JP5136099B2 - Composition for agricultural chemical fine granules, fine granular agricultural chemical formulation, and method for producing fine granular agricultural chemical formulation - Google Patents

Description

  The present invention relates to a composition for an agricultural chemical fine granule, a particulate agricultural chemical formulation, and a method for producing a particulate agricultural chemical formulation.

  Conventionally, there are various forms of agrochemical formulations, and agrochemical formulations in a form corresponding to the usage scene are provided. In the case of solid preparations that are directly sprayed as the preparation form, for example, fine granules and fine granules F are known as fine agrochemical preparations in addition to powders and granules. Compared with powders, these fine granular pesticide preparations have 1) a large particle size and therefore less drift outside the target area. 2) Good reachability to the plant stock when sprayed onto rice plants. ) Although there are advantages such as fewer safety problems due to inhalation, adhesion, etc., they are not always satisfactory due to problems such as peeling after production.

Agricultural Chemical Society of Japan Agricultural Chemicals Formulation and Application Method Study Group, “Agricultural Chemicals Formulation Guide”, published by Japan Plant Protection Association

  An object of the present invention is to provide an excellent finely divided pesticide preparation.

  As a result of studies to provide an excellent finely divided pesticide preparation, the present inventors have found that a fine mineral substance carrier having an oil absorption capacity of 1 to 50 ml / 100 g and a particle size of 45 to 212 μm, a particle size of 0.1 to 20 μm. The present invention has found that an excellent fine pesticide formulation can be provided by using a fine powdery pesticide composition and a composition for pesticide fine granules containing a hot-melt binder having a freezing point of 30 to 100 ° C. Invented.

That is, the present invention is as follows [1] to [12].
[1] Oil absorption capacity: 1-50 ml / 100 g, finely divided mineral carrier having a particle size of 45-212 μm, finely powdered agricultural chemical composition having a particle size of 0.1-20 μm, and a freezing point of 30-100 ° C. A composition for agricultural chemical fine granules containing a certain hot-melt binder.
[2] The content of 0.1 to 10 parts by weight of the finely divided pesticide composition and 0.1 to 10 parts by weight of the hot-melt binder with respect to 100 parts by weight of the finely divided mineral substance carrier [1] A composition for fine agricultural chemicals.
[3] The composition for agricultural chemical fine granules according to [1] or [2], wherein the hot-melt binder is polyethylene glycol having a molecular weight of 1000 to 20000.
[4] The composition for fine agricultural chemical granules according to any one of [1] to [3], wherein the particle size of the fine mineral carrier is 45 to 150 μm.
[5] The composition for an agricultural chemical fine granule according to any one of [1] to [4], wherein the fine powdery agricultural chemical composition is a composition containing a bactericidal active compound, an insecticidal active compound and a fine powdered solid carrier.
[6] The composition for agricultural chemical fine granules according to any one of [1] to [4], wherein the finely powdered agricultural chemical composition is a composition containing clothianidin and a finely divided solid carrier.
[7] The composition for an agricultural chemical fine granule according to any one of [1] to [6], wherein the finely divided mineral substance carrier is cinnabar.
[8] The composition for agricultural chemical fine granules according to any one of [1] to [7] is produced with a continuous twin-screw extrusion kneader at a barrel temperature 1 to 10 ° C. lower than the freezing point of the hot-melt binder. The manufacturing method of the fine-grained agricultural chemical formulation which has the process to granulate.
[9] The composition for agricultural chemical fine granules according to any one of [1] to [7] is continuously biaxial at a barrel temperature 1 to 10 ° C. lower than the freezing point of the hot-melt binder under solvent-free conditions. A method for producing a fine pesticide preparation comprising a step of granulating with an extrusion kneader.
[10] Oil absorption capacity: 1-50 ml / 100 g, finely divided mineral carrier having a particle size of 45-212 μm, a hot-melt binder having a freezing point of 30-100 ° C. and a particle size of 0.1-20 μm A particulate pesticide formulation comprising a finely divided pesticide composition.
[11] The finely divided pesticide preparation according to [10], wherein the particle size of the finely divided mineral substance carrier is 45 to 150 μm.
[12] The finely divided pesticide preparation according to [11], wherein the content ratio of the pesticidal fine particles having a particle size of 63 to 212 μm is 90 to 100 weight percent.

  By using the composition for agricultural chemical fine granules of the present invention, an excellent fine granular agricultural chemical formulation can be provided.

  The composition for an agricultural chemical fine granule according to the present invention comprises an oil absorption capacity of 1 to 50 ml / 100 g and a finely divided mineral substance carrier having a particle size of 45 to 212 μm, a fine powdery agricultural chemical composition having a particle size of 0.1 to 20 μm, and And a hot-melt binder having a freezing point of 30 to 100 ° C.

  In the present invention, a mineral carrier in which the oil absorption of linseed oil in the Japanese Industrial Standard (JIS) K-5101 test is about 1 to 50 ml per 100 g of the carrier is used as the fine mineral carrier. Examples of such mineral carriers include cinnabar and calcium carbonate. In the present invention, a mineral carrier having a particle size of substantially 45 to 212 μm, preferably 45 to 150 μm, and more specifically, a mineral having 95% by weight or more of the total amount of the mineral carrier used in the present invention has the aforementioned particle size. A carrier is used.

  The pulverized pesticide composition used in the present invention can use a pulverized pesticidal active ingredient alone, and also includes one pulverized pesticide active ingredient, a pulverized solid carrier and / or one or more other pesticidal active ingredients. It is also possible to use a mixture with a fine powdery pesticide active ingredient. Furthermore, a pulverized mixture obtained by pulverizing a mixture of one kind of pesticidal active ingredient and a solid carrier and / or one or more other pesticidal active ingredients with a jet mill or the like can also be used. As such a finely divided pesticide composition, the particle size is usually 0.1 to 20 μm, preferably about 0.1 to 10 μm, and fine powdery substance, specifically the total amount of the finely divided pesticide composition used in the present invention. A material in which 95% by weight or more is a fine powder substance having the above-described particle size is used. In addition, the average particle diameter measured by laser diffraction type particle diameter measuring apparatuses, such as MASTERSIZER (trademark) 2000 made from MALVERN, is used for this particle size, for example. Examples of the finely divided solid carrier contained in the finely divided pesticide composition include mineral carriers such as kaolin, bentonite, acidic clay, clay, talc, white carbon, calcium carbonate, sodium hydrogen carbonate, sodium sulfate, ammonium sulfate. Inorganic substance powders such as potassium chloride, saccharides such as lactose (lactose), glucose and sucrose, and urea.

  Specific examples of the pesticidal active ingredient contained in the finely divided pesticidal composition used in the present invention include the following pesticidal active ingredients.

Dimethylvinphos, bentiocarb, NAC, MIPC, bensultap, diflubenzfuron, teflubenzfuron, chlorfluazuron, buprofezin, phenoxycarb, pyridaben, clofentezine, hexithazox, fipronil, ethiprole, clothianidin, imidacloprid, thiacloprid, Active insecticidal active ingredients which are solid at 25 ° C. such as cartap hydrochloride, nitenpyram, dinotefuran and acephate;

Thiuram, teclophthalam, carpropamide, diclocimet, tricyclazole, fusaride, cresoxime methyl, trifloxystrobin, metminostrobin, benomyl, triazine, ferimzone, fursulfamide, probenazole, captan, dietofencarb, diclomedin, TPN, iprodione hexapyramedol , Flutranyl, Mepronil, Oxolinic acid, Pyrimethanyl, Mepanipyrim and Validamycin A, etc., solid active ingredients that are solid at 25 ° C.

  In the present invention, a hot-melt binder that is solid at around 20 ° C. and has a freezing point of 30 to 100 ° C. is used as the binder. Examples of the hot-melt binder having a freezing point of 30 to 100 ° C. include polyethylene glycol, paraffin wax, polyethylene polypropylene block polymer, and higher fatty acid (for example, stearic acid). Specific examples of polyethylene glycol include polyethylene glycol having an average molecular weight of about 1000 to 20000. Specific examples include PEG-6000S (freezing point: 62 ° C., average molecular weight: 8300, manufactured by Sanyo Chemical Industries, Ltd.). It is done.

  The composition for an agricultural chemical fine granule of the present invention includes an oil absorption capacity of 1 to 50 ml / 100 g and a finely divided mineral substance carrier having a particle size of 45 to 212 μm, a fine powdery agricultural chemical composition having a particle size of 0.1 to 20 μm, In addition to the hot-melt binder having a freezing point of 30 to 100 ° C., other components can be further contained within a range that does not affect the effects of the present invention. Such other components include surfactants, stabilizers, preservatives, colorants, fragrances and the like.

  Surfactants optionally used in the present invention include ordinary nonionic surfactants, cationic surfactants, anionic surfactants and amphoteric surfactants, one or two of these. More than types are used.

Among such surfactants, specific examples of nonionic surfactants include polyoxyethylene alkyl allyl ether, polyoxyethylene lanolin alcohol, polyoxyethylene alkylphenol formalin condensate, polyoxyethylene sorbitan fatty acid ester, polyoxyglyceryl mono Fatty acid ester, polyoxypropylene glycol mono fatty acid ester, polyoxyethylene sorbitol fatty acid ester, sorbitan fatty acid ester, polyoxyethylene castor oil derivative, polyoxyethylene fatty acid ester, higher fatty acid glycerin ester, sorbitan fatty acid ester, sucrose fatty acid ester, poly Oxyethylene polyoxypropylene block polymers, polyoxyethylene fatty acid amides, alkylolamides and polio Shi polyoxyethylene alkyl amines and the like,
Specific examples of the cationic surfactant include alkylamine hydrochlorides such as dodecylamine hydrochloride; alkyltrimethyl quaternary ammonium salts such as alkyl quaternary ammonium salts and dodecyltrimethylammonium salts; Midinium salts, alkylisoquinolinium salts, dialkylmorpholinium salts, benzethonium chloride, polyalkylvinylpyridinium salts,
Specific examples of the anionic surfactant include fatty acid sodium such as sodium palmitate; sodium ether carboxylate such as sodium polyoxyethylene lauryl ether carboxylate; amino acid of higher fatty acid such as sodium lauroyl sarcosine and sodium N-lauroyl glutamate Condensates; higher alkyl sulfonates; higher fatty acid ester sulfonates such as lauric acid ester sulfonates; dialkyl sulfosuccinate salts such as sodium dioctyl sulfosuccinate; higher fatty acid amide sulfonates such as oleic acid amide sulfonates Dodecylbenzenesulfonate; diisopropylnaphthalenesulfonate; alkylallylsulfonate formalin condensate; alkenylsulfonate; pentadecane-2-sulfate salt, etc. Secondary alcohol sulfate; polyoxyethylene alkyl ether sulfate such as sodium polyoxyethylene dodecyl ether sulfate; polyoxyethylene alkyl phosphate such as dipolyoxyethylene dodecyl ether phosphate; styrene-maleic acid A salt of a polymer; a salt of an alkyl vinyl ether-maleic acid copolymer;
Specific examples of amphoteric surfactants include N-laurylalanine, N, N, N-trimethylaminopropionic acid, N, N, N-trihydroxyethylaminopropionic acid, N-hexyl-N, N-dimethylaminoacetic acid. 1- (2-carboxyethyl) pyridinium betaine.

  Examples of the stabilizer used arbitrarily in the present invention include an epoxy group-containing compound or antioxidant, phosphoric acid, PAP (isopropyl acid phosphate) auxiliary agent, and the like.

  Examples of the compound having an epoxy group include epoxidized vegetable oils, and more specifically, epoxidized drying oils such as epoxidized linseed oil, epoxidized tung oil, and epoxidized eno oil; epoxidized soybean oil, epoxy Epoxidized semi-drying oils such as epoxidized cottonseed oil, epoxidized sesame oil, and epoxidized rapeseed oil; epoxidized non-drying oils such as epoxidized castor oil, epoxidized olive oil, epoxidized camellia oil, epoxidized peanut oil, and epoxidized coconut oil Can be mentioned.

Examples of the antioxidant include dibutylhydroxytoluene (BHT), butylhydroxyanisole (BHA), tetrakis [3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionyloxymethyl] methane (Irganox 1010 ), 2,4,6-tris (3,5-di-tert-butyl-4-hydroxybenzyl) mesitylene (Ionox 330), erythorbic acid, sodium erythorbate, and isopropyl citrate.
Examples of the preservative include butyl paraben, sorbic acid, and potassium sorbate.

As the extender, those having a particle size of about 0.1 to 20 μm are usually used. For example, talc such as talc powder and wax, silicas such as diatomaceous earth powder and mica powder, and clays In addition to mineral powder, calcium carbonate, sulfur powder, and urea powder, there are usual bulking agents used in agricultural chemical formulations. These bulking agents can be used alone or in a mixture of two or more. .
Examples of the colorant include cyanine green, brilliant blue, yellow No. 1 and the like.
Examples of the fragrances include d-limonene.

  The finely divided pesticide preparation of the present invention has an oil absorption capacity of 1 to 50 ml / 100 g and a finely divided mineral substance carrier having a particle size of 45 to 212 μm, a finely divided pesticide composition having a particle size of 0.1 to 20 μm, and a freezing point Can be produced by granulating the composition for agricultural chemical fine granules of the present invention containing a hot-melt binder having a temperature of 30 to 100 ° C. using a continuous twin-screw extrusion kneader. Such a continuous twin-screw extrusion kneader is usually mainly composed of a cylinder called a barrel, a die corresponding to an outlet, and a screw equipped with various screw elements.

  There are usually multiple barrels through which the screw passes. The screw elements include trapezoidal screw elements, trapezoidal cut screw elements, trapezoidal reverse cuts, ball screw elements, kneading paddles (kneading discs) and the like, and combinations thereof can be arbitrarily performed. The composition for agricultural chemical fine granules of the present invention sent into the barrel is moved into the barrel by a screw, processed in the barrel by a screw element such as a kneading paddle, and extruded from a die. . Normally, each barrel and die can be independently temperature controlled.

  In the present invention, a continuous twin-screw extrusion kneader having basic functions such as a raw material conveying function, a mixing function, a shearing function, a compressing function, a pulverizing function, and a heating function that are generally used in the food and plastic fields. If so, it can be used as it is.

  In addition, there are various types of continuous twin-screw extrusion kneaders such as a non-meshing different direction or same direction rotating kneading extruder and a complete or partially meshing type different direction or same direction rotating kneading extruder, In the present invention, a fully meshing type co-rotating continuous biaxial kneader / extruder is preferable, and specific examples include KRC kneader (manufactured by Kurimoto Steel Co., Ltd.).

  The batch processing in the continuous twin-screw kneading extruder does not necessarily have to be performed in all the barrels of the continuous twin-screw kneading extruder. Can be produced. Here, the collective treatment refers to a treatment in which all the components of the composition for an agrochemical fine granule of the present invention are mixed, kneaded and granulated.

Examples of the batch processing method using the continuous twin-screw kneading extruder include the following methods (1), (2), (3) and (4).
(1) Oil absorption capacity 1 to 50 ml / 100 g and a finely divided mineral substance carrier having a particle size of 45 to 212 μm, a finely divided pesticide composition having a particle size of 0.1 to 20 μm, and a freezing point of 30 to 100 ° C. A method in which all raw materials of the composition for agricultural chemical fine granules of the present invention containing a certain hot-melt binder are simply mixed in advance and fed together from the main feed hole of a continuous twin-screw kneading extruder for batch processing. (2) Among the components of the composition for agricultural chemical fine granules according to the present invention, some of the components are mixed in advance, and this is supplied from the main supply hole of the continuous twin-screw kneading extruder to assist the remaining components. 3. Method of batch processing by supplying from the supply hole (3) Among the components of the composition for agricultural chemical fine granules of the present invention, any single component is supplied from the main supply hole of the continuous twin-screw kneading extruder, and the rest (4) Oil absorption capacity 1-50m 1/100 g and a finely divided mineral carrier having a particle size of 45 to 212 μm and a hot melt binder having a freezing point of 30 to 100 ° C. are kneaded by a continuous twin-screw kneading extruder to obtain a fine particle composite. Manufactured, and then premixed again with the continuous biaxial kneading extruder again with the finely divided composite and the remaining components including the finely divided pesticide composition having a particle size of 0.1 to 20 μm, or The main supply hole is the most basic supply hole for supplying the raw material into the barrel. The auxiliary supply hole is a method for supplying auxiliary components and the like. A supply hole other than the main supply hole that can be supplementarily supplied into the barrel.

  Here, all raw materials of the composition for agricultural chemical fine granules of the present invention or a mixture of some of the plural components are kneader mixer, V type mixer, double cone type mixer, cubic type mixer, ribbon It is performed by a machine such as a mold mixer or manually.

  The supply of the raw material into the barrel can be performed manually or by a raw material supply machine generally equipped in the continuous twin-screw kneading extruder to be used, but any apparatus that can supply the raw material at a constant speed. If there is no particular limitation. Examples of such an apparatus include a screw feeder, a table feeder, a slurry feeder, a pressure feeder, a belt conveyor type quantitative feeder, and an electromagnetic feeder.

Next, processing conditions of the continuous twin-screw kneading extruder will be described.
The barrel temperature of a continuous twin-screw kneading extruder is usually controlled by the water temperature of a circulation device that circulates around the barrel disposed in the continuous twin-screw kneading extruder, and the heat melting property used. It can set suitably according to the kind of binder. Usually, among the hot-melt binders having a freezing point of 30 to 100 ° C., the temperature is set to a temperature below the freezing point or 30 ° C. lower than the freezing point, preferably 1 to 10 ° C. lower than the freezing point of the hot-melt binder. Can do. When the continuous twin-screw kneading extruder is composed of a plurality of barrels, all the barrels may have the same barrel temperature, but the composition for agricultural chemical fine granules of the present invention is substantially collectively. If more than one barrel to be processed is the barrel temperature, the remaining barrels may be at a temperature lower than the barrel temperature.

  The number of rotations (processing speed) of the screw can be set as appropriate depending on the model and type of continuous twin-screw kneading extruder, raw materials, screw shape, etc., and within the allowable range of the continuous twin-screw kneading extruder to be used. Can be set. The longer the overall length of the barrel, the higher the processing capability such as mixing and shearing. Therefore, the continuous twin-screw kneading extruder with the longer overall length of the barrel can increase the rotation speed. Specifically, 30 rpm or more is suitable, and 30 to 300 rpm is preferable.

  The shape of the screw element that can be used and the combination thereof can be selected without particular limitation, but it is preferable to use one or more kneading paddles (kneading discs) having a strong kneading action and shearing action.

  The finely divided agricultural chemical formulation of the present invention obtained by the above operation has a high content ratio of agricultural chemical fine particles having a particle size of 63 to 212 μm, and is suitable for a powder agent, in particular, a fine agent F. The finely divided pesticide preparation of the present invention can be applied to a desired particle size distribution such as 90 to 100 percent by weight of the content of pesticide fine particles having a particle size of 63 to 212 μm, for example, by further adjusting the size and sieving as necessary. It can also be set as the fine-grained agricultural chemical formulation.

  Moreover, since the said operation can be performed on substantially solvent-free conditions, the fine-grained agricultural chemical formulation of this invention can be provided, without passing through a drying process etc.

  The finely divided pesticidal composition used in the present invention is usually 0.1 to 10 parts by weight, preferably 0.1 to 5 parts by weight, and 100% by weight with respect to 100 parts by weight of the fine mineral carrier. The active binder is usually contained in an amount of 0.1 to 10 parts by weight, preferably 0.1 to 5 parts by weight, based on 100 parts by weight of the finely divided mineral carrier.

  The content of the composition for agricultural chemical fine granules of the present invention is usually 50 to 99% by weight, preferably 70 to 95% by weight for the finely divided mineral carrier, and 0.1 to 10% by weight for the finely divided agricultural chemical composition. , Preferably 0.2 to 10% by weight, and the hot-melt binder is usually 0.1 to 10% by weight, preferably 0.2 to 5% by weight.

The finely divided pesticide preparation of the present invention may contain, for example, paddy fields, dry fields, nursery boxes, farmland, orchards, mulberry fields, greenhouses, outdoor fields, etc., forests, lawns, golf courses, etc. Can be used in non-agricultural lands such as roadside trees, roads, shoulders, wetlands, ponds, reservoirs, rivers, waterways, sewers, etc., for example, rice, corn, sugar beet, cotton, vegetables (eg cabbage , Chinese cabbage, Japanese radish, cucumber, potato, eggplant), fruit trees (eg, mandarin orange, pear, peach), tea, tobacco, and other target crops can be used to control the pest when applied at the time of occurrence. . Moreover, generation | occurrence | production of a pest can also be prevented over a long period of time by applying to a target crop beforehand.
In using the finely divided pesticide preparation of the present invention, the finely divided pesticide preparation of the present invention can be used alone, but other agents such as pesticide granules, granular fertilizers, granular cultures, granular plants are appropriately used depending on the use. Nutritional agents, granular plant adjustment control agents, granular hormone agents, granular agricultural materials such as seeds, and the like can also be mixed and used.

The finely divided pesticide preparation of the present invention can be applied by a method in which the finely divided pesticide preparation is generally applied, for example, a method of directly spraying by hand, a back-end type duster, a pipe duster, an aerial Examples thereof include a granulator, a power granulator, a seedling box granulator, a tractor-equipped granulator, a multi-hose granulator, a rice transplanter equipped with a granulator, and the like.
When the finely divided agricultural chemical preparation of the present invention is used in paddy fields or upland fields, the application amount is usually 0.1 to 10 kg, preferably 0.25 to 5 kg per 1000 m ² .

For application of the finely divided pesticide preparation of the present invention, the same forms as ordinary pesticide powders and pesticide granules can be applied, for example, foliage application, water surface application, nursery box application, rice planting application, seedling application period, Examples include sowing season application and germination application. When the finely divided pesticide preparation of the present invention is applied to a seedling box (refers to a method of spraying pesticide granules in a seedling box where rice has germinated and grown), the application amount is the seedling box (usually area) (Approx. 0.16 m ² ) per sheet is usually 5 to 300 g, preferably 25 to 100 g. The application method at that time is, for example, a method of direct application by hand and a seedling box granulator. The method of doing is mentioned.
Further, when the fine pesticide preparation of the present invention is applied during the sowing period, for example, when creating a nursery bed, a layer of the seed and the fine pesticide preparation of the present invention is formed between the floor soil and the covering soil. The finely divided pesticide preparation of the present invention is applied to. Such a nursery is usually prepared in a nursery box, and its application rate is usually 5 to 300 g, preferably 25 to 100 g per nursery box (usually about 0.16 m ² ). Examples of the application method at that time include a method of direct application by hand and a method of application using a seeder with a hopper.

  EXAMPLES Hereinafter, although this invention is demonstrated in detail by Examples, such as a manufacture example and a test example, this invention is not limited only to these examples.

  First, formulation examples of the fine particulate pesticide formulation of the present invention are shown. In addition, a part shows a weight part.

Formulation Example 1
1 part of polyethylene glycol (trade name: PEG-6000S, manufactured by Sanyo Chemical Industries Co., Ltd.) and 25 parts of cinnabar sand (manufactured by Neolite Kosan Co., Ltd.) are placed in a polyethylene bag and mixed manually, and the mixture is mixed with KRC kneader (model number S1). , Manufactured by Kurimoto Seiko Co., Ltd.) at a feed rate of 27.1-36.9 g / min, kneaded and extruded under conditions of a rotation speed of 200 rpm and a barrel temperature of 55.1-56.8 ° C. A shaped complex was obtained. Next, 95.56 parts of this finely divided composite, 2.14 parts of ferrimzone jet mill pulverized product (average particle size 5 μm; hereinafter referred to as ferrimzone pulverized product), and fusalide jet mill pulverized product (average particle size 4 μm; Hereinafter, referred to as pulverized fusalide.) 1.56 parts, and a turbo mill of a mixture of clothianidin and granule clay (trade name: Katsuyama Clay S, manufactured by Katsuyama Mining Co., Ltd.) in a weight ratio of 7: 3 0.74 parts of dry pulverized product (average particle size 15 μm, hereinafter referred to as clothianidin / clay pulverized mixture) was placed in a polyethylene bag and mixed manually, and the mixture was mixed with KRC kneader (model number S1, Kurimoto Seiko Co., Ltd.). From the supply hole of the factory) at a supply rate of 30.5 to 37.4 g / min, and kneaded and extruded under conditions of a rotation speed of 50 rpm and a production temperature of 56.9 to 57.2 ° C. Particulate pesticide formulation (hereinafter, referred to as the present pesticidal formulation (1).) Was obtained.

Formulation Example 2
2.14 parts of ferrimzone pulverized product, 1.56 parts of pulverized fusaride, 0.74 part of clothianidin / clay pulverized mixture, 3.68 parts of polyethylene glycol (trade name: PEG-6000S, manufactured by Sanyo Chemical Industries, Ltd.), silica sand ( 91.88 parts (manufactured by Neolite Kosan Co., Ltd.) are manually mixed using a polyethylene bag, and the mixture is supplied at a feed rate of 30.5 to 34 from the feed hole of KRC kneader (model number S1, manufactured by Kurimoto Steel Works). .4 g / min, kneaded and extruded under the conditions of a rotation speed of 50 rpm and a barrel temperature of 57.0 to 57.2 ° C., and the fine agrochemical formulation of the present invention (hereinafter referred to as the present agrochemical formulation (2)). Got.

Formulation Example 3
1 part of polyethylene glycol (trade name: PEG-6000S, manufactured by Sanyo Chemical Industries Co., Ltd.) and 25 parts of calcium carbonate (trade name: Kansui # 65150-K, manufactured by Nitto Flour Chemical Co., Ltd.) are placed in a polyethylene bag for manual work. The mixture is fed at a feed rate of 32.5 to 33.8 g / min from a feed hole of a KRC kneader (model S1, manufactured by Kurimoto Steel Co., Ltd.), with a rotation speed of 200 rpm and a barrel temperature of 56.4 to The mixture was kneaded and extruded under the condition of 57.3 ° C. to obtain a fine particle composite. Next, 95.56 parts of this finely divided composite, 2.14 parts of ferrimzone pulverized product, 1.56 parts of fusalide pulverized product, and 0.74 part of clothianidin / clay pulverized mixture are placed in a polyethylene bag and mixed manually. The mixture is supplied at a supply speed of 31.6 to 33.0 g / min from a supply hole of a KRC kneader (model S1, manufactured by Kurimoto Steel Works, Inc.), and has a rotation speed of 50 rpm and a barrel temperature of 56.9 to 57.8. The mixture was kneaded and extruded under the condition of ° C. to obtain a finely divided pesticide preparation of the present invention (hereinafter referred to as the present pesticide preparation (3)).

Formulation Example 4
1 part of polyethylene glycol (trade name: PEG-6000S, manufactured by Sanyo Chemical Industries, Ltd.) and 25 parts of cinnabar (manufactured by Neolite Kosan Co., Ltd.) are placed in a polyethylene bag and mixed manually, and the mixture is mixed with a KRC kneader (model number S2). , Manufactured by Kurimoto Seiko Co., Ltd.) and supplied at a feed rate of 172 to 266 g / min, and kneaded and extruded under conditions of a rotation speed of 100 rpm and a barrel temperature of 57 ° C. to obtain a fine particle composite. Next, 95.46 parts of this fine-grained composite, 2.14 parts of ferrimzone pulverized product, 1.56 parts of pulverized fusaride, 0.74 part of clothianidin / clay pulverized mixture, and sodium dioctyl sulfosuccinate (trade name: New Calgen) EX-70 (manufactured by Takemoto Yushi Co., Ltd.) 0.1 parts in a polyethylene bag and mixed manually, and the mixture is fed from a feed hole of a KRC kneader (model number S2, Kurimoto Steel Co., Ltd.) at a feed rate of 113. It was supplied at ˜263 g / min, and kneaded and extruded under conditions of a rotation speed of 100 rpm and a barrel temperature of 58 ° C. to obtain a finely divided pesticide preparation of the present invention (hereinafter referred to as the present pesticide preparation (4)).

  The particle size distribution (unit: weight percent) and oil absorption capacity of cinnabar and calcium carbonate used in Formulation Examples 1 to 4 are as shown in [Table 1].

  Next, test examples are shown.

Ａ₁：供試前の農薬有効成分含量（重量％）
Ａ₂：供試後の農薬有効成分含量（重量％）

その結果を、〔表２〕に示す。 Test example 1
Each of the agricultural chemical formulations (2) to (4) of the present invention was sieved with a sieve having openings of 212 μm and 63 μm. A filter containing 10 g of the test fine granular pesticide preparation (10 g) after measuring the content of each pesticide active ingredient of 10 g of the test fine granule pesticide preparation that passed through the sieve having an opening of 212 μm and not passed through the sieve of 63 μm ( The glass filter (11G-2) was placed so as to be flat on a glass filter (11G-2) having a diameter of 40 mm), and aerated for 2 minutes from the bottom of the glass filter at an air volume of 30 liters / minute. Thereafter, the test fine granular pesticide preparation in the glass filter was recovered, the pesticide active ingredient content was measured, and the peel rate was determined by the following formula (A).

A ₁ : Agrochemical active ingredient content (% by weight) before the test
A ₂ : Pesticide active ingredient content after test (wt%)

The results are shown in [Table 2].

Test example 2
Each of the agricultural chemical formulations (1) to (4) of the present invention was sieved with a sieve having openings of 212 μm and 63 μm. The content ratio (weight ratio) of fine pesticidal fine particles that do not pass through a sieve having an aperture of 212 μm in the test pesticidal formulation was measured, and the production efficiency of the pesticidal fine particles during granulation was evaluated in six stages as follows.

Manufacturing efficiency evaluation Evaluation criteria
(Content ratio of fine agricultural chemical particles that do not pass through a sieve having an aperture of 212 μm)
++: Less than 10% by weight ++: 10-20% by weight
+: 20 to 40% by weight
−: 40 to 60% by weight
-: 60 to 80% by weight
---: Over 80% by weight

The results are shown in [Table 3].

  As is clear from the results of Test Example 1, it can be confirmed that the finely divided pesticide composition of the present invention has a good property in which the peel rate of each pesticidal active ingredient after production is suppressed to less than 10 percent. . Further, from the results of Test Example 2, particularly when a finely divided mineral carrier having an oil absorption capacity of 1 to 50 ml / 100 g and a particle size of 45 to 150 μm is used, a particle size distribution suitable for a fine granule, specifically 63 μm to It can be confirmed that a fine granular agricultural chemical composition containing a large amount of agricultural chemical fine particles having a particle diameter of 212 μm can be easily provided.

Claims (12)

  Oil absorption capacity: 1-50 ml / 100 g, finely divided mineral substance carrier having a particle size of 45-212 μm, fine powdery pesticide composition having a particle size of 0.1-20 μm, and hot melting having a freezing point of 30-100 ° C. A composition for an agrochemical granule containing a sex binder.   The fine agricultural chemical composition according to claim 1, wherein the fine powdery agricultural chemical composition is contained in an amount of 0.1 to 10 parts by weight and the hot-melt binder 0.1 to 10 parts by weight with respect to 100 parts by weight of the finely divided mineral carrier. Pharmaceutical composition.   The composition for agricultural chemical fine granules according to claim 1 or 2, wherein the hot-melt binder is polyethylene glycol having a molecular weight of 1,000 to 20,000.   The composition for an agrochemical granule according to any one of claims 1 to 3, wherein the particle size of the fine mineral substance carrier is 45 to 150 µm.   The composition for an agricultural chemical fine granule according to any one of claims 1 to 4, wherein the fine powdery agricultural chemical composition is a composition containing a bactericidal active compound, an insecticidal active compound and a fine powdered solid carrier.   The composition for fine agricultural chemical granules according to any one of claims 1 to 4, wherein the fine powdery agricultural chemical composition is a composition containing clothianidin and a fine powder solid carrier.   The composition for fine agricultural chemicals according to any one of claims 1 to 6, wherein the finely divided mineral carrier is cinnabar.   A process for granulating the composition for agricultural chemical fine granules according to any one of claims 1 to 7 with a continuous twin-screw extrusion kneader at a barrel temperature 1 to 10 ° C lower than the freezing point of the hot-melt binder. A method for producing a finely divided pesticide preparation.   A composition for agricultural chemical fine granules according to any one of claims 1 to 7 is produced in a continuous twin-screw extrusion kneader at a barrel temperature 1 to 10 ° C lower than the freezing point of the hot-melt binder under solvent-free conditions. The manufacturing method of the fine-grained agricultural chemical formulation which has the process to granulate.   Oil-absorbing ability 1-50ml / 100g and fine-grained agrochemicals having a solidification point of 30-100 ° C and a finely divided pesticide having a particle size of 0.1-20µm A fine pesticide formulation comprising a composition.   The fine particle agricultural chemical formulation according to claim 10, wherein the particle size of the fine mineral substance carrier is 45 to 150 µm.   The fine-grained agricultural chemical formulation according to claim 11, wherein the content ratio of the agricultural chemical fine particles having a particle size of 63 to 212 µm is 90 to 100 percent by weight.