JPS5836955B2 - enzyme particles - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention also relates to particulate enzymes, particularly those commonly used in cleaning compositions, and for other purposes, such as in pharmaceutical compositions.

Enzymes have been used in cleaning compositions for several years.

However, one of the problems with formulating cleaning compositions with enzyme activity is that enzyme dust is produced when formulating enzyme-containing cleaning compositions.

This is unpleasant for those working with the enzyme composition and sometimes results in skin irritation or allergic reactions.

This pulverization of the enzyme can be avoided to a large extent by placing the enzyme in a form other than the powder from which it is normally obtained.

This is effectively achieved by forming the enzyme into solid granules.

Methods of granulating enzymes are known, for example British Patent No. 132.
No. 4116, in which a liquid mixture of the enzyme with a binder, i.e., a low-melting non-ionic emulsifier, is dispersed in droplets by means of a serrated disc and guided into a cooling tower where the enzyme is A method of solidifying droplets is disclosed.

A powder-free product is thus obtained, which is easily incorporated into cleaning compositions.

Although the enzyme particles obtained according to the above-mentioned patent specifications are of good quality and can be used without the risk of powdered products, if mechanical pressure is applied to the particles, e.g. the pressure of the foot of a person walking on the spilled particles. When added, they are easily crushed into small particles and powders, and the enzyme powder from the crushed particles is carried away with the air stream and becomes a scale, so improvements can be made to avoid this disadvantage.

It is an object of the present invention to provide a material that has no or substantially no flexibility (plurality) that will not crumble into powder when subjected to mechanical pressure.
iant) enzyme particles.

The present invention provides a method for producing enzyme-containing particles that undergo no or substantially no powdering when subjected to external mechanical pressure, but which imparts the desired enzyme activity to the particles when they are shaped. (preferably within about 50%)
of dry or substantially dry enzyme, from about 20 to about 60
% (preferably from about 30 to about 50%) of a hydrophilic organic adhesive having an affinity for the enzyme, from about 10 to about 60% (preferably from about 20 to about 45%) for the enzyme composition. Appropriate shaping agent,
and optionally 5 to 5 to the particles when they are formed.
A small amount of water sufficient to give a moisture content of 15% is mixed homogeneously, the resulting mixture is mechanically divided into particles of the desired size, e.g. pellets, and the particles are coated to prevent water loss. It consists of things.

It may not be necessary to add water if the moisture in the blend is sufficient to provide the required moisture in the final product.

A moisture control agent may optionally be added in an amount to maintain the moisture content of the particles (after formation) from about 5 to about 15% at ambient and normal relative temperatures.

The percentages given in this specification and claims are by weight unless otherwise specified.

For cleaning compositions it is preferred that the base formulation be biodegradable, but not necessarily consumable, so that the base formulation can be selected from a wide range of raw materials.

Each component of a pharmaceutical composition intended to be taken orally must be edible and pharmaceutically acceptable.

The enzyme-containing particles obtained according to the invention are extremely useful in cleaning compositions if the enzyme is selected for that purpose from those conventionally used in cleaning compositions.

Examples of such enzymes are proteolytic enzymes (proteases), amylolytic enzymes (amylases) or lipolytic enzymes (lipases) and mixtures thereof.

Examples of suitable proteolytic enzymes include proteolytic enzymes from Bacillus species such as B. subt.
llis), Bacillus licheniformis (S, 1ich)
Enzymes derived from bacteria such as B. eniformis and B. alcalophilus.

The amylolytic enzyme is also preferably an enzyme of bacterial origin, for example an amylolytic enzyme produced by a Bacillus species such as Bacillus subtilis.

Some bacteria simultaneously produce the appropriate proteolytic and amylolytic enzymes.

The lipolytic enzymes that can be used are also preferably enzymes derived from microorganisms.

They are Candeida species such as Candeida cylindra +
(Candida cylindraceae).

Lactase is also useful.

Enzymes useful in pharmaceutical compositions include, for example, invertase, glucoamylase, and the like.

The hydrophilic organic adhesive used to form the enzyme mixture may be selected from starch and cellulose derivatives, but a preferred type of starch derivative is acetylated amylopectin, referred to as "amylopectin gum".

This other gum is amylopectin with a degree of acetylation of about 5 to about 30%.

Examples of other useful adhesives are gum arabic, dextrin,
Karaya gum, methylcellulose, tragacanth and other types of amylopectin, such as methylamylopectin.

Certain starch hydrolyzable substances (preferably with a DE of about 30)
(with text loin equivalent) may also be used.

If the starch hydrolysis product has adhesive properties,
That is, it can be used if it contains an amylopectin derivative.

The shaping agent contained in the enzyme mixture according to the invention 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 lyxose.

Suitable examples of carbohydrates with 6 carbon atoms are glycose, mannose, galactose, fructose and nrubose.

Furthermore, disaccharides, usually having 12 carbon atoms, such as sucrose, maltose or cellobiose, can also be used.

The most preferred carbohydrate is glucose.

Since glucose crystallizes rather easily (as do some other carbohydrates), some or all of the glucose or other carbohydrates may be replaced to some extent with hydrolyzed starch.

Starch hydrolysis products with a DE of about 20 to about 70, preferably about 30 to about 60 are advantageously used.

These starch hydrolysis products are also called glucose syrups.

Preferably, the amount of builder (b) is from about 40 to about 70% of the total amount.
ulder) is used as a substitute for glucose or other carbohydrates.

Suitable shaping agents are glucose, sucrose and starch hydrolysis products.

Starch hydrolysis products with adhesive properties can exhibit a dual function, ie, as adhesive and structuring agent.

A lubricant may be added to the enzyme mixture to facilitate the division of each component mixture into particles by mechanical means.

Suitably about 2 to about 7% (advantageously about 3 to about 5%) of lubricant is added to the enzyme mixture.

Examples of lubricants that can be used according to the invention are polymeric substances such as polyvinyl alcohol, paraffin oil or wax, stearic acid, and polyvinylpyrrolidone.

Glycerol also acts as a lubricant.

Moisture regulators may be included in the enzyme mixture in amounts to maintain the desired moisture content.

In order to maintain the flexibility of the enzyme particles after molding, it is about 5 to about 15
%, preferably from about 5% to about 10%.

Examples of formulations useful in maintaining this water content are polyols having 2 to 6 carbon atoms and 2 to 4 hydroxyl groups attached to different carbon atoms.

Examples of this group of compounds are ethylene glycol: 1,2- and 1,3-propylene glyconyl: 1,2-1,3- and 2,2-butylene glycol; glycerol and nrubitol.

Glycerol and sorbitol are preferably used.

To maintain the above moisture content, a moisture adjustment component of about 0.5 to about 5%, preferably about 1 to about 3%, is added depending on the environment.

Additionally, other substances such as pigments such as titanium dioxide or optical brighteners may be added to the enzyme mixture prior to certain shaping.

Amounts commonly used are from about 1 to about 10%, preferably from about 3 to about 7% pigment (particularly in the case of titanium dioxide).

Furthermore, fillers such as silica, penicillium mycelia, cellulose-containing powders or molluscs, sawdust and bentonite may be added, for example in amounts of 3 to 10%.

This filler may be added for structural stability of the particles, especially when the composition is processed in large quantities.

The components can be mixed together in any order at ambient or even elevated temperatures, the maximum temperature depending on the nature of the enzyme.

The mixture according to the invention is a powder at room temperature, but becomes plastic at elevated temperatures and when pressure is applied.

When exposed to low temperatures, the low temperature is just such that the mixture becomes plastic, and the high temperature depends on the nature of the enzyme.

Temperatures from about 40°C to about 70°C are generally suitable, although other temperatures can or should be used in certain cases.

Plasticization of this mixture can be carried out in a two-dam mixer, but in principle any mixer may be used, in which the mixture is plasticized under mild conditions (low shear) and removed from the mixer. The plasticized mixture can be removed batchwise or continuously.

Immediately after plasticization, the mixture that still retains plasticity is pumped and string-formed.
) through equipment such as gear pumps and extruders.

The filament forming device consists of a single-hole or multi-hole die plate (d
ie plate) through which the desired cross-section is formed, for example from about 0.5 to about 3 mm, preferably from 0.7 to 1.
Threads with a cross section of 5 mm are formed.

By cutting the formed threads, the desired particles are obtained in the form of granules.

A granulation device for this purpose is mounted at some distance from the die plate.

Granulation can also be carried out with a cutting device equipped with one or more movable edges for cutting the extruded product on a die plate.

The cutting device preferably consists of a number of rotating blades such that the blades move across the die plate either continuously or once per revolution depending on the position of the axis of rotation with respect to the die plate.

It is also possible to integrate the plasticizing, pumping and granulating steps into a series of devices, for example a screw extruder.

The hopper of this extruder is filled with a powdered mixture which, when fed into the apparatus, becomes plasticized by the heat and pressure generated by the rotating screw.

The components of the mixture according to the invention can also be heated separately in the desired proportions in a suitable device that combines mixing, plasticizing, pumping and extrusion through a die plate.

An example of such a device is a double screw extruder equipped with mixing means.

From about 0.5 to about 3rrLr depending on the desired size of the enzyme particles
IL, plates with orifices of 0.7 to 1.5 mm are preferably used, but in special cases larger ones are used.
Alternatively, even smaller orifices may be used.

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 water loss, the resulting particles are preferably about 0
．． 5% to about 5% (depending on the type of coating) of the coating, for example, a number of water repellents such as paraffin oil or linseed oil, some waxes such as earth's wax, etc.
th wax), cocoa butter, can-r'' wax, carnauba wax, ceresin wax, lanolin, paraffin wax, beeswax and mixtures thereof.

To avoid agglomeration of the particles which occurs when the particles are placed in a shipping bag, the coated particles as described above may be coated with an anti-caking agent, such as cornstarch or other starch, or an absorbent silica, such as Airosil. Alternatively, it is better to coat it with talc powder.

The enzyme-containing particles obtained according to the invention do not cause any or substantially no enzyme powder formation.

Enzyme powder formation can be determined by standard test methods such as the elutriation test.

This test is carried out on a 61' sample as described in Belgian Patent No. 838125.

The activity of the powder is DU (Delft Units) for proteases - British Patent No. 13533.
17 specification, page 4, line 114 et seq.).

The powder formation measured in one elutriation test is less than about 100 DU, preferably about 50 DU for the particles obtained according to the present invention.
It is below U.

The invention further relates to enzyme particles produced by the method described above.

Depending on the conditions under which the enzyme particles are manufactured, they have a cross-section of between about 0.2 and about 3, preferably between about 0.5 and about 1.5 in the case of cleaning compositions. sell.

For other purposes, such as pharmaceutical compositions to be taken orally, the particle size will generally be larger as in normal practice.

The particles are flexible and can be deformed under pressure without breaking them into powder (powder formation).

However, pressures such as those occurring in a bag filled with the particles should not deform the particles excessively.

The flexibility of the particles is compatible with different bag sizes.

For small bags, the pressure experienced by the particles below the bag is less than for large bags, and for small bags the requirements regarding resistance to deformation are less stringent than for large bags.

The present invention also relates to a cleaning composition comprising, in addition to the usual cleaning composition ingredients, enzyme-containing particles produced by the method described above.

These cleaning compositions further contain one or more detergents, such as non-ionic detergents and anionic detergents (e.g. sodium benzene sulfonate), including enzymatic personal cleaning compositions. It is commonly used as a component of products.

The cleaning compositions usually contain, inter alia, complex phosphates that have a softening effect on the cleaning water (e.g. sodium tripolyphosphate, sodium pyrophosphate) or phosphate-free water softeners (e.g. nitrilotriacetic acid or its salts or citric acid). (sodium chloride).

Other ingredients such as anhydrous sodium silicate, weak alkaline ingredients (e.g. sodium carbonate), oxidizing agents (e.g. sodium perborate), fillers (e.g. sodium sulfate) and other ingredients such as carboxymethyl cellulose, fragrances, optical brighteners and pigments such as titanium dioxide may also be added.

Enzyme particles of proteolytic enzymes produced by the process of the present invention are typically adapted to impart a proteolytic activity of from about 1000 to about 3000 DU/g, preferably from about 1500 to about 2500 DU/P, to the finished cleaning composition. used in large quantities.

The amount of detergent used in the cleaning composition is generally about 4
to about 20%, preferably about 6 to about 12%.

The amount of water softener generally ranges from about 35% to about 55%, preferably about 4%.
0 to about 50%.

The remaining ingredients generally range from about 1% to about 20% with the addition of filler to a total of 100%.

This cleaning composition is manufactured according to conventional methods.

The whole ingredients may be mixed together, but it is also possible to first prepare a masterbatch, ie a masterbatch containing some ingredients to be added in low percentages.

Also included within the scope of the present invention are the enzyme compositions described above that are suitable for producing enzyme-containing particles by the method of the present invention.

The invention is illustrated by the following examples.

Example 1 (A) Preparation of Maxatase® Containing Particles The following ingredients were mixed with heating until all ingredients were dissolved.

1 part by weight of glycerol 2 parts by weight of polyvinylpyrrolidone 0-/1/(Berol)-
80 (C18 with about 80 ethylene oxide units)
Monofatty Alcohol Polyethylene Oxide) This mixture was added to approximately 1.7 MDU/f of maxatase concentrate (26 parts by weight), whereupon the following were added: 5 parts by weight of titanium dioxide, 15 parts by weight of glucose silica. starch hydrolyzate (approximately 43 DE), 15 parts by weight glucose, 33 parts by weight Amylo gum C
LS-0473 (Abebe (Netherlands))
acetylated amylopectin) and about 1 part by weight of water.

The total water content of the resulting mixture was approximately 7%.

The mixture was mixed to a homogeneous paste at a temperature of about 65° C. and applied to an extruder equipped with a perforated plate with l1nvIL orifices.

The extruder was further equipped with two rotating cutting blades immediately after the perforated plate and a jacket for supplying cooling or heating water, if desired.

This paste was extruded at a temperature of 65° C., and the extruded fine threads were immediately cut into small particles with a cutting blade.

The small particles were cooled in a tray.

With the cross section of about 2 sections obtained in this way, o. 43M
Particles with a (calculated) proteolytic activity of DU/f were coated with 1% by weight paraffin oil followed by 3% cornstarch.

The enzyme-containing particles thus obtained can be deformed under mechanical pressure without disintegrating, but under the normal pressure that occurs in the lower part of commonly used bags, these particles are deformed by more than a few percent. There was very little.

Elutriation test showed a value of 18 DU. (B) Formulation into a cleaning composition The particles thus obtained were used in the formulation of a cleaning composition.

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 bicarbonate, 2 parts by weight sodium carboxymethyl cellulose. ,
and 4 fM dialkylphenoxypoly(ethyleneoxy)ethanol.

After intimately mixing these ingredients into a cleaning composition,
．． Five parts by weight of enzyme-containing particles (prepared as described in section (A) above) were added and immediately mixed thoroughly into the cleaning composition.

The cleaning composition thus obtained has the same enzyme activity in the cleaning composition, in which the enzyme-containing particles are replaced by a certain amount of enzyme particles obtained by the method disclosed in British Patent No. 1,324,116. (approximately 2000DU/
It had the same cleaning activity as a similar cleaning composition with P ).

Example 2 Preparation of enzyme-containing particles with different amounts of filler and different coatings Starting from the formulation given in section (A) of Example 1 for enzyme-containing particles, the following fillers and coatings were prepared as follows: The table shows that:

This shows that all the enzyme-containing particles produced gave rather low elutriation test values, with the fourth sample being the most suitable.

The enzyme particles were incorporated into a cleaning composition in the manner shown in Example 1(B).

This cleaning composition exhibited the same cleaning activity as a similar cleaning composition containing enzyme particles as described in GB 1324116.

The elutriation test described above was conducted as follows: a bed of enzyme particles is exposed to a stream of air such that particles with a predetermined final velocity or less are selected by the air stream.

This method is a modification of the standard elutriation test described in BS 3406 Vol. 3 (1963) and uses a powder filter (dust
filter) in a vertically arranged elutriation tube.

The selected particles are collected on a filter, weighed,
Its enzymatic activity is measured (expressed in glycine units or delft units).

The average air flow velocity was 0.8 m/sec. Example 3 Preparation of enzyme-containing particles with varying amounts of other fillers Starting from the formulation shown for enzyme-containing particles in Example 1(A), the following fillers were used: 2% Erosil 972
: 5% and 10% bentonite; 5% penicillin mycelia (obtained from the fermentation broth obtained from penicillin G fermentation), the particles were coated with 1% paraffin oil followed by 1% Erosil 972.

All of the fillers presented here were found to be useful, although the particles containing 10% bentonite tended to be somewhat brittle.

The enzyme particles were incorporated into a cleaning composition according to the method shown in Example 1 (Bl).

This cleaning composition showed the same cleaning activity as a similar cleaning composition containing enzyme particles according to GB 1324116.

Example 4 Modification of the formulation of Example 1 for the production of enzyme-containing particles What happens if the production of particles according to Example 1(A) is repeated? Equal amount of parsley (P
aselii) MD-30C7 (a starch hydrolysis product with a DE of about 35) manufactured by Bebe (Netherlands).

The particles were treated with 1% paraffin oil followed by 1% Erosil 972.
It was coated with.

In another experiment, the preparation of the particles of Example 1(A) was repeated, but in this case the Berolu 80, polyvinylpyrrolidone, and glucose were omitted and 10 parts by weight of bentonite was used instead.

All ingredients were mixed together at a temperature of about 651°C and the resulting paste was extruded and cut into particles.

The particles were coated in the same manner as the particles containing Pase IJMD-30.

The particles produced by both methods according to this example were found to be extremely useful, and the formulation of the cleaning composition [a composition produced in the same manner as in Example 1 (B)] was described in British Patent No. 1,324,116. showed substantially the same cleaning activity as similar cleaning compositions containing enzyme particles.

Example 5 Production of Enzyme-Containing Particles for Medicinal Use The following formulation was used to produce granules according to the invention: 25% glucoamylase (approximately 25000 U/g), 6.25% invertase (approximately 325000 SU/g), 45%. of Amylogum CLS-0473, 20% glucose syrup (a starch hydrolysis product of approximately 43 DE), 3.75% glycerol.

This powder is directly extruded through an orifice with a diameter of 1 mm.
The extrudate was cut to form granules.

The granules were coated as described in Example 3.

Products of this type are useful for oral administration to patients suffering from carbohydrate metabolism inhibition caused by invertase, glucoamylase or isomaltase deficiencies.

Example 6 Alternative method for the production of maxatase-containing particles 4 The following formulation was used for this purpose: 50% maxatase (230 million DU/S'), 3
5% Amylogum CLS-0473, 15% glucose syrup (approximately 43 DE of starch hydrolysis product).

A mixture of this formulation was formed into granules as shown in Example 5.

After granulation, the particles were coated with 5% titanium dioxide.

Example 7 Another alternative for the production of maxatase-containing particles The following formulation was used for this purpose: 45% methylcellulose, 20% maxatase (240 million DU/P), 10
% glucose syrup (approx. 43 DE starch hydrolysis product), 4% paraffin wax, 5% titanium dioxide, 2% glycerol, 14% glucose.

Granules were prepared according to the method described in Example 5 and were shown to have similar properties to the granules of Example 5.

(Coating of the granules was carried out as described in Example 3.

) Example 8 Yet another alternative for the production of maxatase-containing particles The following formulation was used for this purpose: 45% gum arabic, 20% maxatase (24 million DU/g), 10%
glucose syrup (43DE starch hydrolysis product).

4% paraffin wax, 5% titanium dioxide, 2% glycerol, 14% glucose.

The granules were manufactured according to the method described in Example 5 and were shown to have similar properties to the Example 5 granules.

(Coating of the granules was carried out as described in Example 3) Example 9 Amylase-containing product The following formulation was used for this purpose: 25% amylase (164oo BAU/f), 37%
Amylogum CLS-0473, 16% glucose syrup (a starch hydrolyzate of approximately 43 DE), 16% glucose, 5% titanium dioxide, 1% glycerol.

The following alternative formulation was also used: 50% amylase (16000 BAU/P), 35%
Amikogum CLS-0473, 15% glucose syrup (a starch hydrolysis product of about 43 DE).

Granules were manufactured from each formulation according to the method described in Example 5, and both were shown to have similar properties to the Example 5 granules.

(Coating of the granules was carried out as described in Example 3).

Example 10 Several formulations containing maxatase Coating of the particles was carried out as described in Example 3.

Example 11 Alkaline Protease-Containing Product The following formulation was used for this purpose: 34% Amiigum CLS-0473, 17% Glucose, 17% Glucose Syrup (starch hydrolysis product of about 43 DE), 7 % stearic acid, 20% PB92 (1.7 million ADU/7) (1), 5%
of titanium dioxide.

(To) (1) PB92 is an alkaline protease described in US Pat. No. 4,002,572.

The granules were manufactured according to the method described in Example 5 and were shown to have similar properties to the granules of Example 5: in particular, an elutriation test performed on 61 samples showed a value of 95 ADU/P.

(Coating of the granules was carried out as described in Example 3.

) Example 12 Storage stability of maxatase-containing granules according to the invention Commercial cleaning powder containing sodium perborate (40
Use (1).

Example 10 (sample 5) of enzyme granules in an amount to give an activity of 600 oDU/f and pre-coated with a 1:1 mixture of 1% glycerol monostearate and paraffin oil.
) were added and the mixture was mixed thoroughly again.

About 201 liters of each from the above mixture to test storage stability.
Two samples were weighed: the sample immediately after mixing and the sample at 37°C.
Samples were collected after storage for 0.5, 1, 2, and 3 months.

Synthetic tap water containing sodium dithionate (Cab, 2 of 111II19/J) to neutralize the effect of perborate
7.5my/l MgO and 2101n9/l Na
The sample was dissolved in tap water containing HC03 and showing a German hardness of 15°), diluted with the synthetic tap water to a concentration appropriate for the Delft unit activity test, and then tested (see British Patent No. 1,353,317). ) (Test values are shown in series A in the following table).

A similar procedure was carried out using commercially available granules of the same enzyme (trade name: Maxatase P, an enzyme manufactured by Gist-Procades N.■., Netherlands, produced by the method described in British Patent No. 1,324,116). A test was conducted (test values are shown in series B in the following table).

The following results were obtained: This table shows that the storage stability of the A-series granules according to the invention is good and much better than the comparative B-series granules (which also have considerably better stability). It shows.

Example 13 Lactase-containing product The following formulation was used for this purpose: 45% Amylogum CLS-0473, 30% lactase (precipitated), 25% glucose syrup (starch hydrolysis product of approx. 43 DE). ).

Granules were produced as described in Example 5 and coated as described in Example 3.

When the temperature was kept at or below 5.0°C during the manufacture of the granules, the activity of the granules was 95% of the starting activity, but when the temperature was increased to 50-70°C, the residual activity was significantly reduced. It was low, ie 55% of the initial activity.

This example shows that the temperature used is highly dependent on the activity of the enzyme.

Example 14 The following formulation was used to produce particles by the method described in Example 1.

1 part by weight glycerol, 2 parts by weight polyvinylpyrrolidone, 2 parts by weight Verol 80, 1 part by weight Maxatase, 5 parts by weight titanium dioxide, 22 parts by weight glucose syrup (starch hydrolysis product of about 43 DE) , 21 parts by weight of glucose, and 46 parts by weight of amiigum CLS-0473.

The particles produced were coated as described in Example 1.

Claims (1)

[Claims] 1. A method for producing enzyme-containing particles that does not turn into powder at all or substantially when mechanical pressure is applied from the outside, wherein when the enzyme is formed into particles, a desired amount of the enzyme is contained in the particles. of a dry or substantially dry enzyme in an amount to provide enzyme activity of about 20% of a hydrophilic organic adhesive having an affinity for the enzyme.
0 to about 60%, about 10 to 60% of a shaping agent suitable for use in the enzyme composition, and, if necessary, sufficient water to bring the water content in the particles to 5 to 15% upon shaping. A process as described above, characterized in that the mixture obtained is mechanically divided into particles of the desired size and the particles are coated to prevent moisture loss. 2 less than 50% of the enzyme in dry or substantially dry form;
20 to 60 of a hydrophilic organic adhesive with affinity for the enzyme.
%, 20-6 of the shaping agent preferably used in the enzyme composition
0%, optionally a small amount of water, and a sufficient amount of moisture regulator to maintain the moisture content in the particles between 5 and 15% (at the time of molding) at room temperature and normal relative humidity. 2. A method as claimed in claim 1, comprising mechanically dividing the mixture into particles of the desired diameter and coating the particles to prevent loss of moisture content. 3. The method according to claim 1 or 2, wherein the hydrophilic adhesive is selected from starch and cellulose derivatives. 4. The hydrophilic adhesive according to claim 1, 2 or 3, wherein the hydrophilic adhesive is selected from acetylated amylopectin, gum arabic, dextrin, gum karaya, methylcellulose, tragacanth, methylamylopectin and a starch hydrolysis product having adhesive properties. Method. 5. Claim 1, wherein the hydrophilic adhesive is acetylated amylopectin with a degree of acetylation of about 5 to about 30%.
4. The method according to any one of items 4 to 4. 6. A method according to any one of claims 1 to 5, wherein the amount of hydrophilic adhesive used is about 30 to about 50%. 7. The method according to any one of claims 1 to 6, wherein the shaping agent is a water-soluble carbohydrate having 5 to 12 carbon atoms. 8. The method according to any one of claims 1 to 7, wherein the shaping agent is selected from glucose, sucrose and starch hydrolysis products. 9. Any of claims 1 to 8, wherein the shaping agent is a 40 to 70% starch hydrolyzate and a mixture of the hydrolyzate and glucose having a dextrose equivalent of about 20 to about 70. Method described in Crab. 10. The method of claim 9, wherein the starch hydrolysis product has a dextrose equivalent weight of about 30 to about 60. 11. A method according to any of claims 1 to 10, wherein the amount of shaping agent used is about 20 to about 45%. 12 2 to 4 hydroxyl groups attached to different carbon atoms and 2
12. A method according to any one of claims 1 to 11, in which a moisture control agent selected from polyols having .about.6 carbon atoms is added. 13. The method of claim 12, wherein the moisture control agent is selected from glycerol and nrubitol. 14 The amount of moisture control agent used is about 0.5 to about 5%
The method according to claim 12 or 13. 15. The method of claim 14, wherein the amount of moisture control agent is from about 1 to about 3%. 16. The method according to any one of claims 1 to 15, wherein the 16 enzymes are selected from proteases, amylases, lipases, lactases, invertases and glycoamylases. 17. The method of claim 16, wherein the protease is selected from those produced by Bacillus strains. 18 The Bacillus strain is Bacillus subtilis (Bacillus subtilis).
illus subtiLis), B. licheniformis or B. alcalop
hilus). 19. The method of claim 16, wherein the amylase is selected from those produced by Bacillus subtilis. 17. The method of claim 16, wherein the 20 lipase is selected from those produced by Candida strains. 21 Candeida strain is Candeida cylindriase (C
andida cylindraceae). 22. The method of claim 1, wherein the amount of enzyme used is less than about 50%. 23 Claims 1 to 2 further adding a lubricant
The method described in any of Section 2. 24. The method of claim 23, wherein the lubricant is selected from paraffin oil or wax, stearic acid, polyvinyl alcohol, polyvinylpyrrolidone and glycanol. 25. The method of claim 23 or 24, wherein the amount of lubricant used is about 2 to about 7%. 26. The method of claim 25, wherein the amount of lubricant is about 3% to about 5%. 27. A method according to any one of claims 1 to 26, wherein the division of the mixture is carried out by a pump and a filament forming device. 28. The method of claim 27, wherein the filament forming device comprises a single or multi-hole die plate having an orifice with a cross-section of about 0.5 to about 311L7IL. 29. The method of claim 28, wherein the orifice has a cross section of about 0.7 to about 1.5 mm. 30. The method of any of claims 1-29, wherein the particles are coated with about 0.5 to about 5% water repellent. 31 The water repellent is paraffin oil or linseed oil, ground wax,
cocoa butter, candelilla wax, carnauba wax,
31. The method of claim 30, wherein the wax is selected from paraffin wax and beeswax, ceresin wax and lanolin, and mixtures thereof. 32. The method of claim 30 or 31, wherein the particles are further coated with an anti-caking agent. 33. The method of claim 32, wherein the anti-caking agent is selected from cornstarch and other starches, absorbent silica and talcum powder. 34. A method according to any of claims 1 to 33, wherein the dividing of the mixture into particles is carried out at about 40 to about 70'C. 35. A method according to claim 1 for obtaining enzyme-containing particles substantially as described above, which do not become powdered at all or substantially when subjected to external mechanical pressure. 36 Enzyme-containing particles that are substantially the same as those described in the preceding paragraphs, particularly in connection with any of Examples 1 to 14, which do not completely or substantially become powder when external mechanical pressure is applied. A method according to claim 1 for obtaining enzyme-containing particles. 37 dry or substantially dry enzyme, about 20 to about 60% of a hydrophilic organic adhesive with affinity for the enzyme;
An enzyme-containing composition comprising from about 10 to about 60% of a suitable shaping agent for enzyme compositions and a small amount of water. 38 dry or substantially dry enzyme, about 20 to about 60% of a hydrophilic organic adhesive with affinity for the enzyme;
A cleaning composition comprising an enzyme-containing composition comprising from about io to about 60% of a suitable shaping agent for enzyme compositions and a small amount of water and conventional cleaning composition ingredients. 39 The activity of the finished cleaning composition is about 1000 to about 3
39. A cleaning composition according to claim 38, comprising proteolytic enzyme-containing particles in an amount such that 000 DU/f. 40. The cleaning composition of claim 39, comprising protease-containing particles in an amount such that the finished cleaning composition has an activity of about 1500 to about 2500 DU/1. 41 Approximately 4 components are usually included as detergent composition components.
- about 20% detergent, about 35 to about 55% water softener,
40. A cleaning composition according to claim 38 or 39, containing fillers and other conventional detergent composition ingredients added up to 100%. 42. The cleaning composition of claim 41 containing about 6 to about 12% detergent and about 40 to about 50% water softener.