JP2001003094A - Detergent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a detergent compsn. which comprises a group of enzyme- contg. particles and can be dissolved quickly into a washing water so that the action of the enzyme can be effected to the full, and to provide a detergent compsn. in which classification in the detergent is prevented and dust generation of the enzyme is reduced. SOLUTION: This detergent compsn. comprises a group of high bulk-density detergent particles contg. a surfactant, the group showing a dissolving rate of 50% or more and less than 90% when the group is put into water at 5 deg.C, subjected to agitation for 60 sec and then subjected to sieving using a standard sieve defined by JIS Z 8801 (sieve opening of 74 μm), and a group enzyme-contg. particles which shows a dissolving rate of 85% or more under the same condition.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

FIELD OF THE INVENTION The present invention relates to detergent compositions.

[0002]

2. Description of the Related Art Granular detergents are strongly intended to have a high bulk density and a low use amount for convenience of consumers. As one of means for achieving these, an enzyme-containing detergent composition comprising a detergent particle group and an enzyme-containing particle group has been conventionally known.

[0003] From the viewpoint of washing water pH, weak alkali is advantageous in terms of detergency of sebum stains and the like. However, from the viewpoint of enzyme activity, a low pH side is advantageous. It has been. However, even if the enzyme is used, the enzyme activity is higher on the low pH side, and in such a state, after the detergent particles dissolve and the washing water becomes weakly alkaline, the enzyme action occurs when the enzyme-containing particles dissolve. Could not be fully exploited.

[0004] For example, the enzyme-containing particles described in Japanese Patent Publication No. 50-22506 have a small average particle size and a low bulk density, and have a problem that they are easily classified in a detergent and a large amount of dust. In addition, the enzyme-containing particles described in JP-A-7-289259 reduced the amount of dust generated, but did not have sufficient solubility.

[0005]

SUMMARY OF THE INVENTION An object of the present invention is to provide a detergent composition containing a group of enzyme-containing particles having high solubility in washing water so that the action of the enzyme is maximized. It is. It is another object of the present invention to provide a detergent composition which prevents classification in a detergent and suppresses the amount of enzyme dust.

[0006]

That is, the present invention relates to a group of high bulk density detergent particles containing a surfactant (hereinafter referred to as "detergent particles"). Then, the mixture was stirred for 60 seconds under the following stirring conditions, and then JIS Z 8
When subjected to a standard 801 standard sieve (opening 74 μm),
A detergent particle group in which the solubility of the detergent particle group calculated by the formula (1) is 50% or more and less than 90% has a dissolution rate of 8 under the same conditions.
Detergent composition containing 5% or more of enzyme-containing particles: [Agitating conditions: 1 L of hard water (71.2 mg CaCO 3
₃ g / L, Ca / Mg molar ratio of 7/3), 1 g of the sample is charged, and stirred in a 1 L beaker (inside diameter: 105 mm) with a stirrer (length: 35 mm, diameter: 8 mm), rotation speed: 800 rpm [formula (1) ): Dissolution rate (%) = {1- (T / S)} × 10
0 S: Input weight (g) of the sample, T: Dry weight (g) of the residue of the sample remaining on the sieve when the aqueous solution obtained under the above stirring conditions was supplied to the sieve. ].

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The solubility of a detergent particle group calculated by the following method is from 50% to less than 90%, preferably from 55% to less than 90%, more preferably from 60% to less than 90%.

The above-described test stirring conditions will be described more specifically. 1 L of hard water (Ca / Mg molar ratio 7/3) equivalent to 71.2 mg CaCO ₃ / L cooled to 5 ° C. was poured into a 1 L beaker (a cylindrical type having an inner diameter of 105 mm and a height of 150 mm, for example, a 1 L glass beaker manufactured by Iwaki Glass Co., Ltd.) )
While keeping the water temperature of 5 ° C constant in a water bath,
Stirrer (length 35 mm, diameter 8 mm, eg model: ADVA
Rotation speed (800 rpm) at which the depth of the spiral becomes approximately 1/3 of the water depth with Teflon SA (round type) manufactured by NTEC
m). The detergent particles, which were reduced and weighed so as to be 1.0000 ± 0.0010 g, were introduced and dispersed in water with stirring, and stirring was continued. After 60 seconds from the introduction, the dispersion of the detergent particles in the beaker was washed with JIS Z 8 of known weight.
801 standard sieve with a mesh size of 74 μm (diameter 100 m
m), and the water-containing detergent particles remaining on the sieve are collected together with the sieve into an open container of known weight. The operation time from the start of filtration to the collection of the sieve is 10 ± 2 seconds.
The collected residue of the detergent particles is dried with an electric dryer heated to 105 ° C. for 1 hour, and then cooled in a desiccator (25 ° C.) containing silica gel for 30 minutes. After cooling, the total weight of the dried residue of the detergent particles, the sieve, and the collection container is measured, and the dissolution rate (%) of the detergent particles is calculated by equation (1).

The bulk density of the detergent particles is preferably from 500 to
1200 g / L, more preferably 600 to 1000 g / L
L, particularly preferably 650 to 850 g / L. From the viewpoint of economic efficiency, the bulk density is preferably 500 g / L or more,
1200 g / L or less is preferable from the viewpoint of solubility. The average particle size of the detergent particles is preferably 150 to 80.
0 μm, more preferably 250 to 750 μm, particularly preferably 300 to 700 μm. It is preferably 150 μm or more from the viewpoint of preventing the formation of paste, and 8 μm or more from the viewpoint of solubility.
It is preferably not more than 00 μm. The water value of the detergent particles is preferably 10% by weight or less, more preferably 5% by weight or less from the viewpoint of quality.

From the viewpoint of enhancing the interaction between the detergent particles and the enzyme-containing particles, the dissolution rate of the enzyme-containing particles is 85% or more, preferably 87% or more, more preferably 90% or more, and more preferably 93% or more. Is more preferable, and 95% or more is the most preferable. The dissolution rate of the enzyme-containing particles is determined by the same method as that of the detergent particles.

The bulk density of the enzyme-containing particles is preferably 500 to 1000 g / L, more preferably 600 to 1000 g / L, and particularly preferably 70 to 1,000 g / L from the viewpoint of non-classification.
0 to 950 g / L. The average particle size of the enzyme-containing particle group is preferably 150 to 500 μm, more preferably 150 to 4 from the viewpoints of high-speed solubility, low dust generation, and non-classification.
It is 50 μm, particularly preferably 200 to 400 μm.
In addition, from the viewpoint of dust generation and solubility, 125 to 710 μm
Are preferably 80% by weight or more of the whole, and more preferably 90% by weight or more. The moisture value of the enzyme-containing particles is preferably 10% by weight or less, more preferably 5% by weight or less from the viewpoint of quality.

The total amount of the detergent particles and the enzyme-containing particles in the detergent composition of the present invention is preferably from 50 to 100% by weight, more preferably from 70 to 100% by weight, from the viewpoint of sufficiently exerting the action of the surfactant and the enzyme. 100% by weight is more preferred.
In addition, bleach particles, softener particles, defoamer particles,
You may add a fragrance particle group etc. The blending ratio of the two particle groups is preferably 0.2 to 10 parts by weight of the enzyme-containing particle group with respect to 100 parts by weight of the detergent particle group from the viewpoint of washing ability and economy.
0.2 to 5 parts by weight is more preferred. The composition of the present invention comprises:
Known components to be added to ordinary detergent compositions may be included as optional components.

The composition of the detergent particles according to this embodiment is such that the surfactant is 4 to 50% by weight and the alkaline agent is 8 to 50% by weight.
Is preferred. A composition in which the water-insoluble inorganic substance is 10 to 50% by weight and the water-soluble polymer is 1 to 20% by weight is preferable. More preferably, the amount of the surfactant is 5 to 45% by weight,
Particularly preferred is 10 to 50% by weight.

Such detergent particles are described, for example, in Japanese Patent Application Laid-Open No. 61-69897, the disclosure of which is incorporated herein by reference, as a method for obtaining a high bulk density detergent.
JP-A-61-69899, JP-A-61-6990
0, JP-A-5-209200, DE195
The method described in JP-A-29298 can be used. Methods for obtaining higher bulk density detergents include WO 952, the disclosure of which is incorporated herein by reference.
Reference can be made to the invention described in US Pat.
To further illustrate, the main component excluding a part of the water-insoluble inorganic material is kneaded and mixed using a continuous kneader, and the obtained kneaded material and the remaining water-insoluble inorganic material are put into a pulverizer and pulverized. Can be obtained. Then, the obtained detergent particles are sieved to obtain detergent particles having a predetermined average particle size distribution. In addition, as a continuous kneader, for example, KRC2 type manufactured by Kurimoto Iron Works,
Preferable examples of the pulverizer include DKASO6 manufactured by Hosokawa Micron. As another method, for example, it can be obtained by slurrying a main component excluding a part of a water-insoluble inorganic substance or the like, and granulating the slurry with particles obtained by spray drying and a binder substance. The obtained detergent particles are sieved and, if necessary, crushed to obtain detergent particles having a predetermined average particle size distribution.

From the viewpoint of the flowability and non-caking properties of the detergent particles, the detergent particles of the present embodiment are mixed with a surface coating agent,
Further, surface modification may be performed. As a surface coating agent,
For example, aluminosilicate, calcium silicate, silicon dioxide, bentonite, talc, clay, amorphous silica derivatives, silicate compounds such as crystalline silicate compounds, metal soaps, fine powders such as powdered surfactants, carboxymethyl cellulose, Water-soluble polymers such as polyethylene glycol, sodium polyacrylate, polycarboxylic acid salts such as copolymers of acrylic acid and maleic acid or salts thereof;
Fatty acids and the like.

Next, the components constituting the detergent particles will be described. As the water-insoluble inorganic substance, those having an average primary particle size of 0.1 to 20 μm are preferable. For example, clay such as crystalline or amorphous aluminosilicate, silicon dioxide, hydrated silicate, perlite, bentonite, etc. And the like. Of these, crystalline aluminosilicates are preferred in terms of sequestering ability and oil absorbing ability of a surfactant.

Examples of the water-soluble polymer include a carboxylic acid polymer, carboxymethyl cellulose, soluble starch, and saccharides. Among them, a carboxylic acid-based polymer having a molecular weight of several thousands to 100,000 is preferred from the viewpoint of sequestering ability of metal ions, dispersing ability of solid dirt / particle dirt, and ability of preventing re-contamination. Particularly, a salt of an acrylic acid-maleic acid copolymer and a polyacrylate are preferred. Here, the salt includes a sodium salt, a potassium salt, and an ammonium salt.

Examples of the alkali agent include carbonates, silicates, amines such as alkylamines and alkanolamines.

Examples of the surfactant include anionic surfactants, nonionic surfactants, amphoteric surfactants, and cationic surfactants. Examples of the anionic surfactant include a higher alcohol or a ethoxylated sulfate thereof, an alkylbenzene sulfonate, a paraffin sulfonate, an α-olefin sulfonate, an α-sulfofatty acid salt or an ester salt thereof, and a fatty acid salt. No. In particular, when the carbon number of the alkyl chain is 10 to 18
(Preferably 12 to 14) linear alkyl benzene sulfonate and α-sulfofatty acid alkyl ester salt having 10 to 20 carbon atoms are preferable. Examples of the counter ion include alkali metals, alkaline earth metals, ammonia, and alkanolamines. From the viewpoint of adjusting the dissolution rate, it is also preferable to use potassium ions in combination. In the case where the dissolution rate of the detergent particles having a large average particle diameter is set to be 50% or more and less than 90%, potassium ions in all the counter ions are 5%.
% By weight or more, more preferably 20% by weight or more, and particularly preferably 40% by weight or more.

Examples of the nonionic surfactant include an ethylene oxide (hereinafter referred to as “EO”) adduct of a higher alcohol or EO / propylene oxide (hereinafter referred to as “PO”).
Adducts), fatty acid alkanolamides, alkyl polyglycosides and the like. Particularly, the carbon number is 10 to 1
An alcohol adduct of 1 to 10 mol of EO of alcohol 6 is preferred in terms of removing sebum stains, hard water resistance, biodegradability, and compatibility with linear alkylbenzene sulfonates.

The high bulk density detergent particles include builders and bleaching agents (percarbonate, perborate,
Bleach activator, etc.), re-staining inhibitor (carboxymethyl cellulose, etc.), softening agent, reducing agent (sulfite, etc.), optical brightener, foam inhibitor (silicone, etc.), fragrance, etc. .

Next, the components constituting the enzyme-containing particles will be described. The enzyme-containing particle group contains a water-insoluble substance, a water-soluble binder, and an enzyme. The preferred composition is 45% by weight or more of a water-insoluble substance, and the more preferred composition is 5 to 40% by weight of a water-soluble binder and 0.5 to 30% by weight of an enzyme.

The water-insoluble substance is a substance which does not show solubility in water or shows little solubility, does not substantially deactivate enzymes, does not react with a water-soluble binder, and disperses in water. It is not particularly limited as long as it is a substance having the property of performing the above. Such a substance may be either an inorganic substance or an organic substance, but is more preferably an inorganic substance from the viewpoint of heat stability when used in a production method requiring heating such as spray drying. Specific examples include cellulose powder, zeolite, talc, clay, alumina, kaolin, titania, calcium carbonate, barium sulfate and the like, and zeolite and kaolin are particularly preferred in view of dispersibility in water.

Regarding the size of the water-insoluble substance, the average particle size of the primary particles is preferably 20 μm or less from the viewpoint of uniformity of distribution inside the enzyme-containing particles. As the average particle size of the primary particles becomes smaller, the enzyme-containing particle group becomes denser, and since the densification improves the particle strength and suppresses dusting, the average particle size of the primary particles is more preferably 10 μm or less, 0.1 to 5 μm is particularly preferred.

The content of the water-insoluble substance in the enzyme-containing particles is controlled by controlling the generation of dust, disintegrating and dispersing the enzyme-containing particles, and promoting the rapid elution of the enzyme. The content is 45% by weight or more, and preferably 50% by weight or more from the viewpoint of further improving the high-speed solubility. On the other hand, the content is preferably 90% by weight or less, more preferably 80% by weight or less, particularly preferably 70% by weight or less of the enzyme-containing particles from the viewpoints of suppressing dust generation and preventing undissolved residue. Therefore, considering simultaneously satisfying high-speed solubility and low dust generation and preventing the undissolved portion, the content is 50 to 9 of the enzyme-containing particle group.
0 wt% is preferable, 50-80 wt% is more preferable, and 50-70 wt% is particularly preferable.

In the present invention, the water-insoluble substances may be used alone or in combination. When two or more types of water-insoluble substances are used in combination, by mixing particles having different particle sizes or particles having different shapes, the structure of the enzyme-containing particle group can be densified or strengthened to suppress dust generation. It is possible.

The water-soluble binder is not particularly limited as long as it has the ability to bind the components constituting the particles, does not substantially inactivate the enzyme, and has the property of rapidly dissolving in water. 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.

The content of the water-soluble binder in the enzyme-containing particle group is 5% by weight of the enzyme-containing particle group from the viewpoint of low dust generation.
Or more, more preferably 15% by weight or more. From the viewpoint of high-speed solubility, the content is preferably 40% by weight or less, more preferably 30% by weight or less of the enzyme-containing particles. Therefore,
From the viewpoint of low dust generation and high-speed solubility, the content is preferably 5 to 40% by weight of the enzyme-containing particles, and 15 to 30% by weight.
Is more preferred.

[0029] Two or more water-soluble binders can be blended 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 the enzyme-containing particles can be further imparted by combining a binder that dissolves rapidly in water with a binder that has the ability to stabilize the enzyme.

[0030] The enzyme is not particularly limited as long as it is an enzyme exhibiting a cleaning effect when incorporated into a detergent. For example,
One or more selected from cellulase, protease, pectinase, amylase, lipase, and dextranase are preferably used.

The content of the enzyme in the enzyme-containing particles is preferably 0.5% by weight or more, and more preferably 2% by weight, from the viewpoint of expressing the enzyme activity. 30% by weight from the viewpoint of high-speed dissolution
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, for example, 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.

In the enzyme-containing particle group, in addition to the above components,
Other water-soluble substances may be contained. For example, stabilizers, excipients sodium chloride, calcium chloride,
Magnesium chloride, sodium sulfate and the like can be blended. The amount of the other water-soluble substance is preferably in a range where the sum of the contents of the enzyme, the water-soluble binder, and the water-soluble substance does not exceed 55% by weight of the group of the enzyme-containing particles. In particular, the content of other water-soluble substances is preferably not more than 15% by weight of the group of enzyme-containing particles from the viewpoints of fast solubility and low dust generation.
% By weight or less is more preferable.

Preferred combinations of the water-insoluble substance, the water-soluble binder and the other water-soluble substance include, for example, zeolite as the water-insoluble substance, sodium polyacrylate and saccharides as the water-soluble binder, and excipients as other water-soluble substances. For example, a combination such as mirabilite.

In particular, in the present invention, the enzyme-containing particles dissolve faster in the washing bath than the high-bulk-density detergent particles, so that the chlorine scavenger and / or
Alternatively, it is preferable to mix an antioxidant with the enzyme-containing particles. Thereby, a decrease in enzyme activity due to chlorine in the washing bath can be suppressed. For example, organic primary to tertiary amine compounds, inorganic ammonium salts, 1,3-dicarbonyl compounds, tocopherols, BHT, BHA, hydroquinone, sulfites and the like can be mentioned. Of these, monoethanolamine, hydroxyamine, ammonium sulfate, acetylacetone, alkyl acetoacetate, tocophenol, BHT, and sulfite are particularly preferred. Particularly, sulfite is preferable.

A diluent (eg, a bulking agent, a filler, etc.), a drying accelerator, a buffering agent, and the like for keeping the specific activity of the preparation particles constant can be added to the enzyme-containing particles as required. Coloring agents, stabilizers and the like can also be used as appropriate, and further, fragrances, deodorants,
Antistatic agents and the like can also be used.

The preferred structure of the enzyme-containing particles is a structure in which the water-soluble binder is unevenly distributed near the surface rather than inside. As a result, the water-soluble binder is first dissolved in water, and then the water comes into contact with the water-insoluble substance, so that the particles themselves disintegrate and disperse in water. Therefore, the enzyme is eluted into water promptly. Therefore, in the case of the enzyme-containing particles having such a structure, the enzyme can be rapidly eluted even if the particle diameter and the bulk density become large, and there is no undissolved residue. In addition, in the vicinity of the surface of the enzyme-containing particles, since the amount of the binder that binds 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, an enzyme-containing particle group to be measured and a pulverized product of the enzyme-containing particle group which are sufficiently pulverized in an agate mortar or the like to be in a uniform state are prepared. Then, under the condition that information up to about 10 μm can be obtained from the surface of the enzyme-containing particles, a method using both of them together with 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-containing 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-containing particles. .

The measurement conditions for obtaining information up to about 10 μm from the surface of the enzyme-containing 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 type infrared spectrophotometer is a 300 type photoacoustic detector manufactured by MTEC as a PAS cell.

As described above, the enzyme-containing particle group is useful because the enzyme elutes quickly, has no remaining residue, suppresses the generation of dust, and is non-classifying.

A preferable production method is a method in which a slurry containing, for example, a water-insoluble substance, a water-soluble binder, and an enzyme is dried in order to prevent a decrease in solubility due to compaction of the enzyme-containing particles. In order to obtain particles having an unevenly distributed structure, for example, a method of drying the slurry to produce a particle group, and then coating the surface of the particles with a water-soluble binder, and a method of spray-drying the slurry are exemplified. In particular, at the time of heating and drying, a large amount of a water-soluble binder collects in the vicinity of the surface with the movement of water, and therefore, a spray drying method that can easily obtain particles having the above structure is preferable.

When manufacturing by the spray drying method, first,
A slurry containing each component is prepared. The content of each component of the obtained enzyme-containing particle group is a value corresponding to the content of each component in the solid content of the slurry. As used herein, “solids” refers to water-insoluble substances, water-soluble binders, enzymes and other water-soluble substances. 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 since the dust generation of the resulting enzyme-containing 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.
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.

The order of blending the water-insoluble substance, the water-soluble binder and the enzyme when preparing the spray-dried slurry is not particularly limited, but there is an optimal sequence from the viewpoint of slurry blending preparation and dust generation. Can vary depending on the physical properties of the composition, and can be appropriately optimized. For example, when zeolite, sodium polyacrylate, saccharide, and sodium sulfate are used, enzymes, sodium sulfate, sugar, zeolite,
It is preferable to mix them in the order of sodium polyacrylate.

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 blowing temperature during spray drying is preferably 140 to 180 ° C. Performing spray drying in such a temperature range is preferable because productivity is improved and the enzyme is not substantially deactivated.

Further, for the purpose of reducing the amount of dust generated from the enzyme-containing 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 coated on the surface of the particles. May be used for coating. 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 2,000 to 10,000 are more preferable. As a specific coating operation, for example, there is a mode in which the coating agent is melted by heat and applied to the surface of the spray-dried particles.

The enzyme-containing particles having high solubility to the extent specified in the present invention, reduced classification in detergents, and reduced dust-producing enzyme-containing particles have not been known so far. A method for obtaining such an enzyme-containing particle group has not been known. However, as described herein,
By a simple method such as spray drying of a slurry in which a specific component is present, the solubility is high, classification in a detergent is suppressed, and a group of enzyme-containing particles with reduced dust generation can be obtained. For this reason, the action of the enzyme can be sufficiently exerted from a non-conventional approach, and the detergency is improved.

[0048]

[Example] [Low dusting property] The low dusting property in the present invention is as follows.
The particle generation amount is 1000 mg or less per 20 g of the enzyme particle group. This dust generation amount is more preferably 500 mg or less, and further preferably 100 mg or less. The standard value of the amount of generated dust also changes depending on the type of 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.

The amount of dust generated is as follows: a cylinder having a diameter of 2.0 cm and a weight of 32.2.
g of crushed balls 1 and 4 crushed balls.
While rotating at 4 rpm, dry air is passed through the air inlet 4 toward the air outlet 5 at a rate of 20 L / min.
20 g of the enzyme particle group was placed in a rotary dust meter that was collected by the method described above, and the amount of dust was measured when measurement was performed for 20 minutes. The filter 3 used had a diameter of 5.0 cm, a collected particle diameter of 0.5 μm, and a pressure loss of 0.42 kPa at a ventilation rate of 5 cm / s.

The rotary dust meter used for measurement is, for example, a rotary dust meter having a structure shown in FIG.
For example, a dust meter TYPE. III can be used. [Average particle size] 5 using a standard sieve of JIS Z8801.
After shaking for minutes, it was determined from the weight fraction depending on the sieve size. [Bulk density] It was measured by a method specified by JIS K 3362. [Non-classifying property] 1 g of the colored enzyme particles was added to 100 g of the detergent particles (average particle diameter 400 μm, bulk density 750 g / L).
After blending, the mixture was shaken with a mixer. Whether or not classification had occurred was visually determined.

<Preparation of Enzyme-Containing Particle Group> 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. In a counter-current spray-drying tower (diameter 3 m, tower height 10 m), air flow rate 10
0 m ³ / min, blowing temperature 150 ° C., slurry spray amount 2
Spray drying was performed at 00 kg / Hr. Using a sieve, particles of 710 μm or more and particles of less than 125 μm were removed from the obtained particles to obtain four types of crude enzyme-containing particles having a water content of 3.8% by weight.

[0052]

[Table 1]

The cellulase 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. As the saccharide, Maltrich (MR-25, manufactured by Showa Sangyo Co., Ltd.) was used.

5.0 kg of the obtained group of crude enzyme-containing particles was
Stirring tumbling granulator with hot water of 60 ° C flowing through jacket (High Speed Mixer, FS-10, manufactured by Fukae Kogyo Co., Ltd.)
, The main shaft rotation speed 240 rpm, the crushing blade rotation speed 2
The mixture was stirred at 700 rpm. Polyethylene glycol (molecular weight: 6000) 25 melted at 80 ° C. with stirring
0 g was charged as coating. After charging the coating agent, the mixture was stirred for 10 minutes to coat the surface of the particles. From the obtained particle group, remove a particle group of 1410 μm or more using a sieve,
Enzyme-containing particle groups I to IV having a moisture value of 3.1% by weight were obtained. In the enzyme-containing particles of the enzyme-containing particle groups I to IV, a larger amount of the water-soluble binder was unevenly distributed near the surface than inside thereof. Table 1
Shows the physical properties.

<Preparation of Comparative Example of Enzyme-Containing Particle Group> Crude enzyme having protease activity and cellulase activity (Bacill
US sp.) (enzyme powder: 7.5% by weight)
Then, sodium lauryl sulfate was added so as to be 10 parts by weight with respect to 100 parts by weight of the enzyme powder in the aqueous solution to prepare an enzyme aqueous solution.

The enzyme aqueous solution was spray-dried at a hot air temperature of 150 ° C. and an exhaust air temperature of 75 ° C. to obtain a powdered enzyme preparation (particle size: 10 to 5).
0 μm). Next, granulation was performed using a high-speed mixer (FS-5, manufactured by Fukae Kogyo KK) to prepare an enzyme-containing particle group. The dissolution rate of the obtained enzyme-containing particles was 8
It was 0%. The composition of the enzyme-containing particles is as follows.

18 parts by weight of a powdered enzyme preparation, 55 parts by weight of a nuclear substance, 6.5 parts by weight of a binder, 2 parts by weight of titanium oxide,
18.5 parts by weight of sodium sulfate. The nuclear material has a particle size of 500
Sodium chloride having an average particle size of 610 μm, containing 11% by weight of particles having a particle size of μm or less and 9% by weight of particles having a particle size of 700 μm or more, was used. As the binder, polyethylene glycol 6000 (manufactured by Kao Corporation) was used.

Example 1 <Preparation of Detergent Composition 1> High bulk density detergent particles 1 were produced as follows. From the composition shown in Table 2, 3% by weight of nonionic surfactant, 5% by weight of crystalline silicate, 10% by weight of zeolite, 0.2% by weight of fragrance, and enzyme-containing particles are based on the weight in the total detergent composition. 5% solids from the components except for 1.3% by weight
A 0% by weight slurry was prepared and spray-dried to obtain a spray-dried particle group. Then, this was put into a high-speed mixer (manufactured by Fukae Industry Co., Ltd.) together with 10% by weight of crystalline silicate in the total detergent composition, and the remaining 3% by weight was added.
Of the non-ionic surfactant was sprayed to carry out stirring granulation. After granulation, 5% by weight of zeolite was added to all the detergent compositions, and the mixture was stirred to coat the granulated particles on the surface.
The mixture was transferred to a V blender, and the remaining zeolite and the remaining crystalline alkali metal silicate were mixed to prepare a high bulk density detergent particle group 1. Table 2 shows the physical properties of the high bulk density detergent particle group 1.

Detergent composition 1 was obtained by mixing 1.3% by weight of enzyme-containing particle group I and 0.2% by weight of fragrance with this high bulk density detergent particle group 1. Similarly, the comparative example enzyme-containing particles were mixed to obtain Comparative Example detergent composition 1 (Comparative Example 1). Table 3 shows the performance evaluation of the detergent composition.

Example 2 <Preparation of Detergent Composition 2> High bulk density detergent particles 2 were produced as follows. First, LAS-K12 based on the weight of the detergent composition in Table 2 was used.
Wt%, SFE-Na 10 wt%, polyoxyethylene alkyl ether 3 wt%, polyethylene glycol 1
Wt%, zeolite 10 wt%, acrylic acid-maleic acid copolymer 3 wt%, fatty acid sodium 8 wt%, 1
A 50% solids slurry consisting of 1% by weight of No. silicate, 15% by weight of sodium carbonate, 5% by weight of sodium sulfate, 1% by weight of sodium sulfite, and 0.3% by weight of fluorescent dye was prepared and spray-dried. Thus, a spray-dried particle group was obtained. To this, 3% by weight of crystalline silicate and 13% by weight of sodium carbonate based on the weight in the detergent composition were charged into a ribbon mixer and mixed. The obtained mixture was extruded into a cylindrical shape having a diameter of 10 mm by a pre-extrusion type twin-screw extrusion granulator (pelleter double: manufactured by Fuji Paudal Co., Ltd.) and compacted. The obtained pellets were pulverized and granulated with a flash mill (manufactured by Fuji Paudal Co., Ltd.) together with 5% by weight of zeolite in the total detergent composition to perform surface coating.
After removing coarse substances from the granules, the granules were transferred to a V blender, and the remaining zeolite was mixed to prepare two groups of detergent particles. Table 2 shows the physical properties of the high bulk density detergent particles 2
Shown in

Detergent composition 2 was obtained by mixing 1.3% by weight of enzyme-containing particle group II and 0.2% by weight of fragrance with this high bulk density detergent particle group 2. Similarly, a comparative example enzyme-containing particle group was mixed to obtain a comparative example detergent composition 2 (Comparative Example 2). Table 3 shows the performance evaluation of the detergent composition.

Examples 3 and 4 Similarly, detergent compositions 3 and 4 were prepared by combining the detergent particles and the enzyme-containing particles shown in Table 3.

[0063]

[Table 2]

Here, the acrylic acid-maleic acid copolymer was a sodium salt (70 mol% neutralized), and the monomer ratio was acrylic acid / maleic acid = 3/7 (molar ratio). As fluorescent dyes, Tinopearl CBS-X and Tinopearl AM
Weight ratio of S-GX (Ciba Specialty Chemicals) 1
/ 1 mixture was used. As the zeolite, a 4A zeolite having an average particle size of 3 μm (manufactured by Tosoh Corporation) was used. As the crystalline silicate, powder SKS-6 (manufactured by Clariant Tokuyama) was pulverized to have an average particle size of 50 μm.

[0065]

[Table 3]

[Method of Measuring Detergency]
According to the method described in JP-A-168485, column 14, line 6, an artificially stained cloth was prepared. Then, five artificially stained cloths of 10 cm × 10 cm were put in 1 L of the aqueous detergent solution for evaluation and washed at 100 rpm with a tergotometer (washing conditions:
Washing time 5 minutes, detergent concentration 0.0667% by weight, water hardness 4 ° DH, water temperature 10 ° C, rinsing with tap water for 5 minutes. ). The detergency was evaluated by visually comparing a pair of the stained cloths of the product of the present invention and the comparative example after cleaning. As a result, it was found that the product of the present invention had better detergency than the comparative example.

[0067]

EFFECT OF THE INVENTION The detergent composition of the present invention exhibits excellent solubility of washing water in the group of particles containing the enzyme, so that the action of the enzyme can be maximized and the detergency can be sufficiently exerted. In addition, classification in the detergent can be prevented, and the amount of dust generated by the enzyme can be 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. The upper diagram of FIG. 1 shows a front view, and the lower diagram shows a cross-sectional view taken along line AA.

[Explanation of symbols]

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

Continuing from the front page (72) Inventor Yoshinobu Imaizumi 1334 Minato, Wakayama City, Kao Corporation Research Laboratory (72) Inventor Hiroshi Nishimura 1334 Minato, Wakayama City, Kao Corporation Research Laboratory (72) Inventor Hiroyuki Yamashita Minato, Wakayama City 1334 Kao Corporation Research Laboratory F term (reference) 4H003 AB03 AB19 AB21 AB27 AB44 AC08 BA10 CA21 DA01 EA12 EA15 EA16 EA25 EA28 EB22 EB32 EB36 EC01 EC02 EC03 FA28 FA32 FA40 FA41

Claims (3)

[Claims] 1. A high bulk density detergent particle group containing a surfactant, wherein the detergent particle group is put into water at 5 ° C. and stirred for 60 seconds under the following stirring conditions to obtain a standard according to JIS Z8801. When used for a sieve (opening 74 μm), the formula (1)
A detergent composition comprising: a detergent particle group having a solubility of 50% or more and less than 90%, and an enzyme-containing particle group having a solubility of 85% or more under the same conditions:
[Stirring conditions: 1 L of hard water (71.2 mg CaCO ₃ /
L, a molar ratio of Ca / Mg of 7/3) was charged with 1 g of the sample,
In a 1L beaker (inside diameter 105mm), stirrer (length 35)
mm, diameter 8 mm), rotation speed 800 rpm Formula (1): dissolution rate (%) = {1- (T / S)} × 100 S: input weight (g) of sample, T: under the above stirring conditions The dry weight (g) of the solution residue of the sample remaining on the sieve when the aqueous solution obtained as described above was subjected to the sieve. ]. 2. The high bulk density detergent particles contain 4 surfactants.
The detergent composition according to claim 1, which comprises about 50 to 50% by weight, 8 to 50% by weight of an alkaline agent, and has an average particle size of 150 to 800 µm and a bulk density of 500 to 1200 g / L. 3. The enzyme-containing particle group contains 45 water-insoluble substances.
% Or more, containing a water-soluble binder and an enzyme, and having an average particle size of 150 to 500 μm and a bulk density of 5
2. The water-soluble binder has a structure in which the amount of the water-soluble binder is more unevenly near the surface than inside thereof.
The detergent composition according to any one of the preceding claims.