JP3071427B2 - Enzyme particles - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an enzyme particle suitably blended in a detergent. Furthermore, the present invention relates to a method for producing the enzyme particles.

[0002]

2. Description of the Related Art Various enzymes are often blended in detergents such as powder detergents for clothes, powder bleaching agents and powder detergents for automatic dishwashers in order to enhance the detergency. Since the effect is exhibited only when the enzyme is dissolved in water, the enzyme has a property that it takes a certain amount of time to exhibit the effect. Therefore, in order to maximize the performance of the enzyme, it is important that the enzyme particle has a property of rapidly eluting the enzyme from the enzyme particle (referred to as high-speed solubility). In particular, in the current situation where the washing time tends to be shortened with respect to clothing detergents and the like, the importance thereof is increasing more and more.

[0003] Further, in the case of mixing in a detergent, if enzyme particles remain undissolved at the end of washing, a problem such as adhesion of undissolved components to an object to be washed occurs. Therefore, it is important to prevent all the substances constituting the enzyme particles from dispersing within the washing time and from remaining undissolved.

[0004] In order to ensure the safety of the working environment, it is important to reduce the amount of dust generated from the enzyme particles (called the amount of generated dust). Furthermore, when considering after blending with a detergent, it is desirable from the viewpoint of quality that the enzyme particles are uniformly distributed in the detergent. for that purpose,
It is important to make the particle diameter and bulk density of the enzyme particles close to the other particles constituting the cleaning agent to prevent the other particles and the enzyme particles from being classified.

[0005] In view of these points, the properties related to the superiority of the enzyme particles to be added to the detergent include, for example, 1. 1. fast solubility; 2. low dust generation; 3. particle size; For example, there is a demand for an enzyme particle which satisfies the required physical properties for each of them. These properties are closely related to each other. For example, although the solubility is improved by reducing the particle diameter, the amount of dust generated tends to increase at the same time. Increasing the bulk density reduces the amount of dust, but at the same time tends to decrease solubility.
For this reason, it has conventionally been very difficult to obtain enzyme particles that simultaneously satisfy these required physical properties.

For example, in Japanese Patent Publication No. 50-22506, a solution or dispersion in which a detergent enzyme and an inorganic salt coexist in a water-soluble binder solution is spray-dried.
A method for producing microcapsules containing detergent enzymes is disclosed. Particle size 20 to 13 implemented here
Microcapsules in the range of 0 μm are considered to be capable of satisfying good solubility when used in a detergent, but the particle size is very small as compared with the detergent, so classification that occurs between particles is performed. It is difficult to suppress the phenomenon. In addition, since the enzyme particles obtained by this technique have a substantially high content of a water-soluble substance, the strength is weak in a hollow structure, and it is difficult to suppress the amount of dust generation. The required physical properties could not be satisfied at the same time.

[0007] JP-A-7-289259 discloses that a mixture containing a detergent enzyme and an aluminosilicate powder is subjected to stirring tumbling granulation using a water-soluble organic binder to produce a detergent enzyme granulated product. A method for doing so is disclosed. According to this method, with respect to the suppression of the amount of dust generation, the problem is solved by performing granulation. However, it is difficult to satisfy high-speed solubility due to an increase in particle diameter and compaction of particles in granulation, and the above-mentioned required properties of the enzyme cannot be simultaneously satisfied by this method.

[0008]

SUMMARY OF THE INVENTION An object of the present invention is to provide a detergent composition in which, when the enzyme is rapidly eluted, there is no undissolved portion, the generation of dust is suppressed, and when the detergent is blended with other components, It is an object of the present invention to provide an enzyme particle having a property that a classification phenomenon that occurs between particles in an object is unlikely to occur (hereinafter, referred to as non-classification property). It is a further object of the present invention to provide a method for producing the enzyme particles.

[0009]

That is, the present invention provides: (1) (A) a water-insoluble substance and / or a poorly water-soluble substance;
(B) Enzyme particles containing a water-soluble binder and (C) an enzyme, wherein the content of the component (A) is 45% by weight or more, the average particle diameter is 150 to 500 µm, and the bulk density is 500 to 500%. Elution having a structure of 1000 g / L and having the component (B) more near the surface than inside.
Rate of 70% or more, and dissolution of 85% or more of the enzyme particles, [2] (A) water-insoluble substance and / or poorly water-soluble substance,
The method for producing enzyme particles according to [1], wherein the slurry containing (B) a water-soluble binder and (C) the enzyme is spray-dried at a temperature at which the enzyme is not substantially inactivated. It is.

[0010]

BEST MODE FOR CARRYING OUT THE INVENTION About the component (A) The water-insoluble substance and the poorly water-soluble substance of the component (A) used in the present invention are substances that show little or no solubility in water and substantially lose enzymes. It is not particularly limited as long as it is a substance that does not activate, does not react with the water-soluble binder, and has a property of dispersing in water. This substance may be either an inorganic substance or an organic substance, but when used in a production method that requires heating such as spray drying, an inorganic substance is more preferable because higher stability against heat is more advantageous. Specific examples of the water-insoluble substance and the poorly water-soluble substance include cellulose powder, zeolite, talc, clay, alumina, kaolin, titania, calcium carbonate,
Examples thereof include barium sulfate and the like, and zeolite, kaolin, and the like having good dispersibility in water are particularly preferable.

Regarding the size of the water-insoluble substance and the poorly water-soluble substance to be used, the average particle diameter of the primary particles is preferably 20 μm or less from the viewpoint of uniformity of distribution inside the enzyme particles.
Further, the smaller the average particle diameter of the primary particles of the water-insoluble substance and the poorly water-soluble substance, the denser the enzyme particles, and the higher the density, the higher the particle strength and the smaller the average particle diameter of the primary particles. 10 μm or less is more preferable, and 0.1 to 5 μm is particularly preferable.

The content of the component (A) in the enzyme particles is preferably 45% by weight or more of the enzyme particles from the viewpoint of suppressing generation of dust, imparting disintegration and dispersibility to the enzyme particles, and promoting rapid elution of the enzyme. Yes, and 50% by weight from the viewpoint of enhancing high-speed dissolution
The above is preferred. On the other hand, the content is preferably 90% by weight or less of the enzyme particles, from the viewpoint of suppressing dust generation and preventing undissolved residue.
It is more preferably at most 80% by weight, particularly preferably at most 70% by weight. Therefore, considering simultaneously satisfying high-speed solubility and low dusting properties and preventing the undissolved portion, the content is preferably 50 to 90% by weight of the enzyme particles, more preferably 50 to 80% by weight, and more preferably 50 to 70% by weight. % By weight is particularly preferred.

In the present invention, the water-insoluble substance and the poorly water-soluble substance may be used alone or in combination. When two or more water-insoluble substances and poorly water-soluble substances are used in combination, particles having different particle diameters or particles having different shapes are blended to make the structure of the enzyme particles denser or stronger, thereby improving dust generation. It is also possible to suppress. For example, the average particle size of the primary particles is 2 to
When particles having a mean particle diameter of primary particles of 1 μm or less are used in combination with particles of 3 μm, the mean particle diameter of primary particles is 2 μm.
Dust generation can be suppressed as compared with the case where only particles of up to 3 μm are used. As described above, when the particles having different particle diameters are used in combination, the ratio of the small particle diameters is not particularly limited, but from the viewpoint of the dust generation suppressing effect, 5 to 60% by weight of the water-insoluble substance and the poorly water-soluble substance is 5% by weight. Preferably, 5 to 50% by weight is more preferable.

2. About the component (B) The water-soluble binder of the component (B) used in the present invention has the ability to bind the components constituting the particles, dissolves rapidly in water without substantially inactivating the enzyme. There is no particular limitation as long as it has properties. For example, polyethylene glycol and its derivatives, polyvinyl alcohol and its derivatives, water-soluble cellulose derivatives, carboxylic acid-based polymers, starch, saccharides and the like (derivatives include ether compounds and the like). From the viewpoint of productivity and high-speed solubility, carboxylic acid polymers and saccharides are preferable, and salts of acrylic acid-maleic acid copolymers and polyacrylates are more preferable.
As the salt, a sodium salt, a potassium salt, and an ammonium salt are preferable.

[0015] The content of the water-soluble binder in the enzyme particles is preferably 5% by weight or more, more preferably 15% by weight or more of the enzyme particles from the viewpoint of low dust generation. From the viewpoint of fast solubility, the content is preferably 40% by weight or less, more preferably 30% by weight or less of the enzyme particles. Therefore, the content is 5 to 40% by weight of the enzyme particles from the viewpoint of low dusting property and high solubility.
Is preferable, and 15 to 30% by weight is more preferable.

The water-soluble binder used in the present invention may be used in combination of two or more, if necessary. By combining two or more types of water-soluble binders having different effects, the combined effect can be expected.
For example, the stability of enzyme particles can be further imparted by further combining a binder that can be rapidly dissolved in water with a binder having an enzyme stabilizing ability.

3. Regarding the component (C) The enzyme of the component (C) used in the present invention is not particularly limited as long as it is an enzyme that exhibits a cleaning effect or the like when incorporated into a detergent. For example, one or more selected from cellulase, protease, peptinase, amylase, lipase, and dextranase are preferably used.

The content of the enzyme in the enzyme particles is preferably 0.5% by weight or more, more preferably 2% by weight, from the viewpoint of expressing the enzyme activity. From the viewpoint of high-speed solubility, the content is preferably 30% by weight or less, more preferably 25% by weight or less. Therefore, the content is preferably from 0.5 to 30% by weight, more preferably from 2 to 25% by weight, from the viewpoints of enzyme activity expression and rapid solubility.

The enzyme may be used in the form of a concentrated solution obtained by filtering and concentrating a culture containing the enzyme produced by a microorganism, or an enzyme powder obtained by drying the concentrated solution. May be used. When an enzyme concentrate is used, it may contain saccharides, inorganic salts, and the like that cannot be completely separated by filtration.

4. (D) Component The dye of the (D) component used in the present invention is not particularly limited as long as it has high solubility. When used in a production method that requires heating such as spray drying, it is preferable that the heat stability be high. Specifically, red 106
No. 2, Red No. 227, Blue No. 1, Blue No. 2, Green No. 3, Yellow No. 203 and the like. For the content of these dyes,
0.001% by weight or more of the enzyme particles is preferable from the viewpoint of coloring property, and 1.0% by weight of the enzyme particles is preferable from the viewpoint of dispersibility of the dye.
% By weight or less is preferred. And more preferably, it is 0.01 to 0.5% by weight of the enzyme particles. In the present invention, two or more dyes may be used as a mixture. The hue can be easily adjusted by mixing two or more dyes.

5. Other water-soluble substances The enzyme particles of the present invention may contain other water-soluble substances as required, in addition to the above-mentioned water-insoluble substances, poorly water-soluble substances, water-soluble binders, and enzymes. . For example, sodium chloride, calcium chloride, magnesium chloride, sodium sulfate and the like can be blended as a stabilizer and an excipient. The amount of other water-soluble substances is determined by adding the total amount of the enzyme, the water-soluble binder, and the
A range that does not exceed weight% is preferred. In particular, the content of the other water-soluble substance is preferably 15% by weight or less, more preferably 10% by weight or less of the enzyme particles from the viewpoint of high-speed solubility and low dust generation.

Preferred combinations of a water-insoluble substance and / or a poorly water-soluble substance, a water-soluble binder and other water-soluble substances include, for example, zeolite as a water-insoluble substance and / or a water-insoluble substance, and sodium polyacrylate as a water-soluble binder. And saccharides, and other water-soluble substances such as Glauber's salt as an excipient.

6. Regarding the enzyme particles of the present invention, the average particle size of the enzyme particles of the present invention is 150 to 500 μm, and in order to suitably satisfy high-speed dissolution, low dust generation, and non-classification, the average particle size is 200 to 500 μm. 400 μm is preferred. For example, the enzyme particles after production may be adjusted to an average particle size by sieving.

In addition, from the viewpoints of dust generation and solubility, enzyme particles having particles of 125 to 710 μm occupying 80% by weight or more of the whole are preferable, and enzyme particles occupying 90% by weight or more are more preferable. Further, from the viewpoint of non-classification, it is preferable that the particle size distribution is as uniform as possible. In addition, the bulk density of the enzyme particles is 5 from the viewpoint of non-classification.
It is preferably at least 100 to 1000 g / L. The moisture value of the enzyme particles in the present invention is 10% by weight from the viewpoint of quality.
Or less, more preferably 5% by weight or less.

The enzyme particles of the present invention have a structure in which the water-soluble binder of the component (B) is present more near the surface than inside the particles. Because such a water-soluble binder is unevenly distributed in the vicinity of the surface, the water-soluble binder is first dissolved in water, and then the water comes into contact with the water-insoluble substance and the poorly water-soluble substance.
The particles themselves disintegrate and disperse in water. Therefore, the enzyme is eluted into water promptly. Therefore, if the enzyme particles have this structure, the enzyme can be eluted quickly even if the particle diameter or the bulk density increases, and there is no undissolved residue. In addition, in the vicinity of the surface of the enzyme particles, since the amount of the binder for binding the components constituting the particles is large, the particle strength is further improved, and low dust generation can be realized.

The uneven distribution of the water-soluble binder can be confirmed by the following method. First, the enzyme particles to be measured,
The enzyme particles are sufficiently pulverized in an agate mortar or the like to prepare a homogenized pulverized enzyme particle. Then, under the condition that information up to about 10 μm can be obtained from the surface of the enzyme particle, a method using both Fourier transform infrared spectroscopy (FT-IR) and photoacoustic spectroscopy (PAS) (“FT-IR / PAS ”). When the amount of the former water-soluble binder is larger than the amount of the latter water-soluble binder, the enzyme particles to be measured have a structure in which a larger amount of the water-soluble binder is present near the surface than inside the enzyme particles.

The measurement conditions for obtaining information up to about 10 μm from the surface of the enzyme particles include, for example, a resolution of 8 c
m ^-1 , scanning speed 0.63 cm / s, totaling 128 times,
Condition. Apparatus to be used, for example, as infrared spectrophotometer Bio-Rad Laboratories FTS-60A /
The 896 infrared spectrophotometer was used as a PAS cell by MTEC 300
Type photoacoustic detector. FT-IR / PAS is APPL
IED SPECTROSCOPY vol.471311-1316 (1993).

As described above, the enzyme particles of the present invention are useful because the enzyme is rapidly eluted, has no remaining undissolved, suppresses the generation of dust, and is non-classifying.

The enzyme particles of the present invention are preferably colored with a dye from the viewpoint of improving appearance. Enzyme particles obtained by spray-drying a slurry containing a dye have a structure in which more dye is present near the surface than inside the enzyme particle. Enzyme particles having this structure are more vibrant than those having a structure in which the dye is almost uniformly dispersed throughout the particles, and this structure can be confirmed by cleaving the enzyme particles and observing the cross section thereof. Can be.

7. Regarding the production method of the present invention In the production method of the enzyme particles of the present invention, a slurry containing, for example, a water-insoluble substance and / or a poorly water-soluble substance, a water-soluble binder and an enzyme is dried in order to prevent a decrease in solubility due to the compaction of the enzyme particles. The manufacturing method is preferable. Further, in order to obtain particles having a structure in which a large amount of a water-soluble binder is present near the surface than inside the enzyme particles, for example, after drying the slurry to produce particles, the surface of the particles is coated with a water-soluble binder. A method of coating, a method of spray-drying the slurry, and the like are included. In particular, at the time of heating and drying, a large amount of water-soluble binder collects in the vicinity of the surface with the movement of water. Therefore, a spray drying method that can easily obtain particles having the above structure is preferable.

When producing the enzyme particles of the present invention by the spray drying method, first, a slurry containing each component is prepared. The content of each component of the obtained enzyme particles is a value corresponding to the content of each component in the solid content of the slurry. As used herein, “solid content” refers to a water-insoluble substance, a poorly water-soluble substance, a water-soluble binder, an enzyme, and other water-soluble substances. In addition, water is usually used as a dispersion medium for preparing a slurry.

It is preferable to increase the solid content of the slurry for spray drying because the dusting property of the obtained enzyme particles can be reduced. Considering compatibility between high-speed solubility and low dust generation, the solid content of the slurry is preferably 40% by weight or more, more preferably 50% by weight or more. Also,
From the viewpoint of ease of slurry spraying, the solid content is preferably 60% by weight or less. Therefore, the solid content of the slurry is preferably 40 to 60% by weight, and 50 to 60% by weight.
Is more preferred.

When preparing the spray-dried slurry, the mixing order of the water-insoluble substance and / or poorly water-soluble substance, the water-soluble binder, and the enzyme is not particularly limited. Since they exist and the order depends on the physical properties of the formulation, optimization can be performed as appropriate. For example, when zeolite is used as a water-insoluble substance and / or a poorly water-soluble substance, sodium polyacrylate and saccharides are used as a water-soluble binder, and sodium sulfate is used as an excipient, enzymes, sodium sulfate, saccharides, zeolite, and sodium polyacrylate are used in this order. It is preferable to mix them.

The prepared slurry is supplied to a spray dryer. The temperature of the slurry at the time of supply is preferably a temperature at which the enzyme is not substantially deactivated. From the viewpoint of enzyme stability and ease of slurry production, the temperature is preferably from 10 to 40C, more preferably from 20 to 30C.

The air blowing temperature during spray drying is 120 to 220 ° C.
Is preferable, and 140 to 180 ° C. is more preferable. Performing spray drying in this temperature range improves the productivity,
This is preferable because the enzyme is not substantially inactivated.

Further, for the purpose of reducing the amount of dust generated from the enzyme particles obtained by spray drying and improving the storage stability, a coating agent comprising a component which does not impair the solubility of the particles is used on the surface of the particles. May be covered. Examples of the coating agent include a water-soluble thermoplastic substance, specifically, polyethylene glycol and its derivatives, fatty acids, and the like (the derivatives include ether compounds). Particularly, polyethylene glycol and its derivatives are preferable, and those having a molecular weight of about 2,000 to 10,000 are more preferable. As a specific coating operation, for example, there is an embodiment in which these coating agents are thermally melted and adhered to the surface of the spray-dried particles.

The enzyme particles of the present invention may be colored. The method of coloring the enzyme particles is not particularly limited,
It is preferable to use a dye rather than a pigment from the viewpoint of suppressing color transfer to components and particles other than the enzyme particles and suppressing dyeing to clothing and the like. As a coloring method with a dye, for example, a method of coating the enzyme particles with a coating material in which the dye is dispersed to obtain colored enzyme particles, while performing fluid drying on the enzyme particles,
Spraying and coating an aqueous solution in which a dye and a coating agent are dispersed,
A method for obtaining colored enzyme particles, (A) a water-insoluble substance and / or a poorly water-soluble substance, (B) a water-soluble binder,
A method of drying a slurry containing (C) an enzyme and (D) a dye to obtain colored enzyme particles, and the like.
A method of drying the slurry to obtain colored enzyme particles is preferred. In this method, the dye is mixed into the slurry,
The dye can be easily and uniformly dispersed in the slurry, and as a result, particles having high coloring properties of the dye can be obtained. Particularly preferred is a method of spray-drying the slurry containing the dye at a temperature at which the enzyme is not substantially deactivated, thereby obtaining colored enzyme particles. As a result, the obtained particles have a structure in which a large amount of a water-soluble binder or dye exists near the surface. Therefore, color transfer to components and particles other than the enzyme particles is suppressed by this method, and enzyme particles having better coloring properties can be obtained.

[0038]

EXAMPLES The high-speed solubility, low dust generation, average particle size, bulk density, non-classification, and dyeing properties of the present invention are measured by the following methods. [Fast solubility] In the present invention, the enzyme particles having fast solubility have an elution rate of 70% or more and a dissolution rate of 85%.
The above enzyme particles are referred to. The dissolution rate corresponds to the time required for the enzyme to elute from the enzyme particles and exhibit its performance, and the dissolution rate corresponds to the degree of prevention of undissolved residue. Enzyme particles satisfying high-speed solubility are extremely preferable because not only the enzyme acts quickly, but also there is no undissolved residue.

The elution rate of the enzyme was determined as follows. 100 mg of enzyme particles in a 100 mL beaker (105 m inner diameter)
m), put 100 mL of water having a temperature of 20 ° C. and a hardness of 4 ° DH and add a magnetic stirrer (length 35 mm, diameter 8 m)
m) (200 rpm) to obtain an enzyme solution. With respect to this enzyme solution, the value calculated by the formula (1) was defined as the enzyme elution rate. Elution rate (%) = [A × 100] / B (1) A: Enzyme activity value of enzyme solution obtained by stirring for 30 seconds under the above stirring conditions B: Enzyme of enzyme solution under the above stirring conditions Enzyme activity value when it becomes steady when the activity value is measured over time Note that the enzyme activity value may be measured by a method suitable for each enzyme.

For example, in the case of cellulase, the following CM
A C activity measurement method can be used. 0.4 mL of 2.5% by weight carboxymethylcellulose (CMC) aqueous solution,
To a substrate solution consisting of 0.2 mL of 0.5 M glycine buffer (pH 9.0) and 0.3 mL of deionized water, 0.1 mL of the enzyme solution was added and mixed, and the mixture was incubated at 40 ° C. for 20 minutes. . Next, the reducing sugar was quantified using the following 3,5-dinitrosalicylic acid (DNS) method. That is, 1 mL of the DNS reagent was added to 1 mL of the mixed solution after the incubation, and the mixture was heated at 100 ° C. for 5 minutes. Then, after cooling, 4 mL of deionized water was added to the mixture to dilute it. The reducing sugar was quantified by measuring the absorbance at 535 nm. When measured under these conditions,
The amount of the enzyme that releases 1 μmol of reducing sugar in terms of glucose in one minute was defined as one unit.

In the case of a protease, the following casein method can be used. 50 mM boric acid-sodium hydroxide buffer solution containing 1% by weight of casein (pH 10.
0) 1 mL was mixed with 0.1 mL of enzyme solution and incubated at 40 ° C for 10 minutes. Next, a reaction stop solution (0.123 M trichloroacetic acid-0.246 M) was added to this mixture.
Sodium acetate-0.369M acetic acid) 2 mL,
Incubated at 30 ° C. for 20 minutes. Next, this solution was filtered using filter paper (manufactured by Whatman, No. 2).
Proteolytic products in the filtrate were measured by the modified Farlin-Lowry method. When measured under these conditions,
The amount of enzyme that releases 1 mmol of tyrosine per minute is 1
Unit.

The dissolution rate of the enzyme particles was determined as follows. 1 L of water having a temperature of 5 ° C. and a hardness of 4 ° DH is placed in a 1 L beaker (inside diameter: 105 mm), and 1 g of enzyme particles are put therein, and a magnetic stirrer (length: 35 mm, diameter: 8 mm) (800)
r. p. m. ) For 60 seconds. With respect to the obtained aqueous solution, the value calculated by the formula (2) was defined as the dissolution rate of the enzyme particles. Dissolution rate (%) = {1− (D / C)} × 100 (2) C: input weight of enzyme particles (g) D: aqueous solution obtained under the above stirring conditions is JIS Z 8
After passing through a standard 801 standard sieve (opening of 74 μm), the dry weight (g) of the enzyme particles remaining on the sieve (drying condition: held at a temperature of 105 ° C. for 1 hour, and then placed in a desiccator containing silica gel ( (25 ° C.) for 30 minutes.)

[Low dusting property] The low dusting property in the present invention means that the amount of dusting is 1000 mg or less. This dust generation amount is desirably a low value, more preferably 500 mg or less, and still more preferably 100 mg or less. In addition, the reference value of the amount of generated dust varies depending on the type of the enzyme. For example, the amount of dust generated by proteases and the like that strongly affect the human body is preferably 100 mg or less, and more preferably 20 mg or less.

Here, the amount of dust means that four crushing balls 1 having a diameter of 2.0 cm and a weight of 32.2 g are built in a cylinder having a diameter of 6.0 cm and having a shape converging upward, and the crushing balls are rotated. Number 44r. p. m. Rotate the air inlet 4
20L / min of dry air from
Then, 20 g of the enzyme particles were put into a rotary dust meter that collects the particles entrained in the airflow by the filter 3 in the upper converging portion, and the amount of dust when the measurement was performed for 20 minutes was defined as the amount of dust. The filter 3 has a diameter of 5.0 cm, a trapped particle diameter of 0.5 μm, and a pressure loss of 0.4 cm at a ventilation speed of 5 cm / s.
2 kPa was used. The rotary dust meter used for the measurement is not particularly limited. As the dust meter, a rotary dust meter having a structure shown in FIG.
For example, a dust meter TYPE. III can be used.

[Average Particle Size] The average particle size was determined from the weight fraction based on the sieve size after vibrating for 5 minutes using a JIS Z 8801 standard sieve. [Bulk density] The bulk density was measured by a method specified by JIS K 3362. [Non-classifying property] 1 g of the colored enzyme particles was blended with 100 g of detergent particles (average particle diameter: 400 µm, bulk density: 750 g / L), and vibration was applied by a mixer. Whether or not classification had occurred was visually determined.

[Dyeing property] 0.1 g of the colored enzyme particles was mixed with detergent particles (average particle diameter 400 μm, bulk density 750 g /
L) Blended with 10 g. Test cloth (25 × 16cm)
Was spread on the bat, and water having a hardness of 20 ° C. and a hardness of 4 ° DH was poured into the bat until the test cloth was soaked. Next, a blend of the enzyme particles and the detergent particles was sprinkled evenly on the test cloth. Another test cloth was placed on the test cloth, and water was gently poured into the test cloth until the entire cloth was soaked. Thereafter, the temperature was kept at 30 ° C. and the mixture was left overnight. After rinsing the test cloth, press drying was performed. The presence or absence of dyeing on the dried test cloth was visually determined. Polyester and cotton were used for the test cloth.

Example 1 A spray-dried slurry having a solid content of 45% by weight was prepared from the raw materials and water shown in Table 1. The spray-dried slurry was sprayed at a spray pressure of 2.5 MPa using a pressurized spray nozzle. Spray-drying was carried out in a countercurrent spray-drying tower (diameter: 3 m, tower height: 10 m) at a blowing rate of 100 m ³ / min, a blowing temperature of 150 ° C., and a slurry spray rate of 200 kg / Hr. Particles having a size of 1410 μm or more were removed from the obtained particles by using a sieve to obtain enzyme particles having a water content of 4.1% by weight.

[0048]

[Table 1]

The cellulase in Table 1 is an alkaline cellulase described in JP-A-6-343461, and the protease is an alkaline protease K-16 described in JP-A-5-25492. Maltrich (MR-25, manufactured by Showa Sangyo Co., Ltd.) was used as the saccharide.

Example 2 A spray-dried slurry having a solid content of 45% by weight was prepared from the raw materials and water shown in Table 1. Spray drying and sieving were performed under the same conditions as in Example 1 to obtain enzyme particles having a water content of 4.5% by weight.

Example 3 A spray-dried slurry having a solid content of 55% by weight was prepared from the raw materials and water shown in Table 1. Spray drying and sieving were performed under the same conditions as in Example 1 to obtain enzyme particles having a moisture value of 3.4% by weight.

Example 4 A spray-dried slurry having a solid content of 50% by weight was prepared from the raw materials and water shown in Table 1. Spray drying was performed under the same conditions as in Example 1. Next, particles having a particle size of 125 μm or less and particles having a particle size of 710 μm or more were removed using a sieve to obtain enzyme particles having a water content of 3.8% by weight.

Example 5 5.0 kg of the enzyme particles obtained in Example 4 was stirred with a stirring tumbling granulator (flowing through a jacket at a temperature of 60 ° C., high speed mixer, model FS-10, manufactured by Fukae Kogyo KK). ), And the spindle speed 240 r. p. m. Crushing blade rotation speed 2700r. p. m. And stirred. 80 with stirring
Polyethylene glycol melted at ℃ (molecular weight 6,000)
250 g were charged as coating. After putting coating agent, 10
After stirring for a minute, the surface of the particles was coated. From the obtained particles, particles having a size of 1410 μm or more were removed by using a sieve to obtain enzyme particles having a water content of 3.1% by weight.

Table 2 shows the elution rate, dissolution rate, average particle size, bulk density, amount of dust generation, and non-classification of the enzyme particles obtained in Examples 1 to 5. These all satisfied the required physical properties, and were enzyme particles excellent in fast dissolution, suppression of dust generation, and non-classification. When these enzyme particles were measured by the above-mentioned FT-IR / PAS, it was confirmed that all the enzyme particles had more water-soluble binder near the surface than inside the enzyme particles. FIG. 2 shows the results of FT-IR / PAS measurement of the enzyme particles obtained in Example 3.

Comparative Example 1 A spray-dried slurry having a solid content of 55% was prepared from the raw materials and water shown in Table 1, and spray-dried and sieved under the same conditions as in Example 1 to obtain a water content of 4.3% by weight. % Enzyme particles were obtained.
Table 2 shows the elution rate, dissolution rate, average particle size, bulk density, dust generation amount, and non-classification of the obtained enzyme particles.

Example 6 In the composition of Example 1, 0.2 part by weight of dye No. 1 of blue was mixed with 100 parts by weight of the solid content in the slurry at the time of preparing the slurry to obtain a slurry. The slurry was spray-dried and sieved under the same conditions as in Example 1 to obtain enzyme particles uniformly colored blue. The elution rate, dissolution rate, average particle size, bulk density, dust generation amount, and non-classification of the obtained enzyme particles were almost the same as those of the enzyme particles in Example 1. No dyeing property was observed in the enzyme particles. When the enzyme particles were blended into the detergent composition and color transfer was examined, no color transfer was observed for the enzyme particles.

[0057]

[Table 2]

[0058]

According to the present invention, high-speed dissolution, suppression of dust generation,
An enzyme particle having an effect such as non-classification is provided.
Further, according to the present invention, when the enzyme particles are colored with a dye, it is possible to provide the enzyme particles in which the dyeing property to the fibers and the color transfer to the detergent particles are suppressed.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of a rotary dust meter used for measuring a dust generation amount in the present invention. The upper diagram of FIG. 1 shows a front view, and the lower diagram shows a cross-sectional view taken along line AA.

FIG. 2 shows the enzyme particles obtained in Example 3.
It is a figure showing the measurement result by FT-IR / PAS.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Crush ball 3 Filter 4 Air inlet 5 Air outlet 6 Rotary shaft

Continuation of the front page (72) Inventor Hiroyuki Yamashita 1334 Minato, Wakayama City Kao Corporation Research Institute (56) References JP-A-10-23888 (JP, A) JP-A-10-204494 (JP, A) 60-37983 (JP, A) JP-A-2-97388 (JP, A) JP-A-4-506229 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) C11D 3 / 386 C11D 3/12 C11D 17/06 C12N 9/98 BIOSIS (DIALOG) WPI (DIALOG)

Claims (7)

(57) [Claims] 1. An enzyme particle comprising (A) a water-insoluble substance and / or a poorly water-soluble substance, (B) a water-soluble binder, and (C) an enzyme, wherein the content of the component (A) is 45% by weight or more, average particle diameter of 150 to 500 µm, bulk density of 500 to 1000 g / L, and having a structure in which the component (B) is present more in the vicinity of the surface than in the inside, and the elution rate is 70% or more. And an enzyme particle having a dissolution rate of 85% or more . 2. The enzyme particles according to claim 1, wherein the content of the component (B) is 5 to 40% by weight. 3. The enzyme particle according to claim 1, which is colored with a dye. 4. The enzyme particle according to claim 3, which has a structure in which more dye is present near the surface than inside. 5. A slurry containing (A) a water-insoluble substance and / or a poorly water-soluble substance, (B) a water-soluble binder, and (C) an enzyme is spray-dried at a temperature at which the enzyme is not substantially inactivated. The method for producing enzyme particles according to claim 1 or 2, wherein enzyme particles are obtained. 6. A temperature at which the enzyme containing (A) a water-insoluble substance and / or a poorly water-soluble substance, (B) a water-soluble binder, (C) an enzyme, and (D) a dye is substantially inactivated. 4. Spray-drying to obtain enzyme particles.
Or the method for producing enzyme particles according to 4. 7. The method according to claim 5, wherein the solid content of the slurry is 40 to 60% by weight.