JPS62257990A - Production of enzyme granule for detergent - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed Description of the Invention] [Field of Industrial Application] The present invention provides enzyme granules for detergents, which have less enzyme deactivation during production and have a narrow particle size distribution, making it easy to control the particle size. Regarding the manufacturing method.

[Conventional technology and its problems]

Powder detergents for clothing often contain various enzymes to enhance their cleaning action. These enzymes are expected to perform their original enzymatic action during the washing process, but they are easily deactivated by detergent components during storage, and countermeasures have been taken to prevent this. That is, the basic method is to make the contact area with the detergent as small as possible by granulating the enzyme, and at the same time, a stabilizer has been used in combination.

On the other hand, granulation of enzymes is also meaningful for the purpose of avoiding contact with enzymes by workers and consumers as much as possible during the production or use of detergents.

Therefore, for both reasons, there has been a need for enzyme granules that are hard to break and do not generate dust.

To achieve this objective, a method is known in which enzymes are dispersed in molten polyethylene glycol or nonionic surfactants and spray cooled to obtain spherical granules. However, when dispersed in a substance with a high melting point, the enzyme is deactivated by heat due to the long time required for spray cooling, and in a substance with a low melting point, problems such as sticky granule surfaces occur.

Apart from this, it is also known to mix fibers to form granules so that the particles do not break when subjected to mechanical forces. In this case, if the kneaded material containing fibers is extruded and granulated, for example, the productivity will drop significantly.

In addition, when attempting to obtain strong particles by wet granulation using an aqueous solution of starch, carboxymethyl cellulose (CMC), etc. as a binder, the particles are exposed to high temperatures during the drying process, causing enzyme deactivation. Probability is high.

Therefore, in the enzyme granulation process, it has been desired to develop a technology that allows particle size to be controlled arbitrarily to some extent, has a narrow particle size distribution, and shortens the heating time as much as possible. This is expected to not only reduce the burden on equipment for the classification and recovery process of the granulated product, but also eliminate the deactivation of enzymes when re-granulating the recovered product.

[Means for solving problems]

As a result of intensive research to solve the above problems, the present inventors discovered a method for producing enzyme granules with almost no enzyme deactivation during the granulation process and a narrow particle size distribution, and completed the present invention. .

That is, the present invention provides detergent enzyme powder with an average particle size of 0.
, 2mm to 1.2mm+ as the core material, with a melting point or softening point of 35°C to 70°C.
A detergent characterized in that it is granulated using a stirring rotary granulator using a water-soluble organic binder at ℃ so that the average particle size of the granules is 1 to 2 times the average particle size of the core material. The present invention provides a method for producing enzyme granules for use.

The production method of the present invention is characterized in that an enzyme is attached to the surface of core particles using a binder to form spherical particles. Moreover, at this time, it is important not to cause aggregation of the core particles. The granules obtained in this way have a spherical shape with - core particles at the center and enzymes fixed on the surface with a binder, so they are similar to general granules in which fine inorganic salt particles are aggregated with a binder. Compared to granules, spherical granules with a narrow particle size distribution are obtained.

Moreover, the particle size of the granulated product has the advantage that it can be easily controlled by selecting the particle size of the core particles.

The components used in the present invention and the granulation method will be explained below.

Enzyme The enzyme used in the present invention is one that performs its original enzymatic action during the washing process, and examples thereof include one type or a mixture selected from protease, esterase, and carbohydrase.

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

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

Carbohydrases include cellulase, maltase,
Saccharase, amylase, pectinase, α- and β
-Glycosidases and the like.

For detergents, enzymes produced by microorganisms obtained by culture are advantageous in terms of cost. In the present invention, a dried powder after culturing and separation is used. The average particle size is preferably 20% or less of the average particle size of the nuclear material. During powdering, enzyme stabilizers such as calcium chloride and powdering aids such as Glauber's salt and sodium chloride may be added.

1. 1st birthday The core material for granulation is selected from those that meet the following requirements:

(1) It must be water-soluble; in other words, since the product of the present invention is an enzyme granule for detergent formulation, it must be soluble in water.

(2) Do not inhibit enzyme activity or impair enzyme stability.

(3) Those with an average particle diameter of 0.2 mm to 1.2 mm. In principle, the particle size referred to here refers to the value of primary particles, but this does not apply to particles that have been granulated in advance and can be considered as primary particles. Approximately 50% to 100% of the average particle size of the granules
% of the average particle size is used. The narrower the particle size distribution is, the more desirable it is, and in particular, excluding coarse particles with a size twice or more the average particle size brings about good results.

(4) In addition, it is necessary to have a melting point or softening point of 80 degrees or higher, low hygroscopicity, high mechanical strength (and low adhesiveness).

What satisfies the above requirements varies depending on the type of enzyme used, but examples of commonly usable nuclear substances include sodium chloride, potassium chloride, Glauber's salt, soda carbonate, and sugar.

Binder One of the features of the present invention is dry granulation using stirring transfer, as will be described later in the granulation method. Therefore, the binder is selected from substances having a melting point or softening point of 35°C to 70°C. Specific examples include nonionic surfactants such as polyethylene glycol, polyoxyethylene-polyoxypropylene glycol, and polyoxyethylene alkyl ether, and one type or a mixture thereof can be used.

+O([1(Arrangement) In the present invention, in addition to enzymes and binders, titanium oxide, talc, silica, clay, etc. with an average particle diameter of 1 (bat) or less are used in addition to enzymes and binders. In order to stabilize the enzyme, it is also possible to use various inorganic salts such as calcium salts and magnesium salts, or organic substances such as surfactants, sugars, and carboxymethyl cellulose. Hectorite or sepiolite can also be blended to adsorb odorous components derived from culture.Also, it is optional to blend pigments or dyes to color the enzyme granules.

These components may be added in advance during the enzyme powder manufacturing process or may be added during the granulation process of the present invention.

The blending ratio of detergent enzyme, nuclear material, and binder is 1 nuclear material.
It is preferable that the amount of the enzyme powder is 9 to 100 parts by weight and the binder is 9 to 60 parts by weight, and the weight ratio of the enzyme powder to the binder is 0.2 to 2 parts by weight of the binder to 1 part of the enzyme powder.

The present invention is characterized by dry granulation using a stirring and rolling granulator. Specific examples of stirring rotary granulators include Henschel mixer (Mitsui Miike Kakoki @), high speed mixer (Fukae Kogyo ■), and vertical granulator.
(Fuji Sangyo @), etc. What these types have in common is that they have a vertical stirring shaft with stirring blades attached inside the vertical mixing tank. A Ledige mixer (Ledige GmbH, West Germany), which is a horizontal granulator with a horizontal stirring shaft, can be used as well.

The core particles, binder, enzyme powder, and other components as necessary are placed in this tank and mixed by gentle stirring while flowing a heating medium such as hot water through the jacket of the granulator. Care must be taken because vigorous mixing at this point will cause destruction of the core particles. Eventually, the temperature of the raw material in the tank will rise to
When the melting point or softening point of the binder is exceeded, granulation begins centering on the core particles, but spherical particles are formed by rolling action on the surface of the stirring blade.

If the stirring is continued further, coarse lumps may be formed due to agglomeration of particles, and the thermal effect on the enzyme will also increase, which is undesirable. However, it is generally difficult to detect the optimal end point of granulation. Taking advantage of the fact that the power required for stirring (e.g. electric current value) increases when granulation begins, it is easy to determine the composition of the desired granules and to experiment with the agitating rotary granulator to be used in advance. can be done.

The enzyme granules obtained by the production method according to the present invention can be coated with polyethylene glycol or a nonionic surfactant, if necessary. Moreover, at this time, there is no problem in using together the materials mentioned in the section of the other components above.

〔Example〕

EXAMPLES Below, the present invention will be explained in more detail by describing examples of the present invention, but the present invention is not limited to these examples.

In the following examples, all percentages are percentages by weight.

Example 1 <Raw materials> Bacillus with the microorganism deposit number No. 1138
Calcium chloride and Glauber's salt were added to an aqueous solution of alkaline cellulase cultured from a bacterium belonging to the genus Bacillus, and dried in a co-current spray dryer to obtain an average particle size of 5.
0- powder was used. The amounts of calcium chloride and Glauber's salt are 0.5% and 48%, respectively, based on the dry product.

Average 11 Average particle size is 610- and 11% of particles are 500- or less.
, 700- or higher particles used 9% sodium chloride.

Binder polyethylene glycol 6000P (NOF side) was used.

Composition: 35% enzyme powder, 45% nuclear material, 15% binder, 5% titanium oxide.

<Pelletization operation> High speed mixer (Fukae Kogyo ■, FS-10 type)
All of the above raw materials (total 6 kg) were added to the tank, and while 85°C hot water was flowing through the jacket, the stirring blade tip speed was set to 5 m/min.
Mix and stir for seconds. When the temperature of the contents rose to 65°C, the mixer was discharged and immediately transferred to a fluidized bed to cool to 30°C.

<Physical properties of granulated product> The average particle diameter of the obtained enzyme granules was 810 -, 3.6% had a particle diameter of 1410 - or more, and 1.8% had a particle diameter of 350 ttm or less. This shows that the present invention can easily produce granules with a very narrow particle size distribution.

The enzyme activity of the enzyme powder as a raw material and the granulated product was measured by the dinitrosalicylic acid method, and the activity retention rate during the granulation process was determined to be 100%, that is, there was no deactivation at all.

Example 2 <Raw materials> and formulation> are the same as in Example 1.

<Pelletization operation> Henschel mixer <= Imiike Kakoki■, FM-208
Pour all of the above raw materials (8 kg in total) into a mold), and while running 85°C hot water through the jacket, set the stirring blade tip speed to 13.
The mixture was mixed and stirred at m/sec. When the temperature of the contents rose to 67°C, the mixer was discharged and immediately transferred to a fluidized bed for 30
Cooled to ℃.

<Physical properties of granulated product> The average particle diameter of the obtained enzyme granules was 750 J! m, 1
The amount of particles with a particle size of 410 or more was 2.0%, and the amount of particles with a particle size of 360 or less was 3.4%. This example also shows that the present invention produces less fine powder and coarse particles.

In this example as well, the activity retention rate during the granulation process was found to be 100%, confirming that the conditions for the enzyme were satisfactory.

Example 3 <material> The same enzyme powder and binder as in Example 1 were used.

Removal force 1 The average particle diameter is 250-, and 23% of particles are 125- or less.
, Glauber's salt containing 8% particles of 350μ or more was used.

<Composition> Enzyme powder 35%, nuclear material 42%, binder 18%, titanium oxide 5%.

<Pelletization operation> Granulation was carried out using the same equipment and conditions as in Example 1, and the enzyme granules were obtained by cooling.

<Physical properties of granulated product> The average particle diameter of the obtained enzyme granules was 340 mm and 710 mm.
7.4% of the particles had a particle size of tm or more, and 0.9% had a particle size of 177 or less.

This example also shows that according to the present invention, granules with a very narrow particle size distribution can be easily obtained.

When the activity retention rate in the granulation process was determined, it was 100% in this example as well.

Comparative Example 1 <Raw Materials> The same enzyme powder as in Example 1 was used, and the binder was polyethylene glycol #4000 (NOF ■).

<Distribution> Enzyme powder 30%, binder 65%, titanium oxide 5%.

<Pelletization operation> A total of 20 kg of the raw materials were melted and mixed at 85° C. and sprayed and cooled at a pressure of 50 kg/cm 2 from a pressure nozzle with a diameter of 1.61 to obtain spherical enzyme granules. This is the first sample.

Fine powder of 125 or less obtained by classifying this granule 2.5k
g was melted again and spray-cooled in the same manner as the first time. This is the second sample.

<Physical properties of granulated product> The average particle size of the first sample was 220-, 0.3% for particles with a particle size of 500- or more, and 14.
It was 7%.

In the above example, the fraction of particles with a particle diameter of about one-half or less of the average particle diameter of the granules was 5% or less, whereas in this comparative example, this amount was as high as 14.7%. , the particle size distribution is wide;
It is clear that it is inevitable that the burden on the equipment for classification and collection operations will be greater than in the present invention.

When the activity retention rate in the granulation process was determined, it was clear that the first sample was inferior to the present invention in this aspect as well.

Comparative Example 2 <Raw Materials> The same enzyme powder as in Example 1 was used, and the binder was carboxymethylcellulose with a degree of etherification of 0.7 and a purity of 95%. In addition, mirabilite was used.

<Composition> Enzyme powder 35%, binder 0.5%, titanium oxide 5%
, mirabilite 59.5%.

<Pelletization operation> The raw materials except the binder are mixed, and a 4% aqueous solution of the binder is added and mixed. The total weight is 3 kg. This is extruded using a granulator (Fuji Powder A, EXD OS-100
) and then shaped into a cylinder with a diameter of 0.9 mm, further shaped using a Marmerizer (Fuji Powderoo, QJ-400), and then dried in a fluidized bed with warm air at 85°C until the moisture content is 3% or less. did.

Physical properties of the granulated product> The average particle diameter of the obtained enzyme granules was 920-1,410
- 0.8% of the particles had a particle size of - or more, and 2.7% of the particles had a particle size of 500 1M or less. In this example, granules with a very narrow particle size distribution equivalent to or better than that of the present invention can be obtained.

However, when the activity retention rate in the granulation process was determined, it was 97%. This is thought to be caused by the heat during drying.

Claims (1)

[Claims] 1. Detergent enzyme powder is made of water-soluble particles with an average particle diameter in the range of 0.2 mm to 1.2 mm as a core substance,
Using a water-soluble organic binder with a melting point or softening point of 35°C to 70°C, the granules are granulated using a stirring rotary granulator so that the average particle size of the granules is 1 to 2 times the average particle size of the core material. A method for producing enzyme granules for detergents, characterized by granulation. 2. The manufacturing method according to claim 1, wherein the detergent enzyme is one or a mixture selected from protease, esterase, and carbohydrase. 3. The nuclear material is sodium chloride, potassium chloride, mirabilite,
The manufacturing method according to claim 1 or 2, wherein the material is one selected from soda carbonate and sugar or a mixture thereof. 4. The manufacturing method according to any one of claims 1 to 3, wherein the organic binder is one selected from polyethylene glycol, a nonionic surfactant, or a mixture thereof.