JPH10204494A - Powdery enzyme preparation and granule using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a powdery enzyme preparation useful for a detergent for clothing, tableware, housing, etc., capable of exhibiting excellent free fluidity and aggregation resistance during preservation without deactivating an enzyme by including an enzyme and a specific amount of an ionic surfactant. SOLUTION: This preparation comprises (A) an enzyme such as protease, esterase, carbohydrase or lyase and (B) 0.2-10wt.% of the protein amount of the component A of an ionic surfactant [e.g. an alkyl (ether) sulfate or an alkenyl (ether) sulfate]. The preparation is obtained by spray-drying a slurried aqueous solution containing the component A and the component B in a fixed ratio, having 1-20wt.% of solid content concentration.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a powdery enzyme preparation having improved free-flowing properties and cohesiveness during storage and a granulated product containing the same.

[0002]

2. Description of the Related Art Various enzymes are often added to detergents and bleaching agents for clothing to enhance the washing effect. These enzymes are not deactivated during storage, and are sufficiently formulated as a powdered enzyme preparation or a granulated form thereof in order to sufficiently exhibit the activity during the washing step. Powdered enzyme preparations are usually produced by a spray drying method,
When a powdery enzyme preparation is produced from a low-concentration slurry such as an aqueous enzyme solution, it has been recognized that the resulting preparation does not always have sufficient free-flowing properties, and that it absorbs and aggregates during storage. For this reason, handling becomes difficult when preparing a granulated product using the same and / or when blending it into a detergent or a bleaching agent, and problems such as inactivation of enzymes occur.

[0003] In general, the physical properties of a powdery preparation are adjusted by controlling the operating conditions of a drying apparatus, but this has limitations. In addition, it is possible to improve the physical properties of the slurry to be sprayed by increasing the concentration of the slurry.However, if the amount of water in the slurry is excessively reduced, the viscosity of the slurry increases. When the enzyme powder is obtained by drying by a drying method, there is a problem that spraying becomes difficult. In addition, since the precipitation of the enzyme occurs by increasing the concentration of the slurry,
A decrease in recovery is also observed. In addition, although the addition of a drying aid is also effective for improving the physical properties of the powdered enzyme preparation, the amount of addition is limited, and there is a problem that the enzyme activity is reduced when used in a large amount.

[0004]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a powdery enzyme preparation which has no deactivation of the enzyme, and has improved free-flowing properties and improved cohesion during storage. It is to provide granules.

[0005]

The present inventors have made various studies on improving the flowability of a powdered enzyme preparation. As a result, the present inventors surprisingly found that an enzyme such as a hydrolase and a small amount of an ionic surfactant were used. It was found that the enzyme was not inactivated even when uniformly dispersed and coexisted, and that a powdery enzyme preparation with improved free-flowing properties and improved cohesiveness during storage was obtained, thereby completing the present invention. .

That is, the present invention provides a powdery enzyme preparation containing an enzyme and an ionic surfactant in an amount of 0.2 to 10% by weight based on the amount of the enzyme protein. In addition, the present invention relates to an enzyme protein amount of 0.2 to 1%.
It is intended to provide a method for producing the above-mentioned powdery enzyme preparation, which comprises spray-drying an enzyme aqueous solution containing 0% by weight of an ionic surfactant. Further, the present invention provides an enzyme-containing granule comprising the above-mentioned powdery enzyme preparation and a binder.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The enzyme used in the present invention is not particularly limited as long as it is an enzyme blended in a bleach or a detergent. Specific examples include protease, esterase, carbohydrase, lyase and the like.

Specific examples of proteases include pepsin, trypsin, chymotrypsin, collagenase, keratinase, elastase, subtilisin, papain,
Examples include aminopeptidase, carboxypeptidase and the like.

Specific examples of esterases include gastric lipase, pancreatic lipase, plant lipases, phospholipases, cholinesterases, phosphatases and the like.

As carbohydrase, cellulase,
Examples include maltase, saccharase, amylase, pectinase, α- and β-glycosidase. Examples of lyases include carboxy lyase, aldehyde lyase, oxoacid lyase, hydrolyase, lyase that acts on polysaccharides, and ammonia lyase.

Among the ionic surfactants used in the present invention, examples of the anionic surfactant include alkylbenzene sulfonate, alkyl or alkenyl ether sulfate (AES), and alkyl or alkenyl sulfate (A
S), olefin sulfonate (AOS), alkane sulfonate, saturated or unsaturated fatty acid salt, alkyl or alkenyl ether carboxylate, α-sulfo fatty acid salt or ester, amino acid type surfactant, N-acyl amino acid type Examples thereof include a surfactant, an alkyl or alkenyl phosphate or a salt thereof, and a carboxylic acid type polymer surfactant. Examples of the amphoteric surfactant include a carboxy or sulfobetaine type surfactant. Examples of the cationic surfactant include a quaternary ammonium salt. In the present invention, alkyl or alkenyl ether sulfate (AES) and alkyl or alkenyl sulfate (AS) are particularly preferable.

In the powdered enzyme preparation of the present invention, the content of the ionic surfactant is from 0.2 to 10% by weight of the amount of the enzyme protein. Is not obtained, and when the added amount exceeds 10% by weight, the enzyme is inactivated, which is not preferable. In addition, the nonionic surfactant did not show the effect of improving the physical properties.

The powdered enzyme preparation of the present invention may contain a diluent (eg, a bulking agent, a filler, etc.), a drying accelerator, a buffering agent, etc., as required, for keeping the specific activity of the preparation constant. Can be. Examples of the drying accelerator include calcium chloride and sodium sulfate. Examples of extenders or fillers include sulfates, halides, carbonates, phosphates, silicates, borates and the like. More specifically, the following compounds are mentioned.

Sulfates: sodium sulfate, potassium sulfate,
Calcium sulfate, magnesium sulfate, zinc sulfate, ferrous sulfate, sodium thiosulfate, aluminum sulfate Halogen: sodium chloride, potassium chloride, calcium chloride, magnesium chloride, potassium bromide Carbonate: sodium carbonate, sodium hydrogen carbonate, potassium carbonate , Calcium carbonate, magnesium carbonate Phosphate: sodium phosphate, sodium hydrogen phosphate,
Sodium dihydrogen phosphate, potassium phosphate, potassium dihydrogen phosphate, sodium pyrophosphate silicate: sodium silicate, sodium metasilicate,
Potassium silicate, calcium silicate Boric acid (salt): Borax, potassium borate, boric acid Saccharides: All monosaccharides, all disaccharides, for example, maltose type 2
Sugars and trehalose-type disaccharides

These are used singly or as a mixture of two or more. In addition, known coloring agents and stabilizers in the field of granulation or enzyme agents can be used as appropriate, and further, flavoring agents, deodorants, antistatic agents and the like can be used.

The powdered enzyme preparation of the present invention is produced by treating an enzyme aqueous solution containing a predetermined amount of an ionic surfactant according to a conventional method. A slurry having a concentration of 1 to 20% is solidified by spray drying. Is particularly preferable.
Here, it is preferable that all the components necessary for the composition of the target powdery enzyme preparation are blended in the enzyme aqueous solution.

In order to produce the powdered enzyme preparation of the present invention by spray drying, the enzyme aqueous solution may be dried using a conventional spray dryer. The spray dryer generally has a nozzle type and a disk type, and can be used properly depending on the particle size of a target enzyme preparation. A nozzle type is preferable when manufacturing a preparation having a small particle size (1 μm or less), and a disk type is preferable when manufacturing a preparation having a large particle size.

The hot air temperature in the dryer is 100 to 20.
The temperature is preferably 0 ° C, especially 130 to 170 ° C, and the exhaust air temperature (corresponding to the temperature of the enzyme aqueous solution) is preferably 50 to 100 ° C, particularly preferably 60 to 100 ° C.

In order to granulate the powdery enzyme preparation thus obtained, additives necessary for granulation may be blended and granulated according to a conventional method. Such additives include binders. As the binder, a water-soluble organic binder, in particular, (a) polyethylene glycol having a melting point of 35 ° C. or more and its derivatives, polyoxyethylene.
Water-soluble polymers selected from the group consisting of polyoxypropylene copolymers, (b) nonionic surfactants having a melting point or pour point of 35 ° C. or higher, and (c) polycarboxylates having an average molecular weight of 4000 or higher. One type or two or more types may be mentioned.

Particularly preferred water-soluble organic binders include polyethylene glycol (a) and derivatives thereof such as polyethylene glycol, polyethylene glycol sulfate, and methoxypolyethylene glycol, and (b) nonionic surfactants such as poly (ethylene glycol). Examples of the polycarboxylate (c) include alkali metal salts such as polyacrylic acid, acrylic acid-maleic acid copolymer, and polyacetal carboxylate.

In particular, these water-soluble organic binders are useful because they are also components used in detergents. The amount of the ordinary water-soluble organic binder used cannot be unconditionally determined because there is a difference in properties between the binders. However, in order to enhance the enzymatic activity of the obtained enzyme granule as much as possible, the binder effect is expressed with as little as possible. Are generally preferred. Therefore, these water-soluble organic binders
In the enzyme granulated product, usually 5 to 50% by weight, preferably 10 to 10% by weight.
30% by weight is contained.

In the present invention, a powdery extender can be further added, if necessary. As fillers, alkali metal or alkaline earth metal sulfates, carbonates,
One or more inorganic salts selected from the group consisting of hydrochlorides are used. That is, among them, water-soluble inorganic alkali metal salts such as sodium sulfate, sodium carbonate, and sodium chloride are preferable in consideration of the influence on washing and the like. Other extenders include water-soluble organic acid salts such as sodium citrate, talc, titanium oxide, calcium carbonate, zeolite, magnesium carbonate, activated clay, kaolin, diatomaceous earth, bentonite, perlite, acidic clay, and the like.

Further, in the granulated product of the present invention, various inorganic salts such as calcium salts and magnesium salts, or organic substances such as surfactants, sugars and carboxymethyl cellulose can be used. Furthermore, synthetic hectorite or sepiolite can be blended to adsorb odorous components derived from culture. It is also optional to add a dye or a dye to color the enzyme granules.

The granulation means is not particularly limited, and may be wet granulation or dry granulation. The granulation methods include extrusion granulation, tumbling granulation, pulverized granulation, fluidized bed granulation, and spraying. Granulation, crushing granulation and the like can be mentioned. Among them, rolling granulation,
In particular, the stirring rolling granulation method is preferable. Specific examples of the stirring tumbling granulator include Henschel mixer (Mitsui Miike Kakoki Co., Ltd.), high speed mixer (Fukae Kogyo Co., Ltd.),
Vertical granulator (Fuji Sangyo Co., Ltd.) and the like can be mentioned. The common feature is that they have a vertical stirring shaft with stirring blades mounted inside a rigid mixing tank. A Lodige mixer (Lodige), a model granulator with a horizontal stirring axis, can also be used.

The particle size of the granules thus obtained is not particularly limited, but the average particle size is preferably from 200 to 3000 μm, particularly preferably from 350 to 1500 μm.

The enzyme-containing granules of the present invention can be used without coating, but coating is desirable because the stability is further improved. The coating agent for the enzyme-containing granules of the present invention is not particularly limited, but polyethylene glycol,
Water-soluble film-forming polymers such as polyacrylates, polyvinyl alcohol, polyvinylpyrrolidone, cellulose derivatives, starch derivatives, etc .; these polymers and water-soluble or hardly soluble inorganic particles such as talc, clay, titanium oxide, calcium carbonate, etc., or alkali metal silicon And combinations with protecting agents such as acid salts and alkali metal carbonates. The coating agent is preferably used in a weight ratio of 0.01 to 0.7, particularly 0.05 to 0.6, based on the enzyme-containing granules.

The method for coating the enzyme-containing granulated product of the present invention includes a method of coating with an apparatus such as a fluidized bed granulator, a coating pan granulator, and a stirring granulator by a conventional method.

The enzyme-containing granule of the present invention is useful as a component of a detergent composition, and the detergent composition containing the granule is used as a detergent for clothing, tableware, residence, and the like. be able to.

[0029]

EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited thereto.

Example 1 (1) As an enzyme aqueous solution, an aqueous solution containing a crude enzyme having protease activity (derived from Bacillus sp. KSM-K16 (FERM P-3367)) (enzyme protein concentration: 7.5% by weight) was used. Was. In this aqueous solution, relative to the amount of enzyme protein in the aqueous solution,
Various surfactants shown in Table 1 were added so as to be 10% by weight to prepare an aqueous enzyme solution. (2) The enzyme aqueous solution obtained in the control (no surfactant) and the enzyme aqueous solution obtained in (1) was spray-dried with an atomizer type spray dryer at a hot air temperature of 150 ° C. and an exhaust air temperature of 75 ° C. ５０50 μm), and the angle of repose, the angle of collapse, the angle of difference and the degree of cohesion were measured by the following methods. Table 1 shows the results. These were all measured using a powder tester (manufactured by Horikawa Micron Corporation). The residual enzyme activity was about 92% for all powdered enzyme preparations.

(Measurement of angle of repose) The powdered enzyme preparation was placed on a sieve (opening: 710 μm), the sieve was vibrated, and the preparation was measured by an injection method through a funnel to obtain the angle of repose. The smaller the angle of repose is, the better the free flowing property is, and the larger the angle of repose is, the lower the free flowing property is.

(Measurement of collapse angle) After the angle of repose was measured by the above-described method, the angle at which the granular material was collapsed by applying a certain impact was measured and defined as the collapse angle. The smaller the collapse angle is, the better the free flowing property is, and the larger the collapse angle is, the lower the free flowing property is.

(Calculation of Difference Angle) The difference between the angle of repose and the collapse angle was calculated as the difference angle.

(Measurement of Aggregation Degree) 2 g of the powdered enzyme preparation was weighed, and three sieves (mesh 149, 250, 350 μm) were weighed.
m) is placed on the pile, the sieve is vibrated, and the powder remaining on the three sieves after stopping is weighed. From this, the degree of aggregation was measured. The smaller the degree of cohesion, the better the free flowing property,
Larger ones are less free flowing.

[0035]

[Table 1]

Example 2 A raw material having the following composition was granulated with a high-speed mixer (FS-5, manufactured by Fukae Kogyo Co., Ltd.) to obtain an enzyme-containing granule.

[0037]

Table 2 Powdery enzyme preparation obtained in Example 1 18 (% by weight) Nuclear substance (11% by weight of particles having a particle diameter of 500 μm or less, 9% by weight of particles having a particle diameter of 700 μm or more, and an average particle diameter of 610 μm) Sodium binder) 55 Binder (polyethylene glycol 6000 (manufactured by Kao Corporation)) 6.5 Titanium oxide 2 Sodium sulfate Balance

That is, the above-mentioned raw materials (total 3.5 kg) were all charged into a mixer, and agitator 480 rpm, chopper 900 rpm while flowing hot water at 70 ° C. through the jacket.
The contents were heated to 60 ° C., and the hot water was stopped. By granulation operation for about 15 minutes from the input of raw materials,
An enzyme-containing granulated product (98% or more in particle diameter of 350 μm or more and 1000 μm or less) was obtained.

[0039]

[Table 3]

Example 3 As a surfactant, sodium lauryl sulfate (Kao Corporation)
And Emul 10) in the same manner as in Example 1 except that the amount of the surfactant relative to the amount of the enzyme protein was changed to 2, 5, and 10% by weight to produce a powdered enzyme preparation and a control (without a surfactant). did. In the raw material composition shown in Table 2, the powdery enzyme preparation was replaced with these, and the mixture was blended in the same manner except that the amount of the binder was changed to 6.7% by weight. I got

[0041]

[Table 4]

Example 4 As a surfactant, sodium lauryl sulfate (Kao Corporation)
And Emul 10) in the same manner as in Example 1 to produce a powdered enzyme preparation and a control (without surfactant). In the raw material composition shown in Table 2, the powdery enzyme preparation was replaced with these, and the binder amount was changed to 6.7, 7.4,
Except for using 8.1% by weight, the same blending was carried out, and an enzyme-containing granulated product was obtained in the same manner as in Example 2. Granulation yield (%)
Are shown in Table 5.

[0043]

[Table 5]

Claims (3)

[Claims] 1. An enzyme and the amount of the enzyme protein of 0.2 to 1
A powdery enzyme preparation comprising 0% by weight of an ionic surfactant. 2. The method for producing a powdery enzyme preparation according to claim 1, wherein an enzyme aqueous solution containing an ionic surfactant in an amount of 0.2 to 10% by weight of the enzyme protein is spray-dried. 3. An enzyme-containing granulated product comprising the powdered enzyme preparation according to claim 1 and a binder.