JP2002029903A - Elution-controlled agrochemical granule and method for producing the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an agrochemical granule from which the elution of an agrochemically active ingredient is controlled. SOLUTION: This agrochemical granule from which the elution of the agrochemically active ingredient is controlled is characterized in that the granule is obtained by covering the surface of the particle including the agrochemically active ingredient with a synthetic resin and a water-soluble polymer.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a pesticide granule in which elution of an active ingredient of a pesticide is controlled.

[0002]

2. Description of the Related Art When pesticide granules are treated with soil, particles are disintegrated due to the effects of moisture and rain in the soil, and the pesticide active ingredient is gradually released, so that the desired activity is exhibited. . However, if the release rate of the pesticidal active ingredient is too high, there are problems such as affecting plants and eliminating residual effects. In addition, there is a problem that the effect is lost if the release of the pesticidal active ingredient is too slow. For these reasons, various methods for controlling the dissolution of the pesticidal active ingredient have been conventionally studied for the purpose of maintaining the efficacy of the pesticide active ingredient or reducing phytotoxicity. For example, by coating the surface of the particles containing the pesticide active ingredient, as a granule whose dissolution is controlled, (1) a granular sustained-release pesticide in which a pesticide particle containing a water-soluble or transpirable pesticide ingredient is coated with a thermoplastic film; (Japanese Patent Publication No. 64-5002),
(2) Sustained-release granules (JP-B-64-4483) in which a granular composition containing an agricultural chemical active ingredient and a carrier is provided with a coating layer comprising an isocyanate compound and liquid paraffin.
(3) 0.5 to 1 with respect to 100 parts by weight of the pesticide-containing granular material.
A granular pesticidal composition coated with 5 parts by weight of a thermosetting resin (JP-A-10-167904); (4) an inner core containing an active pesticide, a water-soluble polymer and a solid carrier, and a coating layer. Particles, the inner core has an oil absorption of 2
0 or less, and the ratio of the coverage to the oil absorption of the inner core is 0.1 to 10 (JP-A-2000-128705), (5) Poorly water-soluble pesticide active ingredient A coated pesticide granule characterized in that the surface of the pesticide granule consisting of water and a water-swellable substance is coated with a synthetic resin, and a surfactant is blended in or on the coating (Japanese Patent Application Laid-Open No. 268103, JP-A-9-7
7608, JP-A-10-67604),
(6) Pesticide granules containing a poorly water-soluble pesticide active ingredient and coated with two or more layers of a thermosetting resin film and a film made of a waxy substance (Japanese Patent Application Laid-Open No. 11-5704);
(7) A first coating layer made of a highly water-swellable substance is formed on the surface of a granular carrier containing an agricultural chemical component, and a second coating made of an olefin polymer or a condensation polymer is formed on the surface of the first coating layer. Multilayer coated granular pesticide having a layer formed thereon
-9303, JP-A-6-80514),
(8) Time-disintegrating pesticide granules obtained by coating a pesticide granule comprising a water-soluble pesticide component and a water-swellable substance with a polymer of a biodegradable polymer and an olefin (JP-A-9-315904); A) Time-controlled release coated granules (JP-A-10-212205) in which the surface of pesticide particles containing a pesticide active ingredient is coated with a water-insoluble or poorly water-soluble powder and a thermoplastic resin.

[0003] Further, as the granules which are controlled to dissolve by forming a film comprising a mixture of a film-forming substance and a pesticidal active ingredient on the surface of a granular carrier, there are, for example, (10) granules composed of a water-absorbing substance. Agrochemical formulation composition (Japanese Patent Application Laid-Open No. 11-5703) in which a film composed of a low-temperature film-forming hydrophobic polymer and an agricultural chemical active ingredient is formed on the surface, and (11) the agricultural chemical active ingredient is dispersed in the coating. A coated agricultural and horticultural granule (Japanese Patent Publication No. 18-18), characterized in that the composite film of the polyurethane and the water-soluble polymer compound is coated on a granular carrier.
No. 925), (12) A coated pesticide granule obtained by coating the surface of a granular carrier mainly composed of a water-swellable substance or a mineral substance with a composition comprising an agricultural chemical active ingredient and a thermoplastic resin. A time-release type coated pesticide granule characterized by further coating the surface of the granule with a resin (JP-A-9-14)
3005, JP-A-9-216802),
(13) A raw powder obtained by mixing and grinding a pesticide active ingredient and bentonite as essential ingredients, using a mixture of water selected from sugars, polyvinyl alcohol, vinyl acetate resin, acrylic resin and the like as a non-disintegrating carrier. Coated granules (JP-A-5-906).

[0004]

However, even pesticide granules to which these dissolution control techniques have been applied are still unsatisfactory from the viewpoints of dissolution, medicinal properties, phytotoxicity, and the like. For example, the aforementioned (1) to (4), (10),
In the methods (11) and (13), a large amount of resin is required to maintain the intended medicinal effect, and on the other hand, the release of the pesticidal active ingredient takes a long time, and the biological effect deteriorates. In addition, in the methods (5) to (9) and (12), the drug is released after a certain period of time, so that phytotoxicity can be avoided. However, when the drug is released, the drug is released quickly. Poor persistence of drug effect. Therefore, there is a demand for the development of further improved formulation technology for pesticide granules with controlled dissolution.

[0005]

Means for Solving the Problems The present inventors have intensively studied to solve these problems. As a result, they have found that granules in which the surface of solid particles containing an agricultural chemical active ingredient is coated with a synthetic resin and a water-soluble polymer are preferable.
As a result of further research, polyurethane resin as a synthetic resin,
Use of one or more of acrylic acid ester resin, styrene / acrylic acid ester resin, vinyl acetate resin, ethylene / vinyl acetate resin in combination with water-soluble polymer to reduce biological effects The elution amount is moderately controlled to a level that does not occur, and the elution control effect is exhibited over a longer period than in the past. As a result, it has been found that the application of the granules with controlled dissolution increases the duration of the medicinal effect and brings about the effect of reducing the phytotoxicity, and completed the present invention.

Accordingly, the present invention provides a method for coating a surface of a particle containing a pesticidal active ingredient with a synthetic resin, particularly a polyurethane resin, an acrylate resin, a styrene / acrylate resin, a vinyl acetate resin, and an ethylene / vinyl acetate resin. The present invention relates to a pesticide granule characterized by being coated simultaneously with one or more kinds and a water-soluble polymer. The present invention also relates to a method for producing pesticide granules in which the dissolution of such pesticide active ingredients is controlled.

In the present invention, particles containing an agricultural chemical active ingredient may be prepared by the method described below, and this surface may be coated with a synthetic resin and a water-soluble polymer. Either method may be used. That is,
(1) a method of mixing and adding a water-soluble polymer dissolved in water, (2) a method of adding a water-soluble polymer dissolved in water after adding the synthetic resin to the surface of particles,
(3) A method of adding a synthetic resin after adding a water-soluble polymer dissolved in water to the surface of the particles. However, it is important that the synthetic resin or the water-soluble polymer is mixed on the surface of the particles in order to make the dissolution last longer.

The pesticidal active ingredient which can be used in the present invention may be any of those generally used as pesticides such as insecticides, fungicides, herbicides, plant growth regulators, and one or more of these. May be used together.

[0009] Such pesticidal active ingredients include, for example, insecticides such as organophosphorus, carbamate, pyrethroid, chloronicotyl, phenylpyrazole, nelaystoxin, benzoylphenylurea,
Examples include compounds such as natural insecticides, acaricides, nematicides and the like.

Examples of disinfectants include inorganic copper agents, organic copper agents, inorganic sulfur agents, organic sulfur agents, organic phosphorus compounds, benzimidazole compounds, dicarboximide compounds, acid amide compounds, triazole compounds, imidazole compounds, and methoxy compounds. Acrylate, strobilurin, anilinopyrimidine, dithiolane, quinoxaline, aminopyrimidine, phenylpyrrole, triazine, cyanoacetamide,
Examples include compounds such as guanidines, antibiotics, and fungicides of natural products.

Examples of herbicides include phenoxy acid, carbamate, acid amide, acetanilide, and the like.
Urea type, sulfonylurea type, pyrimidyloxybenzoic acid type, triazine type, diazine type, diazole type, piperidylium type, dinitroaniline type, aromatic carboxylic acid type, imidazolinone type, fatty acid type, organic phosphorus type, amino acid type, diphenyl ether type And nitrile compounds.

The plant growth regulator includes, for example, ethylene, indoleacetic acid, gibberellin and the like.

Specific specific pesticidal active ingredients contained therein are described, for example, in "Agrochemical Handbook 1998 Edition".
(Japan Plant Protection Association, December 15, 1998
Issue), “Shibuya Index 8th Edition” [“SH
IBUYA INDEX: 8th Edition "
(Published December 15, 1998)], "The Pesticide Manual, 11th Edition"["The Pesticide
ide ManualEleventh Edition
n "(British Crop Protection)
n Council))].

The pesticidal active ingredient used in the present invention is not limited to these examples only, but may be applied if it is necessary to control the dissolution of the pesticidal active ingredient. In addition, various other insecticides, fungicides, herbicides, plant growth regulators, etc. other than those described above can also be used. The amount of these pesticidal active ingredients added to the preparation is generally 0.01 to 90% by weight, preferably 0.1 to 80% by weight, based on the total amount of the preparation.

The synthetic resin that can be used in the present invention is not limited to the use of a specific resin, but preferred synthetic resins include polyurethane resin, acrylate resin, styrene / acrylate resin, and vinyl acetate. Resin, ethylene-vinyl acetate resin. Examples of the polyurethane resin include Superflex 126, Superflex 150, Superflex 160 (these are trade names of Daiichi Kogyo Seiyaku Co., Ltd.), Hydran A
P-40 (trade name of Dainippon Ink and Chemicals, Inc.)
And the like. Examples of the acrylate resin include Movinyl 745 (trade name, manufactured by Hoechst Gosei Co., Ltd.), Polysol AP-4690, and Polysol AP-6.
09L, POLYSOL AP-4770 (trade name, manufactured by Showa Polymer Co., Ltd.), Aquabrid 4173 (trade name, manufactured by Daicel Chemical Industries, Ltd.) and the like.
Examples of the styrene-acrylate resin include Movinyl 860 (trade name of Hoechst Gosei Co., Ltd.), Polysol AP-4710, Polysol AP-4750,
POLYSOL AP-5051 (the above are trade names manufactured by Showa Polymer Co., Ltd.) and the like. Examples of vinyl acetate resin include Movinyl 116 (trade name of Hoechst Gosei Co., Ltd.), Polysol SH-502, Polysol CR-
12-42, and Polysol AX-500 (trade names, manufactured by Showa Polymer Co., Ltd.). ethylene·
Examples of vinyl acetate resin include Movinyl 101E (trade name of Hoechst Gosei Co., Ltd.), Polysol P-3,
Polysol P-38 (the above names are trade names, manufactured by Showa Polymer Co., Ltd.). However, examples of the synthetic resin that can be used in the present invention are not limited to only these examples.

In addition, there is no problem in using one or more of these synthetic resins in combination with the formulation, and the amount of the synthetic resin added depends on the dissolution control effect and economical efficiency. 0.1 to 40% by weight therein, preferably 0.1 to 40% by weight.
3 to 30% by weight. The range of the addition amount is appropriately determined in consideration of the type of the synthetic resin to be used, the water solubility, the period for controlling elution, the chemical damage to the plant, and the like.

The water-soluble polymer that can be used in the present invention is not particularly limited as long as it forms a film.
Examples include polyvinyl alcohol (PVA), starch, dextrin, methylcellulose, carboxymethylcellulose (CMC), sodium alginate, polyethylene glycol (PEG), pullulan, xanthan gum, sodium polyacrylate, and water-soluble soybean polysaccharides. There are various grades of these water-soluble polymers such as those having different molecular weights. However, in the present invention, the use of specific polymers is not limited. In addition, there is no problem in using one or more of these water-soluble polymers even if they are used in combination in the preparation. )) Is 0.01 to 10% by weight, preferably 0.1 to 7% by weight. The width of the addition amount may be appropriately determined in consideration of the same reason as the width of the addition amount of the synthetic resin.

The ratio of the synthetic resin to the water-soluble polymer is not limited to a specific ratio, but may be 1: 100.
４4000: 1, preferably from 3:70 to 300:
It is one.

As the particles for containing the pesticidal active ingredient used in the present invention, an inorganic carrier or an organic carrier usually used for pesticide granules is used. Examples of such an inorganic carrier include, for example, clay, diatomaceous earth, bentonite, talc, siegrite, sericite, acid clay, quartzite, pumice, zeolite, vermiculite, white carbon, vitreous powder obtained by pulverizing shirasu balloon and the like. Yes, examples of organic carriers include saw iron, straw, pulp, fir, starch, lactose and the like. However, the particles containing the pesticidal active ingredient used in the present invention are not limited to these, but do not adversely affect the pesticidal active ingredient used, such as decomposing, and also, the pesticide in water Those which can release the active ingredient gradually are preferably used.

In the present invention, the granules include widely used granules as they are, as well as fine granules having a small particle size, jumbo granules having a large particle size, and a pack containing the present granules in a pack. It can also be applied to agents.

In practicing the present invention, a stabilizer, a binder, an organic solvent, an antiseptic and antibacterial agent for the pesticide active ingredient may be used during the formulation process for incorporating the pesticide active ingredient into solid particles, if necessary. , A pH adjuster, a surfactant and the like can be added. That is, as a stabilizer of the pesticide active ingredient,
An antioxidant, an ultraviolet ray inhibitor, a crystal precipitation inhibitor and the like may be added as necessary, and sorbic acid, potassium sorbate, parachloro-metaxylenol, butyl paraoxybenzoate and the like may be added as preservatives and antibacterial agents.

Examples of organic solvents that can be used include petroleum, animal oil, and vegetable oils. For example, petroleum solvents include alkylbenzene, phenylxylylethane,
There are paraffin and the like, and animal oils include beef tallow, lanolin and the like, and vegetable oils include soybean oil, rapeseed oil, castor oil and the like. If necessary, generally used substances such as calcium carbonate, magnesium carbonate, sodium hydroxide, phosphoric acid, hydrochloric acid, and citric acid may be added as pH adjusters.

Examples of the binder include dextrin, cellulose, methylcellulose, ethylcellulose, carboxymethylcellulose, and those derived from natural products.
Hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, starch, carboxymethyl starch, pullulan, sodium alginate, ammonium alginate, dextran, mannan, pectin, tragacanth gum, mannitol, sorbitol, propylene glycol alginate ester, guar gum, locust bean gum, gum arabic Alternatively, there are saccharide-based substances such as xanthan gum, and protein-based substances such as gelatin and casein. Examples of synthetic substances include polyvinyl alcohol, polyethylene oxide,
Examples include polyethylene glycol, an ethylene / propylene block polymer, sodium polyacrylate, and polyvinylpyrrolidone.

Surfactants which can be used in the present invention include nonionic surfactants, anionic surfactants, cationic surfactants, amphoteric surfactants, and the like. Oxyethylene alkyl ether, polyoxyethylene alkyl aryl ether, polyoxyethylene styryl phenyl ether, polyoxyethylene alkyl ester, polyoxyethylene sorbitan alkylate, polyoxyethylene phenyl ether polymer, polyoxyethylene alkylene aryl phenyl ether, polyoxyethylene Examples include alkylene glycol, polyoxyethylene, and polyoxypropylene block polymers. Examples of anionic surfactants include lignin sulfonate, alkylaryl sulfonate, and dialkyl sulfonate. Hosakushineto, polyoxyethylene alkyl aryl ether sulfates, alkylnaphthalene sulfonates, polyoxyethylene styryl phenyl ether sulfates, and the like lauryl sulfate. Examples of the cationic surfactant include an alkylamine salt, and examples of the amphoteric surfactant include an amidobetaine type,
There are imidazaline type and the like, but it is not limited to these examples.

[0025]

BEST MODE FOR CARRYING OUT THE INVENTION The pesticide granules of the present invention with controlled elution can be easily prepared by the following methods.

1. Preparation method of particles containing pesticidal active ingredient Add the pesticidal active ingredient, extender, and, if necessary, surfactant, binder, etc., and mix and grind with a hammer mill (trade name of Fuji Paudal Co., Ltd.) Thereafter, the mixture is kneaded with water, granulated by using an extrusion granulator, dried by a fluidized bed dryer, and sized to prepare. Alternatively, granulation may be performed by a tumbling granulator while adding water to the powder mixture, followed by drying and sizing. Further, the powder mixture may be dispersed in water and produced by a spray drying granulator, or a fluidized bed in which the binder is sprayed and granulated by spraying a binder, an aqueous solution or an active ingredient while the powder mixture is fluidized. It can also be produced by a granulator.

2. Coating method of synthetic resin and water-soluble polymer on particles containing pesticidal active ingredient Put solid particles containing pesticidal active ingredient prepared by method 1 into a fluidized granulating dryer and spray on the surface of the particles A synthetic resin and a water-soluble polymer dissolved in water are sprayed from a nozzle by any one of the following methods (1) to (3) and dried. By doing so, a simultaneous coating of a synthetic resin and a water-soluble polymer can be formed on the surface of the solid particles containing the pesticidal active ingredient. In this way, the granules with controlled elution according to the present invention are obtained. In addition, it can also be produced by a method in which a sugar-coated film coating apparatus is used to spray a synthetic resin and a water-soluble polymer dissolved in water from a spray nozzle, followed by drying.

When the synthetic resin and the water-soluble polymer are sprayed, (1) the synthetic resin and the water-soluble polymer dissolved in water are mixed and sprayed from the same nozzle. After adding to the surface of the particle containing the active ingredient, a water-soluble polymer dissolved in water is sprayed, or (3) the water-soluble polymer dissolved in water is added to the surface of the particle containing the pesticide active ingredient. After that, any method of spraying the synthetic resin may be used.However, in order to achieve long-lasting elution, the synthetic resin or the water-soluble polymer must be synthesized before the film is completely formed. It is important that the resin and the water-soluble polymer mix at the surface of the particles.

[0029]

Next, the present invention will be described more specifically with reference to examples and comparative examples.

In each of the examples and comparative examples, No.
Is No. in the table. Corresponding to In addition, “parts” means all parts by weight.

The coating method of the above (1) is described in Examples 1, 4, 7
To 9, and the coating method of (2) is described in Examples 2, 5, and 10.
The coating method of (3) is shown in Examples 3, 6, and 11, respectively.

Example 1 Kasugamycin (hydrochloride: the same applies hereinafter) as an antibiotic bactericide 2.0 parts, sodium lignin sulfonate 2.0
Parts, 0.2 parts of phosphoric acid and 89.5 parts of clay are mixed with a hammer mill (trade name of Fuji Paudal Co., Ltd.). Thereafter, 30.0 parts (3.0 parts as polyvinyl alcohol) of a 10% aqueous polyvinyl alcohol solution (degree of saponification 80 to 83, degree of polymerization 500) was added to this mixture, and a double-arm kneader (manufactured by Fuji Paudal Co., Ltd.) was added. And mix. Next, the mixture is granulated with an extrusion granulator (manufactured by Nippon Pharmaceutical Co., Ltd.) equipped with a screen having a diameter of 1.0 mm, further dried with a fluidized bed dryer (manufactured by Fuji Paudal Co., Ltd.), sieved, and used Solid particles containing the active ingredient are obtained. These particles 96.7
Parts were placed in a fluidized-granulation dryer, and 10.0 parts (3.0 parts as a polyurethane resin) and 5 parts of Superflex 126 (30% polyurethane resin, trade name of Daiichi Kogyo Seiyaku Co., Ltd.) were added to the surface of the particles. A mixed solution of 6.0 parts (0.3 parts as polyvinyl alcohol) of a 20% aqueous polyvinyl alcohol solution (degree of saponification 98 to 99, degree of polymerization 1700) was uniformly sprayed using a spray nozzle. Then dry,
The granules of the present invention were obtained.

Example 2 First, 10.0 parts of Superflex 126 (described above) (3 parts of polyurethane resin) were applied to particles containing an agrochemical active ingredient prepared according to Example 1 using the apparatus according to Example 1. .0 part) before spraying and forming a complete coating.
% Polyvinyl alcohol aqueous solution (saponification degree 98-99,
6.0 parts (0.3 parts as polyvinyl alcohol) were sprayed. Then, it dried and obtained the granule of this invention.

Example 3 A 5% aqueous polyvinyl alcohol solution (degree of saponification 98 to 99, degree of polymerization) was first applied to the particles containing the pesticidal active ingredient prepared according to Example 1 using the apparatus according to Example 1. 170
0) 6.0 parts (0.3 parts as polyvinyl alcohol)
Was sprayed, and 10.0 parts (3.0 parts as a polyurethane resin) of Superflex 126 (described above) were sprayed before forming a complete film. Then, it dried and obtained the granule of this invention.

Example 4 Particles containing an agrochemically active ingredient were prepared according to Example 1 using 87.8 parts of the clay of Example 1 and then superflex 160 (polyurethane resin 30%, Daiichi Kogyo Seiyaku Co., Ltd.) 6.67 parts (trade name of a company) (2.0 parts as a polyurethane resin) is sprayed, and polysol SH-502 (vinyl acetate resin 50%,
A mixture of 4.0 parts (trade name, manufactured by Showa Polymer Co., Ltd.) (2.0 parts as vinyl acetate resin) and 20.0 parts (1.0 part as pullulan) of a 5% pullulan aqueous solution was sprayed. Then, it dried and obtained the granule of this invention.

Example 5 10.0 parts of kasugamycin, 0.5 part of sodium lauryl sulfate and 50.5 parts of clay are mixed by a hammer mill. Add 10% potato starch aqueous solution 2 to this mixture.
Add 0.0 parts (2.0 parts as potato starch), knead with a double arm kneader and mix. Then 1.0mm
The mixture is granulated by an extrusion granulator equipped with a screen having a diameter, dried by a fluidized bed drier, and then sieved to obtain particles containing the pesticidally active ingredient. 63.0 parts of the particles are placed in a sugar coating film coating apparatus, and 60.0 parts of Polysol SH-502 (described above) (30.0 parts as a vinyl acetate resin) are sprayed. 70.0 parts of an aqueous solution of pullulan (7.0 parts as pullulan) were sprayed. Then, it dried and obtained the granule of this invention.

Example 6 Particles containing the pesticidally active ingredient were prepared according to Example 5 using 77.4 parts of the clay of Example 5, and then 0.5% by using an apparatus according to Example 5. Xanthan gum aqueous solution 2
Spray 0.0 parts (0.1 parts as xanthan gum),
Before a complete coating is formed, Polysol AP-4690
28.6 parts (10.0 parts as an acrylic ester resin) were sprayed (35% of an acrylic ester resin, trade name, manufactured by Showa Polymer Co., Ltd.). Thereafter, drying was performed to obtain the granules of the present invention.

Example 7 Particles containing an agrochemically active ingredient were prepared according to Example 5 using 71.5 parts of the clay of Example 5, and polysol AP-4710 was prepared using an apparatus according to Example 5. (50% of styrene / acrylate resin, trade name of Showa Polymer Co., Ltd.) 30.0 parts (15.0 parts as styrene / acrylate resin) and 100.0 parts of 1% sodium alginate aqueous solution (sodium alginate) (1.0 part) was sprayed and then dried to obtain the granules of the present invention.

Example 8 Particles containing an agricultural chemical active ingredient were prepared according to Example 5 using 74.4 parts of the clay of Example 5, and then Polysol P-38 was prepared using an apparatus according to Example 5. (Ethylene / vinyl acetate resin 48%, trade name of Showa Polymer Co., Ltd.)
25.0 parts (12.0 parts as ethylene-vinyl acetate resin
Parts) and 5% aqueous solution of polyvinyl alcohol (degree of saponification 98)
-99, polymerization degree 500) 2.0 parts (0.1 parts as polyvinyl alcohol) and 5% aqueous solution of pullulan 20.0
Parts (1.0 part as pullulan) was sprayed, and then dried to obtain the granules of the present invention.

Example 9 2.5 parts of simethrin, a triazine herbicide, 1.0 part of sodium lauryl sulfate, 10.0 parts of diatomaceous earth, 81.1 parts of clay, and 5.0 parts of carboxymethylcellulose were treated with a hammer mill. After mixing, 30.0 parts of water is added to 99.6 parts of the mixture, and the mixture is kneaded and mixed with a double-arm kneader. Next, the mixture is granulated by an extrusion granulator equipped with a 1.2 mm diameter screen, dried by a fluidized bed dryer and then sieved to obtain particles containing an agricultural chemical active ingredient. 99.6 parts of the particles were put into a sugar-coated film coating apparatus, and hydran AP-40 (described above) (0.3 as a polyurethane resin) was added.
Parts) and 5% aqueous solution of polyvinyl alcohol (degree of saponification 98)
(99 parts, polymerization degree: 1700) A mixture of 2.0 parts (0.1 part as polyvinyl alcohol) was sprayed and then dried to obtain the granules of the present invention.

Example 10 The clay of Example 9 was used in an amount of 79.7 parts, and particles containing the pesticidally active ingredient were prepared according to Example 9. Then, using an apparatus according to Example 9, polysol AP-4710 was used. (Described above)
3.0 parts (1.5 parts as a styrene acrylate resin) are sprayed, and before a complete film is formed, 0.1 part is sprayed.
60.0 parts of 5% potato starch (0.3 parts as potato starch) was sprayed. Then, it dried and obtained the granule of this invention.

Example 11 Particles containing an agrochemical active ingredient were prepared in the same manner as in Example 9 except that the clay of Example 9 was used in 76.2 parts. 6.0 parts (0.3 parts as polyvinyl alcohol) of an aqueous solution (degree of saponification 98-99, degree of polymerization 1700) is sprayed, and before a complete film is formed, polysol SH-502 (described above).
16.7 parts (5.0 parts as a vinyl acetate resin) were sprayed. Then, it dried and obtained the granule of this invention.

Comparative Example 1 The clay of Example 1 was used in an amount of 89.8 parts, and particles containing a pesticidally active ingredient were prepared in accordance with Example 1. Then, using an apparatus in accordance with Example 1, Superflex 126 ( As described above)
10.0 parts (3.0 parts as a polyurethane resin) were sprayed and then dried to obtain comparative granules.

Comparative Example 2 Particles containing an agrochemical active ingredient were prepared in the same manner as in Example 1 except that the clay of Example 1 was 92.5 parts, and 5% polyvinyl alcohol was used in an apparatus in accordance with Example 1. 6.0 parts (0.3 parts as polyvinyl alcohol) of an aqueous solution (degree of saponification 98 to 99, degree of polymerization 1700) was sprayed, and then dried to obtain comparative granules.

Comparative Example 3 10.0 parts of Superflex 126 (described above) (3.0 polyurethane polyurethane resin) were applied to the particles containing the pesticidally active ingredient prepared according to Example 1 using the apparatus according to Example 1. Part) was sprayed and dried to form a complete film. Thereafter, 6.0 parts (0.3 parts as polyvinyl alcohol) of a 5% aqueous polyvinyl alcohol solution (degree of saponification 98 to 99, degree of polymerization 1700) were sprayed and dried to obtain comparative granules.

Comparative Example 4 A 5% aqueous solution of polyvinyl alcohol (degree of saponification 98-99, degree of polymerization 1700) was applied to particles containing an agricultural chemical active ingredient prepared according to Example 1 by using an apparatus according to Example 1.
After spraying 6.0 parts (0.3 parts as polyvinyl alcohol) and drying, a film was completely formed. Thereafter, 10.0 parts (3.0 parts as a polyurethane resin) of Superflex 126 (described above) were sprayed and dried to obtain comparative granules.

Comparative Example 5 The clay of Example 5 was used in an amount of 57.5 parts, and particles containing a pesticidally active ingredient were prepared according to Example 5. Then, using an apparatus according to Example 5, Polysol SH-502 was used. (Described above) 6
0.0 parts (30.0 parts as a vinyl acetate resin) were sprayed and then dried to obtain comparative granules.

Comparative Example 6 The clay of Example 5 was used in an amount of 77.5 parts, and particles containing the pesticidally active ingredient were prepared in accordance with Example 5. Then, using an apparatus in accordance with Example 5, Polysol AP-4690 was used. (Described above)
28.6 parts (10.0 parts as acrylate resin)
Part) was sprayed and then dried to obtain comparative granules.

Comparative Example 7 Particles containing an agricultural chemical active ingredient were prepared in the same manner as in Example 5 except that the clay of Example 5 was used in an amount of 72.5 parts, and polysol AP-4710 was prepared using an apparatus in accordance with Example 5. (Described above)
30.0 parts (15.0 parts as a styrene acrylate resin) were sprayed and then dried to obtain comparative granules.

Comparative Example 8 Particles containing an agrochemically active ingredient were prepared according to Example 5 using 75.5 parts of the clay of Example 5, and then Polysol P-38 was prepared using an apparatus according to Example 5. (Described above)
0 parts (12.0 parts as ethylene / vinyl acetate resin) were sprayed and then dried to obtain comparative granules.

Comparative Example 9 1.0 part of sodium lauryl sulfate, diatomaceous earth 10.0
Parts, 81.1 parts of clay and 5.0 parts of carboxymethylcellulose were mixed by a hammer mill.
30.0 parts of water is added to 1 part, and the mixture is kneaded and mixed with a double-arm kneader. Next, the mixture is granulated by an extrusion granulator equipped with a screen having a diameter of 1.2 mm, further dried by a fluidized-bed dryer, and then sieved to obtain particles. 97.1 parts of the particles are put into a sugar-coated film coating apparatus, and the following mixed solution is placed on the surface of the particles: 2.5 parts of simethrin, a triazine herbicide, 1.3 parts of hydran AP-40 (described above). (0.3 parts as a polyurethane resin) and a 5% aqueous polyvinyl alcohol solution (degree of saponification 98 to 99, degree of polymerization 170)
0) 2.0 parts (0.1 part as polyvinyl alcohol)
Was sprayed and then dried to obtain comparative granules.

COMPARATIVE EXAMPLE 10 The clay of Example 9 was used in an amount of 79.7 parts and the particles containing the pesticidal active ingredient prepared according to Example 9 were subjected to 0.5% potato by using an apparatus according to Example 9. Starch 60.0
(0.3 parts as potato starch) and then dried to form a complete coating. Thereafter, 3.0 parts of Polysol AP-4710 (described above) (1.5 parts as a styrene-acrylate resin) were sprayed and dried to obtain comparative granules.

COMPARATIVE EXAMPLE 11 The clay of Example 9 was used in an amount of 79.7 parts, and the particles containing the pesticidal active ingredient prepared according to Example 9 were applied to a polysol AP-4710 (using the apparatus according to Example 9). As described above)
After spraying 3.0 parts (1.5 parts as a styrene acrylate resin), it was dried to completely form a film. Then, 0.5% potato starch 60.0%
(0.3 parts as potato starch) was sprayed and dried to obtain comparative granules.

[0054]

The pesticide granule of the present invention, the dissolution of which is controlled, can control the dissolution of the pesticide active ingredient over a long period of time as compared with the conventional preparations. As a result, when the pesticide granule of the present invention is applied to soil, the elution of the pesticide active ingredient is controlled later than in the past, due to moisture or rainfall in the soil,
It elutes gradually. As a result, phytotoxicity to plants can be avoided, and residual effects are imparted. In addition, the period can be appropriately extended by selecting the synthetic resin and the water-soluble polymer to be used and the amount thereof.

In order to specifically show the elution control effect of the present invention, test examples will be described.

Test Example 30 bottles were placed in a stoppered Erlenmeyer flask having a capacity of 200 ml.
200 ml of hard water at 3 ° C. was added, and 1 g of the pesticide granules prepared in Examples and Comparative Examples were added.
After inverting 0 times, it is left still in a thermostat at 30 ° C. After one day, three days, five days, ten days, and thirty days, the conical flasks are taken out and inverted 30 times, and 5 ml of the test solution is immediately collected. Thereafter, analysis was performed by HPLC, and the elution rate (%) was calculated by the following equation.

[0057]

(Equation 1)

The results are shown in Tables 1 and 2.

[0059]

[Table 1]

[0060]

[Table 2]

Claims (7)

[Claims] 1. A pesticide granule in which elution of a pesticide active ingredient is controlled, wherein the surface of particles containing the pesticide active ingredient is coated with a synthetic resin and a water-soluble polymer. 2. The pesticide granule according to claim 1, wherein the surface of the particles containing the pesticide active ingredient is coated so that the synthetic resin and the water-soluble polymer are mixed. 3. The synthetic resin is a polyurethane resin, an acrylate resin, a styrene / acrylate resin,
The pesticide granule according to claim 1, wherein one or more of vinyl acetate resin and ethylene / vinyl acetate resin are used in combination. 4. A method for producing pesticide granules with controlled elution of pesticide active ingredients, wherein the pesticide active ingredients are supported on a granular carrier, and the surface thereof is coated with a synthetic resin and a water-soluble polymer. 5. The method for producing pesticidal granules according to claim 4, wherein the surface of the particles containing the pesticidal active ingredient is coated so as to be mixed with the synthetic resin and the water-soluble polymer. 6. The method according to claim 4, wherein the order of coating with the synthetic resin and the water-soluble polymer is either the first with the synthetic resin, the first with the water-soluble polymer, or both. 5. The method for producing pesticide granules according to 5. 7. The synthetic resin is a polyurethane resin, an acrylate resin, a styrene / acrylate resin,
7. A combination of one or more of vinyl acetate resin and ethylene / vinyl acetate resin.
A method for producing the pesticide granule according to the above.