure fiber 3 cellulose.

4

There are several types of cellulose in fiber 5 form on the market, e.g. "CEPO" and "ARBOCEL". In a publication 6 from Svenska Tråmjolsfabrikerna AB, "Cepo Cellulose Powder" states that the approximate maximum fiber length for Cepo S / 20 cellulose is 500 μιη, that the approximate average fiber length is 160 μπι, that the approximate maximum 3

DK 157937 B

fiber width is 50 μπι and that the approximate average fiber width is 30 μπι. It is also stated that Cepo SS / 200 cellulose has an approximate maximum fiber length of 150 μπι, an approximate average fiber length of 50 μιη, an approximate maximum fiber width of 45 μπι, and an approximate average fiber width of 25 μπι. Cellulose fibers of these dimensions are particularly suitable for use in the enzyme-containing granules of the invention.

Typical synthetic fibers are made of polyethylene, polypropylene, polyesters, especially nylon, polyvinyl formal and poly (meth) acrylic compounds.

The binders used in the process of the invention are those binders conventionally used in the granulation field which have a high melting point 15 or no melting point at all, and which are of a non-waxy nature, e.g. polyvinylpyrrolidone, dextrins, polyvinyl alcohol, and cellulose derivatives, including e.g. hydroxypropyl cellulose, methyl cellulose or CMC. It is not possible to form a granule based on cellulose, enzyme, filler and a binder, as defined above, without the use of a granulation aid as defined below.

All enzymes can be granulated by the method of the invention. Preferably, proteinases, amylases, lipases and cellulases according to the invention are granulated.

Specific examples are ALCALASE® (a Bacillus licheniformis proteinase), ESPERASE® and SAVINASE® (microbial alkaline proteinases produced according to English Patent No. 1,243,784), CELLUZYME® (a Humicola insolens cellulase according to US Patent No. 4,435,307 ) and TERMAMYL® (a Bacillus licheniformis amylase). The enzyme may be introduced into the granulator as a pre-dried ground powder or as a solution, e.g. a concentrated enzyme solution prepared by ultrafiltration, reverse osmosis or evaporation.

The filler is used only to set the desired enzyme activity in the finished granules. Since the enzyme introduced into the granulator already contains diluent impurities which must be considered as fillers, further

DK 157937 B

4 fillers are not always necessary to standardize the enzymatic activity of the granules. If a filler is used, it is usually organic or inorganic salts which may be soluble or insoluble in water, e.g.

Na2 SO4, NaCl, CaCO3, or minerals or silicates, e.g. kaolin or bentonite, but other inert fillers which do not adversely interfere with the subsequent use of the product may be used.

The granulation aid is water and / or a waxy material. The granulation aid is always used as a liquid phase in the granulation process; therefore, if a waxy material is present, it is either dissolved or dispersed in the water or melted. A waxy material is meant a material which exhibits all of the following properties: (1) the melting point is between 30 ° C and 100 ° C, preferably between 40 ° C and 60 ° C, (2) the material is tough and not brittle, and (3) the material exhibits a substantial degree of plasticity at room temperature.

Both water and waxy materials are granulating aids, i.e. they are both active during the formation of the granules; the waxy material remains as a component of the finished granules, whereas most of the water is removed during drying. Thus, in order to attribute all quantities to the finished dry granules, all percentages are calculated on the basis of the total dry solids, with the exception of the core, which means that water, which is one of the granulating aids, is not added to the other ingredients when Calculate the percentage of water, whereas the waxy material, the second granulating aid, must be added to the other dry ingredients when calculating the percentage of waxy material. Examples of waxy materials are polyglycols, fatty alcohols, ethoxylated fatty alcohols, higher fatty acids, mono-, di- and triglycerol esters of higher fatty acids, e.g. glycerol monostearate, alkylarylethoxylates and coconut monoethanolamide.

If a large amount of waxy material is used, relatively little water should be added, and vice versa. Thus, the granulating aid may be either water alone, 5

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waxy material alone or a mixture of water and waxy material. In cases where a mixture of water and waxy material is used, the water and waxy material may be added in any order, e.g. first the water and then the waxy material, or first the waxy material and then the water, or a solution or suspension of the waxy material in the water. In the case of using a mixture of water and waxy material, the waxy material may be soluble or insoluble (but dispersible) in water.

If no water is used in the granulating aid, drying is usually unnecessary. In this case, the granulating aid is a molten waxy material and one only needs to cool to cause the particles to solidify. In most cases, however, some drying is carried out and the drying is usually carried out as a fluid-mass drying, whereby small amounts of dust and small granular grains are blown away from the surface of the granulate. However, any type of drying can be used. In the case where water is not used as a granulating aid, a liquid conditioner or anti-caking agent may be added to the granulate either before or after the cooling step, e.g. smoke silica, e.g. the commercial products AEROSIL or CAB-0-SIL.

The granulator may belong to any of the known types of mixing granulators, drum granulators, bowl granulators or modifications thereof. If a mixer granulator is used, e.g. a mixing drum from the German company Gebr.

Lodige Maschinen G.m.b.H, 479 Paderborn, Elsenerstrasse 7-9, 30 DT, it is preferred that small rotating blades are mounted in the granulator to compact the granulate.

Optional additives such as dyes, pigments, disintegrants or enzyme stabilizers may be added, e.g. antioxidants.

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6

A preferred embodiment of the granulate according to the invention is characterized by the characterizing part of claim 2. In this embodiment, a satisfactory coating around the core can always be obtained.

A preferred embodiment of the granulate according to the invention is characterized by the characterizing part of claim 3. This provides a satisfactory mechanical strength.

A preferred embodiment of the granulate according to the invention is characterized by the characterizing part of claim 4. Under 4% by weight of fibers no satisfactory fiber effect is obtained, and with more than 20% by weight of fibers the production becomes cumbersome and the product expensive.

A preferred embodiment of the granulate according to the invention is peculiar to that of the characterizing part of claim 5. This embodiment represents an extension of the sequence processing capabilities of a wash float.

A preferred embodiment of the granulate according to the invention is characterized by the characterizing part of claim 6. The enzymes in question are the most common granular enzymes for industrial use.

A preferred embodiment of the granulate according to the invention is characterized by the characterizing part of claim 7. This results in a cheap granulate.

The invention also encompasses a process for preparing the granulate according to the invention.

The process for preparing the granulate according to the invention is characterized by the method of claim 8.

30 In order to produce a granule containing only enzyme in the nucleus, no enzyme should be added, except for the enzyme already present in the nucleus.

The introduction of a core and auxiliaries, either dissolved or suspended as extremely fine particles, into a particulate material made using a fluidized mass is known from Danish patent application no.

981/86, but the introduction of a core and cellulose fibers or

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7 artificial fibers in relation to a granule made by drum granulation is new. It is believed that the new combination of the core and the cellulose fibers or synthetic fibers, which can wrap themselves around the core as a coherent mesh structure, is the reason for the extraordinarily high physical strength of the granulate according to the invention.

The process according to the invention can be carried out both discontinuously and continuously.

The invention will be illustrated by the following 10 examples.

The activity units used in the examples are defined as follows: I Activity-I Definition | enzyme_j_unit_1 specified in |

I II

proteolytic | KNPU_ | AF 220/1-GB |

I I I

amylolytic | KNU_ | AF 215/1 GB |

I I I

20 Lipolytic | LU_ | AF 95/4-GB | on request, these AF publications can be obtained from NOVO INDUSTRI A / S, Novo Allé, 2880 Bagswaard, Denmark.

In the examples, the core material exhibited a cubic shape in the case of the core being NaCl, and a rounded, irregular shape in the case of the core being Na 2 SO 2.

EXAMPLE 1 9.0 kg of NaCl core material having a particle size between 250 and 300 μπι is introduced into a fuzzy mixer FM 130 D / lMZ and mixed with

DK 157937 B

8 5.2 kg SAVINASE® concentrate (34 KNPO / g) 3.0 kg fiber cellulose, Arbocel BC 200 1.2 kg TiC> 2 1.5 kg adhesive carbohydrate 5 10.1 kg finely ground Na2 SO4

The total portion comprising 30 kg of dry matter is sprayed with 4.0 kg of water, as described in Example 1 of U.S. Patent No. 4,106,991, and a post-granulation is performed for 5 minutes with the rapidly rotating knife set 10 (see FIG. 3 of Danish Patent No. 146857, corresponding to U.S. Patent No. 4,106,991), whereby the powder components are evenly and compactly distributed around the core surfaces. The moist granules are dried in a fluidized mass to give a product having the following properties.

15 Core: 30%, shell: 70%

Enzyme activity: 5.3 KNPU / g

Particle size distribution: 3.5%> 1000 µm 5.0%> 850 -6.8%> 710-20 11.0%> 600 - 17.0%> 500 -42.0%> 420 -65.0% ) 355 - 77.0%> 300 - 90.0.0> 250 - 3.5% <210 - 1.9% <180 - 0.1% <150 -

Average diameter: 390 μιη 30 The amount of dust and the physical strength are measured according to two different methods: A. The elutration dust method, as described in NOVO publication AF 129/3-GB, which can be obtained from NOVO INDUSTRI A / S.

35 B. The Novo wear dust method, as described in NOVO publication AF 225/1-GB, which can be obtained from NOVO INDUSTRI A / S.

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DK 157937B

It is apparent from the following table that the values of dust and physical strength of the granules of this example are superior to the corresponding values of the prior art.

5 | Invention, | Prior art

Method In this example_ | (US 4,106,991) _ I I active, µg | | active, μg _I total, mg I (4 KNPU / g) | total, mg | (4 KNPU / g 10 A 1 15.4 I 8800_1 10-30 I 10,000-20,000

II II

B 1 11.9 I 4100_1 10 - 20 1 10,000-20,000 EXAMPLE 2 7.5 kg of core material having a particle size between 300 and 500 µπι is introduced into a fuzzy mixer FM 130 D / lMZ and mixed with 9.0 kg SAVINASE ® concentrate (28 KNPU / g) 3.38 kg fiber cellulose, Arbocel BC 200 0.9 kg TiC> 2 20 7.5 kg finely ground Na2 SO4

The total portion is sprayed with 6.4 kg of binder solution (a 27% aqueous solution of adhesive carbohydrates). The granulate is further processed and dried as described in Example 1 to give a product having the following properties:

DK 157937 B

10

Core: 25%, must: 75%

Enzyme activity: 8.0 KNPU / g

Particle size distribution: 6.7%> 1000 µπι 7.5%> 850 - 5 11.0%> 710 - 16.0%> 600 - 34.0%> 500 - 62.0%> 425 - 78.0%> 355 - 10 90.0%> 300 - 4.0% <250 - 1.9% <210 - 0.9% <180 -

Average diameter: 450 μπι 15 The amount of dust and the physical strength are shown in the following table.

Method in "'I M

Total, mg I (4 KNPU / g)

I I

20 A 1 3.8 I 1390_

I I

BI 9.4 In EXAMPLE 3 6.0 kg of sodium citrate ^ 21 ^ 0 (i.e., sodium citrate with 25 molecules of crystal water) core material with rounded, irregular shape particles and a particle size distribution as set forth below is introduced into a fuzzy mixer FM 50 and mixed with 2.2 kg SAVINASE® concentrate (38 KNPU / g) 30 0.6 kg T1O2 0.7 kg adhesive carbohydrate 1.5 kg fiber cellulose, Arbocel BC 200 5.0 kg finely ground Na2SO ^ 11

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The total portion is sprayed with 2.0 kg of water and the further treatment and drying is carried out as in Example 1 to give a product having the following properties: 5 Particle size distribution: Sodium citrate, Product core 15%> 1000 μια 19%> 850 - 26% > 707 - 10 1.2 42%> 600 - 20 64%> 500 - 50 83%> 420 - 70 92% p 755 - 20 1.7% <300 - 15 10 0.5% <250 -

Average diameter: 565 μπι

The amount of dust and physical strength is shown in the following table.

Method I I * 20 total, mg I (4 KNPU / g)

I I

EXAMPLE 4 In this example, the shell is applied to the core in two steps, as shown below.

Step 1 7.5 kg of sodium sulfate core material with particle sizes between 300 and 500 μπι is introduced into a fuzzy mixer FM 50 and mixed with

DK 157937 B

12 4.5 kg SAVINASE® concentrate (28 KNPU / g) 1.7 kg fiber cellulose, Arbocel BC 200 0.45 kg TiC> 2 3.75 kg finely ground Na2 SO4 5 The mixed dry components are sprayed with 3.0 kg of a binder solution (a 27% aqueous solution of adhesive carbohydrates) and the granulate is otherwise treated as in Example 1, but without the drying step.

Step 2 10 Without removing the moist granulate from Step 1 from the mixer, mix it with 4.5 kg of SAVINASE® concentrate (28 KNPU / g) 1.7 kg fiber cellulose, Arbocel BC 200 0.45 kg TiC> 2 15 3.75 kg finely ground 3.0 kg of the same binder solution as that used in step 1 is sprayed onto the blender contents.

The granulate is further processed and dried as in Example 1 to give a product having the following properties: 1 2 3 4 5 6 7 8 9 10 11

Core: 25%, shell: 75% 2

Enzyme activity: 8.7 KNPU / g 3

Particle size distribution: 4.8%> 1000 μπι 4 6.3%> 850 - 5 9.5%> 707 - 6 20.0%> 600 - 7 47.0%> 500 - 8 71.0%> 425 - 9 82.0%> 355 - 89.0%> 300 - 11 5.5%> 250 - 3.0% <210 -1.4% <180 -0.6% <150 -

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13

Average diameter: 490 μπι The amount of dust and physical strength is shown in the following table.

Method 1 1 M9 5 _I total, mg 1 (4 KNPU / g)

I I

A I 2.0 1 1300

I I

BI 8.4 In 7100 EXAMPLE 5 15 kg of a protease core (prepared according to US Patent No. 4106991, Example 1, except that Na2SO4 was used instead of NaCl and that SAVINASE® was used as the proteolytic enzyme 15 instead of ALCALASE®) with a particle core of 300-900 μπι and of almost spherical shape was introduced into a Lodige mixer of type FM50. At this stage, the proteolytic core is provided with a coating containing an amylolytic enzyme (BAN) prepared by B. amyloliquefaciens by mixing the core 20 with a powder.

The composition of the powder is: 0.90 kg BAN concentrate (925 KNU / g) 0.50 kg fibrous cellulose, DIACEL 200 0.25 kg TiO2 2.90 kg Na2SC> 4

The mixture consisting of grains and powder is mixed and 2.05 kg of a 27.3% aqueous solution of adhesive carbohydrate is then sprayed.

The granulate is treated and dried as in Example 1, 30 to give a granulate having the following properties: 14

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Enzyme activity: 4.7 KNUP / g (proteolytic) 36.0 KNU / g (amylolytic)

Particle size distribution: 0.8%> 1000 μιη 13.5%> 850 - 5 41.1%> 707 - 66.4%> 600 -86.7%> 500 -95.7%> 425 -98.7 %> 322 - 10 0.06% <300 -

Average diameter: 600 -

Dust content: {in 300 - 900 μιη fraction)

Mstode I Granules according to example | _cores_

I I

A: I 13.0 mg 1320 µg 4.0 Button / g | 25.1 mg 8040 µg 4.0 KNUP / g _1 13.5 - 452 - 240 KNU / g | _

I I

B: I 1.6 mg 361 - 4.0 KNUP / g | 14.0 mg 5500 pg 4.0 KNUP / g _ 1.7 - 327 - 240 KNU / g | _ 1 2 3 4 5 6 EXAMPLE 6 2 10 kg SAVINASE® cores of the same kind as the 3 SAVINASE® cores, As described in Example 5, 4 is coated with a powder containing an amylolytic enzyme, whereby the powder forms coatings around the cores. The composition of the 6 powder is as follows:

DK 157937 B

1.2 kg BAN (925 KNU / g) 0.5 kg fibrous cellulose, DIACEL 200 0.2 kg titanium dioxide 2.3 kg Na 1.2 kg of PEG (PEG = polyethylene glycol) in 0.6 kg of water. The granulate is treated and dried as described in Example 1.

After drying, the granulate is cooled to room temperature, whereby the wax solidifies. This results in a granulate having the following properties:

Activity: 5.4 KNUP / g 72.0 KNU / g

Particle size distribution: 3.3%> 1000 µπι 15 17.3%> 850 - 40.1%> 707 -58.9%> 600 -78.2%> 500 -91.7%> 425 - 20 97.7% > 355 - 0.9% <300 -

Average diameter: 600 μπι

Dust content: (in 300 - 900η μπι fraction)

DK 157937B

ie

Method I Granules according to Example [_cores_

I I

A: | 24.8 mg 217 μπι 4.0 BUT / g | 21.3 mg 10800 μη 4.0 KNUP / g _ 1.1 - 4600 - 240 KNU / g)

5 I I

B: I 29.5 mg 1160 μη 4.0 KNU / g 1618.0 - 770000 - 4.0 KNU / g _ 30-30 - 12800 - 240 KNU / g | EXAMPLE 7 10 kg of a NajSO particle size 300-10 500 µπι is introduced into a Lodige mixer, type FM 50, wherein the core is provided with a coating containing an amylolytic enzyme, using a three-step process, as follows:

Initially, 10 kg of grains are mixed with a powder consisting of: 15 0.6 kg of BAN (750 KNU / g) 0.3 kg of fibrous cellulose, DIACEL 200 0.2 kg of titanium dioxide 1.3 kg of Na2 SO4

For the sake of brevity, this powder is hereinafter referred to as 2.4 kg of powder P 2.

The mixture of grains and powder is heated to 65 ° C and this temperature is maintained throughout the process.

Then 0.7 kg of pure molten PEG 4000 (i.e., PEG of molecular weight 4000) is sprayed at a temperature of 70 ° C on the heated mixture of grains and powder. A granulation treatment is performed, as indicated in Example 1, but only for 1 minute.

Now, an additional 2.4 kg of the powder P 2 is introduced into the mixer, followed by 0.5 kg of PEG 4000, and a granulation treatment extending over 1 minute, as previously indicated.

DK 157937 B

17

Then an additional 2.4 kg of the powder is introduced into the mixer, followed by 1.2 kg of PEG 4000 and a granulation treatment extending over 1 minute as previously indicated.

Activity: 63 KNU / g 5 Particle size distribution: 0.3%> 1000 μπι 0.5%> 850 -4.3%> 707 - 24.4%> 600 -54.5%> 500 - 10 73.2%> 425 - 87.1%> 355 - 97.4% <300 - 9.0% <250 -

Average diameter: 550 µm Dust content: (in 300 - 900 µm fraction)

Method: A: 2.0 mg 327 pg of 240 KNU / g B. 4.6 - 717 - - 240 - EXAMPLE 8 20 13 kg of a lipase produced on a Na2 SO4 core according to Danish Patent Application No. 4499 / 87 with an activity of 2600 LU / g is introduced into a Lodige mixer of type 50, in which the core is provided with a coating containing SAVINASE® protease using a three-step process, as follows:

The 13 kg lipase cores are mixed with a powder consisting of: 18

DK 157937B

1.00 kg ground SAVINASE® concentrate of 39.5 KNPU / g 0.12 kg fibrous cellulose, DIACEL 200 0.09 kg titanium dioxide 0.91 kg Na2 SO4 5 For the sake of brevity, this powder is hereinafter referred to as 2.12 kg powder P2 *

The treatment temperature is 20-30 ° C.

Then, 0.9 kg of a binder solution containing a 25% aqueous solution of an adhesive carbohydrate is sprayed onto the mixture in the Lødige mixer.

Then an additional 2.12 kg of powder P2 is introduced into the mixer, followed by 0.7 kg of the above-mentioned binder solution introduced by spraying.

Then an additional 2.12 kg of powder P2 15 is introduced into the mixer, followed by 1.15 kg of binder solution introduced by spraying. Finally, granulation, compacting and drying are performed as indicated in Example 1.

A granulate having the following properties is obtained:

Core: 67% wt% Coating: 33% wt% 20 Activity: 17,900 LU / g (lipolytic) 6.0 KNUP / g (proteolytic)

Particle size distribution: 2.3% 1000 μπι 12.0% 850 - 29.1% 707 - 25 48.7% 600 - 71.5% 500 - 86.5% 425 - 95.1% 355 - 3.0% 300 - 30 Average diameter: 590 μπι

Dust content: (in 300 - 900 μπι fraction)

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19

Method | Granules by Example - | _Core_

I I

A: In 3.9 rag 3360 µg 4.0 KNPU / g | _I 6.0 - 0 µg LU / filter | 32.4 mg 200 LU / filter

5 I I

B: I 1.0 mg 1340 μς 4.0 KNUP / g | _I 1.7 -_0 µ9 LU / f ilter_ | 29.0 rag 142 LU / filter

Claims (8)

Enzyme-containing granule, characterized in that it comprises a core having an average particle size of between 200 and 700 μπι, and wherein the amount of the core is between 15 and 40% by weight of the granulate and the core is surrounded by a coating comprising cellulose fibers or synthetic fibers in an amount of from 1.5 to 40% by weight, based on the dry weight of the granulate, with the exception of the core, a binder in an amount of 0 to 15% by weight, based on the dry weight of the granulate, 10 with the exception of the core, a filler and one or more granulating aids in an amount up to approx. 70% by weight, based on the dry weight of the granulate, with the exception of the core, and that the core and / or coating contains an enzyme. Granule according to claim 1, characterized in that the core 15 has a shape corresponding to a maximum ratio between the largest and smallest dimension of approx. 3, preferably approx. 2, especially approx. 1.5. Granule according to claims 1-2, characterized in that the cellulosic fibers or synthetic fibers have an average fiber length of 50 - 1000 µm and an average fiber width of 5 - 50 µm, preferably 10 - 40 µm. Granule according to claims 1-3, characterized in that the amount of cellulose fibers or synthetic fibers is between 4 and 20% by weight, based on the dry weight of the granulate, with the exception of the core. 1 Granule according to claims 1-4, characterized in that the core and coating contain an enzyme and that the enzyme in the core is a different enzyme than the enzyme in the coating. DK 157937 B Granule according to claims 1-5, characterized in that the enzyme is a protease, an amylase, a lipase, a cellulase or an oxidase. Granule according to claims 1-6, characterized in that the filler consists of or comprises inorganic salts. Process for the preparation of an enzyme-containing granule according to claims 1-7, characterized in that a core having an average particle size of between 200 and 700 μπι and in an amount of 10 between 15 and 40 wt. % of the finished granules, 1.5 to 40% by weight cellulose fibers or synthetic fibers, from 0 to 15% by weight of a binder, as well as enzyme and filler in an amount which produces the desired enzyme activity in the finished granules, a liquid granulating aid consisting of a waxy material and / or water in an amount of from 5 to 70% by weight, whereby the maximum amount of waxy material is 70% by weight and the maximum amount of water is 70% by weight, all of which are not precise percentages refer to the total amount of dry matter, with the exception of the core, and where the order of introduction of the various materials is arbitrary, except that at least the majority of the granules The auxiliary agent is introduced after at least a substantial portion of the dry matter is introduced into the granulator, whereby the granulation is preferably carried out at a temperature between 20 and 70 ° and then dried, if necessary.