JPS62269684A - Production of enzymic granule - Google Patents

Abstract

PURPOSE:To obtains an enzymic granule with improved granulating property and yield, by blending enzymic flour or an aqueous solution containing an enzyme with specific amounts of fine fibers and a lubricant and, as desired, another additive, granulating the resultant blend in a granulator and drying the resultant granule. CONSTITUTION:1-70wt% one or two or more of enzymic flours or aqueous solutions thereof of alkali protease, alkali esterase, alkali carboxylase and alkali nuclease derived from microorganisms, 0.5-30wt% fine fibers having preferably 100-500mu average fiber length and 0.05-0.7 denier fiber diameter, preferably 5wt%- balance of talc and, as necessary, extender, filler, binder, granulating agent, colorant, stabilizer, reinforcing agent, etc., are preferably charged into a mixing and stirring granulator or drum granulator, granulated at 10-50 deg.C temperature and dried in a fluidized bed dryer to afford the aimed enzymic formulation having normally 0.1-2mm diameter.

Description

[Detailed Description of the Invention] 3. Detailed Description of the Invention [Field of Industrial Application] The present invention relates to a method for producing enzyme granules, and more specifically, to a method for producing enzyme granules with improved granulation properties and yield. .

[Prior art] Enzyme granulated products, unlike powders, have good fluidity and
It has great advantages such as being easy to clean, does not stick to the vessel wall, does not form agglomerates, and is stable.In recent years, it has rapidly become popular in various industries such as food, pharmaceuticals, detergents, leather, textiles, and seafood processing. It is being done.

In particular, enzymes containing proteolytic enzymes, lipolytic enzymes, starch-degrading enzymes, etc. with catalytic activity that alter or denature dirt and stains derived from biological proteins (dirt, blood, etc.) and make them easier to remove. Detergents containing enzymes have been in the spotlight, and various products have been developed, accounting for about 30% of the industrial enzyme market.

[Problems to be Solved by the Invention] Enzyme granules such as enzyme granules for detergents are desired to have good disintegration properties in liquid and to have high strength when normally handled.

However, it is a very difficult problem to produce granulated products that have sufficient strength and at the same time exhibit sufficient solubility as enzyme granules. Manufactured.

For this reason, when manufacturing granules, the issue is how to efficiently produce particles having a desired particle size.

Conventional enzyme granules are manufactured by granulating enzyme-containing powders with water using a granulator with or without a binder, but enzymes generally exhibit strong stickiness during granulation. .

In particular, in the case of enzymes with low specific activity, when attempting to maintain the intended enzyme activity in the final product, the enzyme content may reach 15% or more or even 20% or more, resulting in a significant decrease in granulation properties due to stickiness. Powder for granulation adheres and accumulates on the inner wall of the granulator, resulting in unsanitary conditions and often causing operational problems. Even if attempts are made to maintain granulation properties by adjusting the amount of water and filler used in this case, the scope of application is narrow and the granules often grow too quickly, making it difficult to control the particle size. , leading to poor yield and the finish condition (roundness, luster, shape of particles, etc.)
It was also defective. Furthermore, particles with inaccurate particle sizes or particles that adhere to the inner wall of the granulator are crushed and recycled to the granulation process, but there is also the problem that enzymes are deactivated during crushing.

[Means for Solving the Problems] The present inventors have discovered that the various problems described above can be solved by using a lubricant during granulation of enzyme granules, and have completed the present invention.

That is, the present invention provides enzyme powder or enzyme-containing aqueous solution 1 to
10% by weight, fine fibers 1o, s~30% by weight, lubricant 5~
The present invention provides a method for producing enzyme granules in which the balance weight % and other additives are granulated using a granulator, and then dried and powdered.

Hereinafter, the raw material compounding components used in the present invention will be explained.

(1) Enzymes are enzymes of animal, plant, or microbial origin that are generally used in detergents, and specific examples include the following.

Proteases: pepsin, trypsin, chymotrypsin, cathepsin,
subtilcin, collagenase, keratinase, elastase, papain, promeline, pancreatin, carboxypeptidase, aminopeptidase, dipeptidyl carboxypeptidase esterase: lipase (gastric lipase, pancreatic lipase, plant lipase, phospholipase), cholinesterase, phosphatase; Rabi: amylase, maltase, saccharase, cellulase,
Lysotium, pectinase, glucosytase; Nuclease: ribonuclease, deoxyribonuclease.

Among these enzymes, alkaline protease, alkaline esterase, and alkaline carboxylase calinuclease, which are active in the alkaline region of detergent aqueous solutions, are used, but enzymes of microbial origin are particularly preferably used because they have a wide range of temperatures. .

The enzymes mentioned above may be used in a dry state or in the form of an aqueous solution, singly, or in combination of two or more.

(2) Fine fibers are added to maintain appropriate strength and disintegrability of enzyme granules, and are fine fibers such as natural fibers such as cellulose, nylon, polyethylene, polypropylene, vinylon, polyester, or acrylic.
Average fiber length 100-500μ, fiber diameter 0.05-0.7
Denier ones are preferably used. Especially from 0.35
O, SO denier vinylon fibers can be cut to any desired fiber length up to a minimum of 0.3 m using a dry cutting method, imparting desirable properties to the granules.
5# vinylon staple fibers are preferably used.

(3) A lubricant is an essential ingredient for improving the granulation properties of enzyme granules with strong adhesive properties. Lubricants include talc, magnesium salts of silicic acid, aluminum salts, calcium salts, Powders such as zirconium salts, anhydrous silicates, sterotex, magnesium oxide, wax stones including kaolin, calcium, magnesium, potassium or sodium stearate or polyethylene glycol 6.000 are used. Among these, talc can be particularly preferably used in view of the finished state of the granulated product, product yield, balance of physical properties such as residual rate of enzyme activity, and cost.

(4) Other additives that may be used as desired include:
For example, there are bulking agents or fillers used as diluents to keep the specific activity of enzyme granules constant, sodium sulfate, f
Calcium tate, aluminum sulfate, potassium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate,
Calcium phosphate and the like can be used alone or in combination. These have an average particle size of 100μ, preferably 20μ
The following are preferably used.

In addition, adhesive hydrophilic substances used for granulation as binders, such as polyvinyl pyrrolidone, polyvinyl alcohol, and cellulose derivatives, such as hydroxypropylcellulose and methylcellulose, are generally added to the system as an aqueous solution. However, in some cases, only water may be used without a binder.

Further, as a granulating agent, water or a waxy substance having a melting point of 30 to 70'C can be used by melting or dissolving or dispersing it in water. As the granulating agent, for example, polyethylene glycol, ethoxylated aliphatic alcohol, polyethylene glycol monooleate, fatty acid monoethanolamide, etc. are used. Granulating agents are useful for forming granules, and each can also be used alone.

Other colorants (titanium oxide and other coloring pigments), stabilizers, and reinforcing materials that are known in the field of granulation or enzyme preparations can be used.

[Manufacturing method] The method for manufacturing enzyme granules of the present invention includes, as a granulation composition,
Enzyme powder or enzyme aqueous solution described above 1-70% by weight, fine fibers 0, 5-30% by weight, lubricant 5-balance % by weight
And, if desired, an extender or filler, a binder, a granulating agent, a coloring agent, a stabilizer, a reinforcing agent, etc. are placed in a granulator and granulated.

Any type of granulator can be used, and a mixing granulator, a drum granulator, etc. are preferably used. Granulation is 10
Performed at a temperature of ~50°C, enzymes, fibers, lubricants and optionally other additives are first charged to a granulator, which is then supplemented with water and/or as a liquid binder and/or granulating agent. Alternatively, granulation is generally performed by supplying a wax-like substance into the system through a nozzle, but the loading method can be carried out in any order. Further, after drying, powdering with wax and a coloring agent makes it possible to obtain granules with a desired consistency.

After granulation, the obtained granules are dried, for example, in a fluidized bed dryer. Dry granules usually have a diameter of 0.1 to 2#.

[Effects of the Invention] According to the method of the present invention, even when granulating an enzyme bulk powder with relatively low activity, the granulation performance and yield are significantly improved. It is possible to perform suitable granulation without adhesion or accumulation on the surface, and to obtain spherical granules with a smooth surface.
), and the effect increases with the amount added, and even if multiple particles are used, there is no co-location, so the workability and economic efficiency of granule manufacturing is improved, the shape retention of granules, It has excellent abrasion resistance, can suppress the generation of dust and crushed particles to extremely low levels, and has excellent disintegration properties in water, and because off-spec products during manufacturing can be recycled to the granulation process. It has many desirable features for industrial production of enzyme granules, such as reduced enzyme deactivation during pulverization.

[Example] The present invention will be explained below with reference to Examples and Comparative Examples.

Example 1 API-21 powder (alkaline protease produced from Bacillus NKS-21: JP-A-53-1349)
90) 530g, talc 1.330g, 0.
35 denier, O, SS length vinylon tip 80g,
Titanium oxide 609 was loaded into the Nara Machine Manufacturing Granulator LHA-10, the mixing blade was set at 20 rpm, and the chopper rotor was set at 3.0 rpm. The charges were mixed by spinning at ooorpm for 5 minutes.

Next, while the mixing blade and rotor blade were still rotating at the above rotational speed, 30% of polyethylene glycol 4.000 was added to it.
% aqueous solution U from an air-operated nozzle. After spraying, the rotation speed of the mixing blade was increased to 350 ppm (the rotation speed of the chopper remains unchanged, the same applies hereafter) for 7 minutes, and the rotation speed of the mixing blade was increased to 45 Orpm for 8 minutes. 550pp
The rotational speed of the mixing blades was increased one after another for 3 minutes at m for 3 minutes and for 1 minute at aoorpm, and mixing was continued until the temperature inside the granulator reached the temperature at which granulation was possible. Enzyme granules were obtained.

The obtained granules were dried in a fluidized bed dryer to a moisture content of 3% or less.

The particle size distribution was as follows.

Particle size distribution>1.2 shoes 13.0% 0.35~1.2M 83.6%<0.35
#3.4% Comparative Example 1 Granules were granulated under conditions relatively similar to those of Example 1 without using a lubricant (talc), but the resulting granules had large surface irregularities and a small particle size. The irregularities were noticeable.

Namely, crushed sodium sulfate l, aaog, powdered enzyme (API-21) 380g, vinylon chips 8
0shi and titanium oxide 609 in Nara machine manufacturing granulator (L)
IA-10 type) and its mixing blade was 200rl)m
After mixing for 5 minutes using the chopper rotor at 3.00 rpm, polyethylene glycol 4.0
230 g of a 30% aqueous solution of 00 was supplied by spraying, and after the spraying was completed, the rotation speed of the mixing blade was increased to 350 rpm, and mixing was continued for 6 minutes.The rotation speed of the mixing blade was increased to 45 Orpm, and mixing was continued for 12 minutes.

The obtained granules had a relatively large number of fine particles, with noticeable irregularities in particle size such as lumpy, potato-like, and ellipsoidal shapes, and were dried to a moisture content of 3% or less using a fluidized bed dryer. After drying, the particle size distribution after drying was determined, and the following results were obtained.

Lari Koketsu〉1.2yo 19.0%0.35~
1.2. 53.8%<0.35mm
27.2% Example 2 Ground Sodium Sulfate 7709, Powdered Enzyme (API-
21> 390g, fiber diameter 0.5 denier, fiber length 0
．． Using 80 g of #5 vinylon chips, 60 g of titanium oxide, and 700 g of magnesium silicate as a lubricant, the charge was placed in a granulator (L made by Nara Tonoki Co., Ltd.) as in Example 1 and Comparative Example 1.
MA-10) and mixed (5 minutes, mixer blades at 35 Or
pm, chopper rotor 3. OOOrpm). Next, with the rotational speed of the mixing blade and rotor blade unchanged, water 3
05g was sprayed from an air-operated nozzle, and after the spraying was completed, the rotational speed of the mixing blade was increased to 45% for 2 minutes at the same rotational speed.
The mixture was mixed at 0 rpm for 5 minutes (the rotor speed remained the same) and then dried to obtain a finished product. The 1q enzyme granules were spherical to elliptical in shape, had a glossy surface, and were grayish white in color, and were generally of good quality.The particle size distribution was measured and the following results were i51.

Particle size distribution>1.2M 14.3%0.35~1.
2# 82.0%<0.35M
3.7% Example 3 Powdered enzyme 380g, crushed sodium sulfate 8809,
Talc 6009, vinylon chips 80g, titanium oxide 6
09 was loaded into a granulator and granulated in the same manner as in Example 2 (however, the granulating agent was 330 g of water). As a result, a product comparable to Example 2 in terms of finish and yield was obtained.

Comparative Example 3 In order to contrast with Example 2, a product with a composition in which talc was removed and replaced with sodium sulfate was granulated in the same manner as in Example 3 (except that the granulating agent was 220 g). The particle size distribution after drying was as follows.

Distribution> 1.2 shoes 32.9% 0.35~1.
2mm 55.6%<0.35 #1I
1111.5% Mackerel fixed decoction μm After granulation and drying, the enzyme granules were sieved using Tyler mesh 48 mesh and 12 mesh sieves to form granules of 0.3~
A particle size of 1.2# was collected.

Each 1g of these granules was mixed into 15 agate balls with a diameter of 14M.
Individual agate pots (ball mill containers, diameter yo [x
70 mm in height), rotated at a rotational speed of 150 ppm for a certain period of time, pulverized, diluted with a diluent, and placed in an analytical instrument (Autoanalyzer).
T) l-IISampler and SIC, Chrom
The enzyme residual activity value was measured using atocorder-11>. The results of measuring enzyme residual activity values for the samples of Example 1 and Comparative Example 2 are shown below.

Claims (1)

[Scope of Claims] 1) Produced by adding 1 to 70% by weight of enzyme powder or enzyme-containing aqueous solution, 0.5 to 30% by weight of fine fibers, 5 to 3% by weight of lubricant, and other additives as desired. A method for producing enzyme granules, which comprises drying the granules after granulating them using a granulator. 2) The manufacturing method according to claim 1, wherein the fine fibers have an average fiber length of 100 μm to 500 μm and a fiber diameter of 0.05 to 0.7 deniers. 3) The production method according to claim 1 or 2, wherein the enzyme is one or a mixture of two or more of protease, amylase, lipase, and cellulase originating from a microorganism. 4) The manufacturing method according to claim 1, 2 or 3, wherein the lubricant is powder of talc, magnesium silicate and/or kaolin. 5) The manufacturing method according to claim 1, wherein after granulation and drying, molten wax treatment is performed. 6) The manufacturing method according to claim 5, wherein the molten wax is polyethylene glycol. 7) The manufacturing method according to claim 5 or 6, wherein the molten wax-coated particles are powdered with a coloring agent. 8) The manufacturing method according to claim 7, wherein the colorant is titanium oxide.