JP2001192302A - Agrochemical granule and its manufacturing method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain agrochemical granules free from caking even in a long term storing, little in powdering and excellent in hydration characteristic and dispersibility. SOLUTION: This agrochemical granule comprises the agrochemical active ingredient; dextrin; water and water-soluble organic solvent or their mixed solvent, and zeolite.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention
The present invention relates to an agricultural chemical granule having good storage stability, a simple production method, and economical efficiency, and a method for producing the same.

[0002]

2. Description of the Related Art Conventionally, as a high-concentration pesticide formulation which is diluted and sprayed with water, and a pesticide formulation which is directly sprayed on paddy fields and fields,
Examples include emulsions, flowables (suspension), wettable powders, fine granules, powders and the like. However, since the emulsion uses a large amount of an organic solvent as a carrier, there are problems in safety such as flammability, odor, toxicity, irritation, and influence on the environment. In addition, flowable agents have problems such as aggregation, sedimentation and particle growth of dispersed particles after long-term storage, and stability of active ingredients. In addition, wettable powders, fine granules and powders are powder or fine granular preparations, so that at the time of production and preparation of a spray liquid, the scattering of fine powder and the complexity of measuring the drug are problematic. At the time of direct spraying, the influence on the environment due to the scattering of fine powder has become a problem.
In order to solve these problems, many studies have been made on granulation or granulation of preparations.

[0003] For example, granular pesticide wettable powders containing pesticidal active ingredients, starch and water-soluble inorganic salts (JP-B-53-1)
No. 2577); an emulsion containing an agricultural chemical active ingredient, and a water-soluble inorganic salt in which the amount of water of crystallization is adjusted (JP-A-56-71002);
Solid granular hydratable herbicide composition containing pyranose ring-containing polymer compound such as starch, hydrated magnesium sulfate and water (Japanese Patent Publication No. 64-12244); for a formulation containing a water-repellent active ingredient Wettable powder composition containing water, glycols or glycol ethers (JP-B-5)
-12321); a water-soluble pesticide granule containing a water-soluble pesticide active ingredient, lactose and a surfactant as essential components (JP-A-6-92803); containing a pesticide active ingredient and diatomaceous earth; Granular wettable powder further containing a surfactant (JP-A-6-128102); Granule containing an agrochemical active ingredient and anhydrous silica having an average particle size of about 5 to 20 nm (JP-A-9-315902) A water dispersible agricultural chemical granule containing acephate, dextrin having a degree of polymerization of 30 or less, and ammonium sulfate (JP-A-10-1396);
No. 07 gazette) are being studied.

[0004] However, conventional granular pesticide preparations or granular pesticide preparations are poor in hydration and dispersibility even when poured into water, and cannot be completely sprayed even if sufficiently stirred, or due to moisture absorption. There is a problem that the properties as a granular pesticide formulation or a granular pesticide formulation such as solidification cannot be sufficiently exhibited, and it has not always been satisfactory.

[0005] For this reason, there has been a strong demand for the development of pesticide granules that are less powdery, easy to measure and handle, and stable in storage and storage. In particular, pesticide granules containing a water-soluble pesticidal active ingredient may be solidified by pressurization or humidification when stored for a long period of time, and there has been a demand for improved storage stability.

[0006] Further, since the heat drying step of the pesticide granule requires a large amount of energy and time, it has been desired to develop a technique for producing the pesticide granule which can omit the heat drying step. In addition, when using an agricultural chemical active ingredient that is easily decomposed by water or heating, easily volatilized by drying, or has relatively high toxicity, the heating and drying process causes a decrease in the content of the agricultural chemical active ingredient, In some cases, problems such as environmental pollution may occur, and it has been desired to develop a technology for producing pesticide granules safely and inexpensively with no decrease in content even with such pesticide active ingredients.

[0007]

The present inventors have conducted intensive studies in order to solve the above-mentioned problems, and as a result, dextrin; water, a water-soluble organic solvent or a mixed solvent thereof; It has been found that, by blending, a pesticidal granule with less powdering, good hydration and dispersibility can be obtained without caking even after long-term storage. Furthermore, the manufacturing method can be easily formed into granules simply by mixing the above-mentioned components,
Since the fluidity can be easily imparted, the usual heating and drying step can be omitted, and it is economical. The present inventors have found that easy-to-use pesticide active ingredients or relatively toxic pesticide active ingredients can be easily and inexpensively formulated into granules having good physical properties and completed the present invention.

[0008]

The present invention provides an agricultural chemical active ingredient; dextrin; water, a water-soluble organic solvent or a mixed solvent thereof; and an agricultural chemical granule characterized by containing zeolite; and an agricultural chemical active ingredient; This is a method for producing a pesticide granule by granulating a composition containing dextrin; water, a water-soluble organic solvent or a mixed solvent thereof; and zeolite without drying the granulated product.

In the pesticidal granule of the present invention, the pesticidal active ingredient may be any pesticidal active ingredient such as an insecticide, a bactericide or a herbicide as long as it is solid at normal temperature, and one or more pesticidal active ingredients may be used. Components can be used.

Examples of the insecticide include pyrimidifen, milbemectin, mesomil, acephate, thiocyclam, imidacloprid, nitenpyram, acetamiprid, pyridafenthion, dimethoate, PMP, CMP
VMP, dimethylvinphos, DEP, NAC, MTM
C, MIPC, PHC, MPMC, XMC, benflacarb, pirimicarb, oxamyl, thiodicarb, cypermethrin, cartap, bensultap, diflubenzuron, teflubenzuron, chlorfluazuron, buprofezin, hexthiazox, fenbutazin oxide,
Pyridaben, clofentezine and the like.

As a bactericide, for example, (RS) -2-
(4-Fluorophenyl) -1- (1H-1,2,4-
Triazol-1-yl) -3-trimethylsilyl-2
-Propanol, hydroxyisoxazole, teclophthalam, diclomedine, pyroquilon, diram, thiuram, captan, TPN, fusalide, tolclofosmethyl, fosetyl, thiophanatemethyl, benomyl, carbentazole, thiabentazole, dietofencarb, iprodione, vinclozolin, procymidone, fluorimide , Oxycarboxin, mepronil, flutranyl, pencyclon, metalaxyl, oxadixyl, triadimefon, hexaconazole, trifolin,
Blasticidin S, kasugamycin, polyoxin,
Validamycin A, PCNB, Dazomet, Triazine, Probenazole, Isoprothiolane, Tricyclazole, Tetraconazole, Triclamide and the like.

Examples of herbicides include pyrazolate,
Glyphosate, bensulfuron-methyl, simazine, linuron, dimelone, atrazine, paraquat, oxolinic acid, glyphosinate, bialaphos, bentazone, bromobutide, ashram, benzofenap, bromacil, azimsulfuron, ethoxysulfuron, imazosulfuron, pyrazosulfuron-ethyl, fezosulfuron-ethyl , Pyributicarb, cafenstrole, etobenzanide, oxadialgyl, naproanilide, clomethoxynil, sidurone, chloromethoxyphene, pyrazoxyfen and the like.

The pesticidal active ingredient of the present invention is preferably a water-soluble pesticidal active ingredient having a solubility of at least 0.5 g / L at 20 ° C. in water, more preferably hydroxyisoxazole, Glyphosate, methomil, acephate,
Cartap, thiocyclam, acetamiprid, nitenpyram, imidacloprid, glufosinate or bialaphos, even more preferably mesomil, acephate, thiocyclam, hydroxyisoxazole, glyphosate or glufosinate, most preferably mesomemil.

The compounding amount of the pesticidal active ingredient of the present invention is usually 0.5 to 95% (percentage by mass in the pesticidal granules. Hereinafter, unless otherwise specified, the percentages related to the compounding amounts of the components are the same. And preferably 1 to 80%.

The dextrin used in the agricultural chemical granule of the present invention is obtained from various starches such as wheat starch, potato starch, corn starch, tapioca starch by enzymatic decomposition, acid decomposition, alkali decomposition or a combination thereof. Dextrin, preferably maltodextrin, acrodextrin or erythrodextrin, and even more preferably maltodextrin. Specifically, AMICOL No. 3L, AMICOL No. 1 (the trade name, manufactured by Nisse Chemical Co., Ltd.), Paindex # 3 and Paindex # 6 (the trade name, manufactured by Matsutani Chemical Industry Co., Ltd.).

The dextrin of the present invention is preferably a dextrin having a reducing sugar content (DE) of 5 to 50%.

The reducing sugar content (DE) is the ratio of reducing sugar in the solid content, and is described in Experimental Agricultural Chemistry (2) (3rd edition)
It can be measured according to the method described on pages 6 to 127.

The amount of the dextrin used in the present invention is usually
It is 1 to 10% in the pesticide granule, preferably 2 to 8%.
%.

The water-soluble organic solvent used in the pesticide granules of the present invention is a water-soluble organic solvent usually used in pesticide preparations, which is difficult to volatilize and dissolves in water at 20 ° C. at 80% or more. Those that can be used are preferred. Preferably, the dextrin is capable of dissolving 0.05 g / ml or more at 20 ° C., preferably ethylene glycol, diethylene glycol, propylene glycol, glycerin, N-methyl-2-pyrrolidone, dimethyl sulfoxide, formamide, dimethyl Formamide, dimethylacetamide or dimethylacrylamide, even more preferably ethylene glycol, diethylene glycol, propylene glycol, N
-Methyl-2-pyrrolidone or dimethylsulfoxide, most preferably ethylene glycol or diethylene glycol. The water-soluble organic solvent used is 2
A mixed solvent of more than one kind can also be used. In addition, water and a water-soluble organic solvent can be used as a mixed solvent. When mixed and used, water and a water-soluble organic solvent are mixed and used so that the above dextrin can be dissolved at 20 ° C. in an amount of 0.05 g / ml or more. The mixed solvent of water and the water-soluble organic solvent can be usually used by mixing at an arbitrary ratio, and preferably, the mixing ratio is 1: 9 to
9: 1.

The amount of the water, water-soluble organic solvent or mixed solvent thereof of the present invention is usually 0.5 to 5 per pesticide granule.
10%, preferably 1 to 8%.

The zeolite used in the pesticidal granule of the present invention is a hydrous silicate of aluminum containing an alkali metal such as sodium or potassium or an alkaline earth metal such as calcium. It has the characteristics of being easily reversibly dehydrated, binding to weakly retained water, and having a three-dimensional network structure. For example, mesolite (cubic system), fish-eye stone (tetragonal system), chabazite It is a fine powder obtained from minerals and synthetic products such as (trigonal), sodalite (orthorhombic), volatilite, bazite, and dolomite (both are monoclinic). 1 of the zeolite of the present invention
The loss on drying at 05 ° C. is preferably 10% or less, more preferably 5% or less. The maximum value of the particles of the zeolite of the present invention is preferably 63 μm or less,
More preferably, it is 45 μm or less.

The amount of the zeolite used in the present invention varies depending on the type and amount of other components, the loss on drying of the zeolite, the production model, and the like. Is 2 to 8%.

The agricultural chemical granule of the present invention may optionally contain a water-soluble carrier or a surfactant.

The water-soluble carrier to be used is not particularly limited as long as it is used for ordinary solid agricultural chemicals. For example, inorganic salts such as ammonium sulfate, sodium benzoate, potassium chloride and sodium hydrogen carbonate; lactose; Saccharides such as sucrose and glucose; urea; and the like, preferably ammonium sulfate, sodium benzoate, lactose or sucrose.

The amount of the water-soluble carrier used is usually from 0.1 to 90%, preferably from 1 to 7%, in the pesticide granule.
0%.

The surfactant used in the pesticide granule of the present invention is not particularly limited as long as it is one used for ordinary pesticides, and may be an anionic surfactant, a nonionic surfactant, or a cationic surfactant. Any surfactant such as an amphoteric surfactant and a zwitterionic surfactant can be used, and one or more of these surfactants can be used.
Further, when a surfactant is used as a granulation improver,
It can also be used as a solution of water, the above organic solvent or the above mixed solvent.

Examples of the anionic surfactant include, for example,
Naphthalenesulfonic acid, phenolsulfonic acid, alkylnaphthalenesulfonic acid and formalin condensate of these sulfonic acids, alkenylsulfonic acid, alkylsulfonic acid, ligninsulfonic acid, alkylarylsulfonic acid, polystyrenesulfonic acid, polycarboxylic acidstyrenecarboxylic acid and carboxylic acid Acid condensates, polyoxyethylene alkyl ether sulfates, polyoxyethylene alkyl aryl ether sulfates, dialkyl sulfosuccinic acids, higher fatty acids, etc., alkali metal salts, alkaline earth metal salts, ammonium or various amine salts, polyoxy Ethylene alkyl ether phosphate ester, polyoxyethylene alkyl aryl ether phosphate ester, polyoxyethylene aryl aryl ether phosphate ester and the same Alkali metal salts of phosphoric acid esters, such as alkaline earth metal salts, ammonium or various amine salts and the like, preferably, the sodium dodecylbenzenesulfonate {Specifically, Neopelex No.
6F powder (trade name, manufactured by Kao Corporation) and Neogen Powder (trade name, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.). {Or sodium dioctyl sulfosuccinate} Specifically, Jeropon SDS (trade name, manufactured by Rhone Poulin Nichika Corporation) and Newcol 291PG
(Trade name, manufactured by Japan Emulsifier Co., Ltd.). ｝
It is.

Examples of the nonionic surfactant include, for example,
Polyoxyethylene alkyl ether, polyoxyethylene alkyl aryl ether, polyoxyethylene aryl aryl ether, polyoxyethylene alkyl ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, block copolymer of polyoxyethylene and polyoxypropylene, Higher fatty acid alkanol amides and the like, preferably having an HLB value of 9 to 13 from the viewpoint of solubility in water and wetting action.
Of the range.

Incidentally, these surfactants to which ethylene oxide has been added may partially contain propylene oxide.

Examples of the cationic surfactant include, for example,
Examples thereof include an alkylamine salt, a quaternary ammonium salt, a pyridinium salt, and an amine oxide.

Examples of the zwitterionic surfactant include amino acid type and betaine type surfactants.

The surfactant used in the present invention includes:
Preferably, it is an anionic surfactant or a nonionic surfactant, more preferably, sodium dodecylbenzenesulfonate, sodium dioctylsulfosuccinate or a nonionic surfactant having an HLB value of 9 to 13. It is.

The amount of the surfactant to be used is usually 0.01 to 10% in the pesticide granules, preferably 0.1 to 10%.
1 to 5%.

The pesticidal granules of the present invention can contain other additives used for ordinary pesticidal granules, such as bitters, coloring agents, inorganic carriers, preservatives and the like. These may be selected according to the kind of the pesticidal active ingredient to be used.

The bittering agent is not particularly limited as long as it is commonly used in agricultural chemicals, and preferably includes sucrose octaacetate. The amount of the bitter agent to be used is usually 0.05 to 0.5%, preferably 0.1 to 0.3%, in the pesticide granule.

The colorant is not particularly limited as long as it is generally used in agricultural chemicals, and examples thereof include pigments.
Preferably, it is Brilliant Blue FCF, Cyanine Green G or Erio Green G. The amount of the coloring agent used is generally 0.05 to 0.5%, preferably 0.1 to 0.3%, in the pesticide granule.

The inorganic carrier is not particularly limited as long as it is generally used for agricultural chemicals, and includes, for example, a mineral carrier, and is preferably amorphous silicon dioxide, diatomaceous earth, calcium carbonate, clay or talc. is there. The amount of the inorganic carrier used is usually 0.1 to 90%, preferably 0.5 to 70%, in the pesticide granule.

The preservative is not particularly limited as long as it is commonly used in agricultural chemicals, and is preferably sorbic acid, potassium sorbate, parachlorometaxylenol, butyl parahydroxybenzoate or sodium dehydroacetate. is there. The amount of preservative used is usually in pesticide granules,
It is 0.1 to 3%, preferably 0.5 to 2%.

[0039]

BEST MODE FOR CARRYING OUT THE INVENTION The pesticidal granules of the present invention include, among granulation methods used in the production of ordinary pesticide granules, for example, stirring granulation, tumbling granulation and fluidized bed granulation. It can be manufactured by a granulation method using an agitating mixer or a granulation method using an extrusion granulator such as an extrusion granulation method.

In the granulation method using a stirring mixer, granulation can be usually performed using 1 to 10% of water, a water-soluble organic solvent or a mixed solvent thereof in a pesticide granule.
Specifically, the pesticidal active ingredient, dextrin and other necessary ingredients are added and uniformly mixed in a stirring mixer. At this time, when the solid component is a lump, it is preferable to pulverize the solid component into a suitable powder to facilitate the mixing operation. An appropriate powder particle size is about 1 to 100 μm. Next, an appropriate amount of water, a water-soluble organic solvent or a mixed solvent thereof is added to the mixture within the range of 1 to 10%, and the mixture is further smoothed in the above-described stirring mixer, and the maximum particle size is reduced. Stir and mix until granules of about 1000 μm are obtained. Further, zeolite and the rest of other components are added to the mixture, and the mixture is taken out when the mixture becomes smooth, and the mixture is sieved to a required particle size classification without drying to obtain a pesticide granule.

In the granulation method using an extrusion granulator, granulation can be performed using 1 to 10% of water, a water-soluble organic solvent, or a mixed solvent thereof in a pesticide granule. Specifically, first, the pesticidal active ingredient, dextrin and other necessary ingredients are uniformly mixed. At this time, when the solid component is a lump, it is desirable to pulverize the solid component to an appropriate particle size in the same manner as in the granulation method using a stirring mixer. Next, an appropriate amount of water, a water-soluble organic solvent or a mixed solvent thereof is added to the mixture in a range of 1 to 10%, and the mixture is kneaded well using a kneading machine such as a double-arm kneader, and is extruded using an extrusion granulator. Granulate. Further, the granules are added with zeolite and, if necessary, the rest of the other components to impart fluidity to the granules, and without drying, sieved to a required particle size to obtain pesticide granules. .

The bulk density of the pesticide granule of the present invention thus obtained is usually from 0.2 to 1.2 g / ml,
Preferably, it is 0.5 to 1.0 g / ml.

The particle size of the pesticidal granules of the present invention varies depending on the type and use of the active ingredient, but is preferably such that it does not powder and easily disintegrates and disperses in water.
5 to 5 mm, preferably 0.1 to 3 mm,
More preferably, it is 0.3 to 1.5 mm.

As the method for spraying the pesticide granules of the present invention, a usual pesticide spraying method can be used. When the agricultural chemical granule of the present invention is used after being diluted with water, it is usually 2 to 20,000.
The spray liquid is adjusted by diluting it about twice, and the spray liquid can be sprayed. Examples of the method of spraying the spray liquid include a method in which the spray liquid is sprayed directly from a bottle made of resin, glass, paper, or the like to a paddy field or a field, a spray method using a sprayer, a jolo, or the like. Further, seed immersion or the like can be performed using the spray liquid.

When the pesticidal granules of the present invention are directly applied without dilution, the amount applied to paddy fields and fields is usually 1
10 to 5000 g per 0 ares, preferably 1
It is 00-3000 g. In this case, there are a method of directly treating soil or paddy fields and a method of treating plant foliage. Furthermore, seed dressing, seedling box treatment, and the like can be performed.

The pesticide granule of the present invention is used to avoid moisture.
It is preferable to store in a moisture-proof container or the like. Examples of such containers include, for example, a material in which resin, aluminum, paper, and the like are bonded as necessary, and a bottle, bag, box, or the like made of a material in which aluminum or silica is deposited on the surface of resin, paper, or the like. It is simple.

Hereinafter, the present invention will be described in more detail with reference to Examples, Comparative Examples, and Test Examples, but the present invention is not limited thereto. The percentages and parts used herein are all percentages and parts by weight unless otherwise specified.

[0048]

【Example】

[0049]

Example 1 Pesticide granules containing 80% mesomil 80 parts mesomil drug substance and 8 parts AMICOL No. 1
(Dextrin, DE17, manufactured by Nisse Chemical Co., Ltd., easily dissolved in water and dissolved in ethylene glycol at about 0.13 g / ml at 20 ° C.) was sufficiently mixed. To 88 parts of this mixture, 2.5 parts of water and 2.5 parts of ethylene glycol were added, and the mixture was stirred at room temperature using a Spartan Luzer 2H (stirring granulator manufactured by Fuji Paudal Co., Ltd.).
The mixture was stirred and granulated until the maximum particle size became about 1000 μm. To the obtained granules, 7 parts of zeolite 3S (Zeolite manufactured by San Zeolite Co., Ltd.) was added and mixed to obtain a pesticide granule of the present invention containing 80% mesomil.

[0050]

Example 2 Pesticide granules containing 45% mesomil 45 parts mesomil bulk, 1 part Neoperex No. 6
F powder (surfactant manufactured by Kao Corporation) 40.9
Two parts of ammonium sulfate (“Industrial Ammonium Sulfate” manufactured by Mitsui Toatsu Chemicals, Inc.) and one part of Nip Seal NS (amorphous silicon dioxide manufactured by Nippon Silica Co., Ltd.) were mixed with Eck Sample Mill KIIW-1 (Fuji Powder). (Hammer mill manufactured by Co., Ltd.). For 87.92 parts of this crushed product,
5 parts of AMICOL No. 3 L (dextrin, DE33, manufactured by Nisse Chemical Co., Ltd., easily dissolved in water and dissolved in ethylene glycol at about 0.15 g / ml at 20 ° C.), 0.03 parts of brilliant blue FCF (Rakuto Chemical Co., Ltd.) Company pigment) and 0.05 parts of Monopet S
OA (sucrose octaacetate manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) was added and mixed well. To 93 parts of this mixture, 3 parts of ethylene glycol were added, and the maximum particle size was about 100 at room temperature using a Spartan Luiser 2H.
The mixture was stirred and granulated until it became a granule of 0 μm. To the obtained granules, 4 parts of zeolite 3S was added and mixed.
% Of the pesticide granules of the present invention.

[0051]

Example 3 Pesticide granules containing 45% mesomil 45 parts mesomil bulk, 1 part Neoperex No. 6
F powder, 39.92 parts of ammonium sulfate and 1 part of nip seal NS were mixed with Ec Sample Mill KIIW-1.
It was ground in a mold. For 86.92 parts of this ground product, 5 parts of AMICOL No. 3 L (dissolves easily in water and dissolves in diethylene glycol at about 0.09 g / ml at 20 ° C.), 0.03 parts of brilliant blue FCF and 0.05 parts of monopet SOA were added and mixed well.
To 92 parts of this mixture, 3 parts of diethylene glycol was added, and using a Spartan Luiser 2H at room temperature,
The mixture was stirred and granulated until the maximum particle size became about 1000 μm. To the obtained granules, 4 parts of zeolite 3S and 1 part of nip seal NS were added and mixed to obtain a pesticide granule of the present invention containing 45% of mesomil.

[0052]

Example 4 Agrochemical Granules Containing 45% Mesomil 45 parts of mesomil drug substance and 1 part of Nipsil NS
It was pulverized with an Ec Sample Mill KIIW-1. For 46 parts of this pulverized product, 5 parts of Paindex # 3 (Dextrin, DE25 manufactured by Matsutani Chemical Industry Co., Ltd.) is easily dissolved in water, and is dissolved in ethylene glycol at about 0.15 g / ml at 20 ° C. ), 39.92 parts of edible lactose (lactose manufactured by Megre Japan Co., Ltd.), 0.03 part of brilliant blue FCF and 0.1% of brilliant blue FCF.
05 parts of monopet SOA were added and mixed well. To 91 parts of this mixture, 1 part of Geropon SDS (a surfactant manufactured by Rhone Poulin Nichika KK), 2 parts of water and 2 parts of ethylene glycol were added, and a double-arm kneader (FM manufactured by Fuji Sangyo KK) was added. -NW), and extruded and granulated with a basket type granulator (RG-5M manufactured by Kikusui Seisakusho) to a particle size of 1.0 mmφ. The obtained granules 96
4 parts of zeolite 3S were added to each part and mixed.
The agricultural chemical granules of the present invention were obtained by sieving the sections of 0 to 1500 µm.

[0053]

Example 5 Pesticide granules containing 45% mesomil 45 parts of mesomil and 1 part of nip seal NS
It was pulverized with an Ec Sample Mill KIIW-1. For 46 parts of this pulverized product, 5 parts of AMICOL No. 1 (dissolve about 0.10 g / ml in dimethyl sulfoxide at 20 ° C.), 40.92 parts of edible lactose,
0.03 parts brilliant blue FCF and 0.05 parts monopet SOA were added and mixed well. To 92 parts of this mixture, 1 part of Newcol 291PG (a surfactant manufactured by Nippon Emulsifier Co., Ltd.) and 3 parts of dimethyl sulfoxide were added, kneaded well in a double-arm kneader, and then using a basket-type granulator. It was extruded and granulated with a particle size of 1.0 mmφ. To 96 parts of the obtained granules, 3 parts of zeolite 3S and 1 part of nip seal NS were added and mixed.
The １1500 μm section was sieved to obtain the pesticide granule of the present invention.

[0054]

Example 6 Pesticide granules containing 50% acephate 50 parts acephate drug substance, 1 part Jeropon SDS,
4 parts of AMICOL No. 3 L and 35.5 parts of ammonium sulfate were mixed well. To 90.5 parts of this mixture, 2.5 parts of diethylene glycol was added, and the maximum particle size was about 100 at room temperature using a Spartan Luiser 2H.
The mixture was stirred and granulated until it became a granule of 0 μm. 6 parts of zeolite 3S and 1 part of nip seal NS are added to the obtained granules.
Was added and mixed to obtain an agricultural chemical granule of the present invention containing 50% of acephate.

[0055]

Example 7 Pesticide granules containing 50% acephate 50 parts of acephate drug substance, 4 parts of AMICOL No. Three
L and 40 parts of sodium benzoate (manufactured by Aioi Kako Co., Ltd.) were thoroughly mixed. To 94 parts of this mixture, 1 part of Newcol 291PG and 3 parts of ethylene glycol were added, kneaded well in a double-arm kneader, and extruded with a basket-type granulator to a particle size of 1.0 mmφ to perform granulation. To 98 parts of the obtained granules, 2 parts of zeolite 3S was added and mixed, and the mixture was sieved in a range of 500 to 1500 μm to obtain an agricultural chemical granule of the present invention containing 50% of acephate.

[0056]

Example 8 Pesticide granules containing 30% hydroxyisoxazole 30 parts of hydroxyisoxazole drug substance, 1 part of Neoperex No. 6F powder, 3 parts of AMICOL No.
1 and 58 parts of sucrose were mixed well. This mixture 92
Parts of ethylene glycol, 2 parts of ethylene glycol was added, and the maximum particle size was about 100 at room temperature using Spartan Luiser 2H.
The mixture was stirred and granulated until it became a granule of 0 μm. 5 parts of zeolite 3S and 1 part of nip seal NS are added to the obtained granules.
Was added and mixed to obtain an agricultural chemical granule of the present invention containing 30% of hydroxyisoxazole.

[0057]

Example 9 Pesticide granules containing 30% of hydroxyisoxazole 30 parts of hydroxyisoxazole drug substance, 1 part of Neoperex No. 6F powder, 5 parts of AMICOL No.
1 and 54.5 parts of edible lactose were mixed well. To 90.5 parts of this mixture, 0.5 parts of Geropon SDS, 2 parts of water and 2 parts of ethylene glycol were added, and the mixture was kneaded well in a double-arm kneader. It extruded and granulated at 0.0 mmφ. To 95 parts of the obtained granules, 5 parts of zeolite 3S was added and mixed, and a 500 to 1500 µm section was sieved to obtain an agricultural chemical granule of the present invention containing 30% of hydroxyisoxazole.

[0058]

Example 10 Pesticide granules containing 30% hydroxyisoxazole 30 parts of hydroxyisoxazole drug substance, 1 part of Neoperex No. 6F powder, 3 parts of AMICOL No.
1 and 58 parts of sucrose were mixed well. This mixture 92
Add 2 parts of water to each part and add Spartan Luiser 2H
And stirred at room temperature until granules having a maximum particle size of about 1000 μm were obtained. To the obtained granules, 5 parts of zeolite 3S and 1 part of Nipsil NS were added and mixed to obtain a pesticide granule of the present invention containing 30% of hydroxyisoxazole.

[0059]

COMPARATIVE EXAMPLE 1 Pesticide granules containing 45% mesomil 45 parts mesomil bulk, 1 part Neoperex No. 6
F powder, 44.92 parts of ammonium sulfate and 1 part of nip seal NS were mixed with Ec Sample Mill KIIW-1.
It was ground in a mold. For 91.92 parts of this ground product, 5 parts of AMICOL No. Add 3 L, 0.03 parts of Brilliant Blue FCF and 0.05 parts of Monopet SOA,
Mix well. To 97 parts of this mixture, 3 parts of ethylene glycol was added, and the mixture was stirred and granulated at room temperature using a Spartan Luiser 2H until granules having a maximum particle size of about 1000 μm, containing 45% mesomil and containing zeolite. A pesticide granule containing no is obtained.

[0060]

COMPARATIVE EXAMPLE 2 Pesticide granules containing 45% mesomil 45 parts mesomil drug substance, 1 part Neoperex No. 6
F powder, 42.42 parts of ammonium sulfate and 1 part of nip seal NS were added to Eck Sample Mill KIIW-1.
It was ground in a mold. With respect to 89.42 parts of the ground product, 5 parts of AMICOL No. Add 3 L, 0.03 parts of Brilliant Blue FCF and 0.05 parts of Monopet SOA,
Mix well. To 94.5 parts of this mixture, 3 parts of ethylene glycol was added, and the mixture was stirred and granulated at room temperature using a Spartan Luiser 2H until the granules had a maximum particle size of about 1000 μm. To the obtained granules, 2.5 parts of nip seal NS were added and mixed to obtain pesticide granules containing 45% mesomil and containing no zeolite.

Next, the quality of the pesticidal granules of the present invention will be specifically shown in Test Examples.

[0062]

[Test Example 1] Consolidation test of agricultural chemical granules In a transparent stoppered glass bottle (7 cm inside diameter, 13 cm height)
The pesticide granules described in Examples 1 to 10 and Comparative Examples 1 and 2 were put so that the height became 6 cm, the surface was flattened, plugged, and left at 40 ° C. for 5 days. The glass bottle was turned over by 180 °, the state of caking of the pesticide granule was observed, and the evaluation was made according to the evaluation criteria in Table 1 below. Table 2 shows the results.

[0063]

[Table 1] Evaluation criteria for consolidation status of pesticide granules ─────────────────────────────────── Evaluation Contents of consolidation of pesticide granules ─────────────────────────────────── − Quiet glass bottle No lumps are observed even if the robot is turned over. + When the glass bottle is turned over, lumps are observed, but they are easily broken and the size is less than 5 mm. ++ When the glass bottle is turned over, a lump is observed, and the lump is relatively hard, and the size is 5 mm or more. ++ The whole contents are solidified and hardly collapse even if the glass bottle is turned over. ───────────────────────────────────

[0064]

Test Example 2 Water disintegration test of pesticide granules 500 g of the pesticide granules described in Examples 1 to 10 and Comparative Examples 1 and 2 were put in an aluminum heat seal bag, and sealed.
Stored in a thermostat at 30 ° C. for 30 days.

Into a 250 ml stoppered cylinder, 250 ml of purified water at 20 ° C. and 3 times hard water each were added, and the above pesticide granules were added to adjust the dilution factor to 250 times. Each time the cylinder was inverted one time (turned 180 degrees and then returned to its original position), the sample was observed for disintegration and the number of times until no granules were observed was measured. Table 2 shows the results.

[0066]

[Test Example 3] Dust scattering test of pesticide granules Pesticide granules 2 described in Examples 1 to 10 and Comparative Examples 1 and 2
0 g is placed in a colorless and transparent glass bottle having a diameter of 9 cm, a height of 18 cm, and an inner volume of 1 liter. Cover, shake vigorously up and down five times, and let it stand still. The time until no longer observed was measured by visual observation. Table 2 shows the results.

[0067]

[Table 2] Consolidation, disintegration in water and dust scattering of pesticide granules ─── Test pesticide No solidified granules are observed and no suspended particles are observed Granules Condition Number of times (times) Time to increase (seconds) ───────────── ───────────────────── Example 1 + 8 2 Example 2-55 Example 3-7 3 Example 4-65 Example 5-8 3 Example 6 + 38 Example 7-8 3 Example 8 + 55 Example 9-65 Example 10-82 2 ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ 比較 比較 Comparative Example 1 +++ 70 Comparative Example 2-830 薬 Pesticide granule of the present invention (Examples 1 to 10) Caking is less likely to occur during storage, it shows excellent water disintegratability, scattering of dust was less. On the other hand, the pesticide granule of Comparative Example 1 containing no zeolite caused caking upon storage. Also, instead of zeolite, a highly water-absorbent nip seal N
In the pesticide granule of Comparative Example 2 using S, dust was easily scattered and dusting of suspended particles was observed for a long time.

[0068]

EFFECTS OF THE INVENTION The pesticide granules of the present invention have no dust at the time of measuring or preparing a drug solution or when directly spraying, and are not only easy to measure and handle, but also can prevent caking during long-term storage. It has the feature of. The pesticidal granules of the present invention are easily disintegrated or dissolved in water, and are convenient preparations to replace conventional powdered aqueous solvents and liquids. Furthermore, the production method of the present invention does not require a heating and drying step, can save a lot of energy and time, and is particularly safe in the production of granules of highly toxic compounds or highly volatile compounds. It has the feature that the workability and workability are greatly improved.

Claims (13)

[Claims] 1. A pesticidal granule comprising a pesticidal active ingredient; dextrin; water, a water-soluble organic solvent or a mixed solvent thereof; and zeolite. 2. The reducing sugar content (DE) of dextrin
The pesticide granule according to claim 1, wherein the content is 5 to 50%. 3. The solubility of dextrin in water, a water-soluble organic solvent or a mixed solvent thereof is 0.05 at 20 ° C.
The pesticide granule according to claim 1 or 2, which is at least g / ml. 4. A water-soluble organic solvent comprising ethylene glycol, diethylene glycol, propylene glycol, N
The pesticide granule according to claim 1 or 2, wherein the pesticide granule is one or more selected from the group consisting of -methyl-2-pyrrolidone, dimethylsulfoxide, and dimethylacetamide. 5. The pesticide granule according to claim 1, wherein the water-soluble organic solvent is ethylene glycol, diethylene glycol or a mixed solvent thereof. 6. The method according to claim 1, further comprising a water-soluble carrier.
The agricultural chemical granule according to any one of the above. 7. The method according to claim 1, further comprising a surfactant.
The agricultural chemical granule according to any one of the above. 8. The pesticide granule according to any one of claims 1 to 7, wherein the pesticidal active ingredient is water-soluble. 9. The method according to claim 1, wherein the pesticidal active ingredient is one or more selected from the group consisting of mesomil, acephate, thiocyclam, hydroxyisoxazole, glyphosate and glufosinate. The pesticide granules according to the above. 10. The pesticide granule according to claim 1, wherein the pesticidal active ingredient is mesomil. 11. The pesticide granule according to any one of claims 1 to 10, wherein the amount of water, a water-soluble organic solvent or a mixed solvent thereof is 0.5 to 10% in the pesticide granule. . 12. A method for producing a pesticidal granule according to claim 1, wherein a composition comprising a pesticidal active ingredient; dextrin; water, a water-soluble organic solvent or a mixed solvent thereof; and zeolite is granulated. 13. The method for producing a pesticide granule according to claim 12, wherein the content of water, a water-soluble organic solvent or a mixed solvent thereof in the composition is 0.5 to 10%.