JP2011006396A - Elution-regulating type agrochemical composition, and agrochemical granule - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide agrochemical granules containing a highly water-soluble agrochemical active ingredient, maintaining the elution of the chemical for a long period of time while keeping a sufficient elution efficiency of the chemical, and in addition the inexpensive and easily producible agricultural granules showing the chemical elution-regulating effect and also showing quick sinking property in water at their spraying application on water-filled fields such as the paddy fields of paddy rice cultivation, and also a method for producing the same, avoiding the decomposition of the thermally unstable agrochemical active ingredient in its production processes.SOLUTION: This agrochemical composition comprises (a) the agrochemical active ingredient, (b) a fatty acid and/or fatty acid derivative, (c) hardly water-soluble polysaccharides and (d) an inorganic substance. Further the agrochemical granules are obtained by mixing the agrochemical composition and then granulating.

Description

  The present invention relates to an agrochemical granule for efficiently controlling pests generated in paddy fields. Specifically, the present invention relates to an agrochemical active composition containing an agrochemical active ingredient, a fatty acid and / or a fatty acid derivative, a poorly water-soluble polysaccharide, and an inorganic substance, and further relates to an agrochemical granule obtained by granulating this. The present invention relates to an agrochemical granule that controls the elution of active ingredients with high water solubility, lengthens the elution period, reduces the number of spraying, and saves labor. In addition, by adding a surfactant to the agrochemical granule and / or coating the surface of the agrochemical granule obtained by extrusion granulation, the lightness of the specific gravity of the fatty acid derivative and water repellent to the water surface of the grain The present invention relates to an agrochemical granule that exhibits uniform efficacy by preventing the localization of the granule by flowing water and wind and the runoff from paddy fields that occur as a result of ascent.

  In recent years, the aging of farmers has become more and more serious, and labor saving of farm work has been demanded. Along with this, techniques related to labor-saving spray formulations and spraying methods for agricultural chemicals are being studied. Furthermore, from the viewpoint of reducing the environmental burden, it is desirable to reduce the amount and number of use of agricultural chemicals and accelerate the use period. In response to these requests, agrochemical granules have been developed for the purpose of controlling the elution of pesticide active ingredients and extending the elution period so that the drug can be eluted for a long period of time in a single application of pesticide. . Therefore, it is necessary to develop a formulation technology that controls the dissolution rate of agricultural chemical active ingredients in soil and water. Has been developed. Among these, dissolution controlled preparations using fatty acids and / or fatty acid derivatives and various waxes are known. For example, Patent Document 1 discloses a herbicidal granule comprising a sulfonylurea herbicide, activated carbon, paraffin wax, and a mineral carrier. Patent Document 2 discloses an agrochemical granule characterized by containing an alcohol type wax. Furthermore, Patent Document 3 discloses an agrochemical granule characterized by containing a montan wax derivative mixture.

JP 63-35504 A Japanese Patent Laid-Open No. 11-292706 JP 2000-351705 A

However, the elution controlled agrochemical granules shown in Patent Documents 1 to 3 cannot maintain long-lasting elution and cannot obtain a sufficient biological effect. Or the elution efficiency of active ingredients of agricultural chemicals is not enough, and some or much of the drug remains in the agricultural chemical granules, so that sufficient elution for obtaining a biological effect at a certain application rate cannot be obtained. was there. Moreover, in order to control the elution of a pesticidal active ingredient having high water solubility for a long period of time, it is necessary to increase the proportion of wax in the pesticidal granules. When such pesticide granules are used under paddy field flooding after rice planting, the grains float on the water surface due to their low specific gravity and water repellency, and due to variations in the distribution of agricultural chemical formulations due to water flow and the loss of drugs Becomes insufficient. In addition, it is localized in a certain part of the rice field under the influence of the wind, which may cause not only a uniform effect but also phytotoxicity. Furthermore, the manufacturing method of the agrochemical granule which uses the fatty acid and / or fatty acid derivative of Patent Documents 1 to 3 as a base material, after heating and melting the base material fatty acid and / or fatty acid derivative and the pesticidal active ingredient, It is obtained by crushing and granulating the cooled and solidified material. However, when an agrochemical active ingredient that is decomposed by heat is used, it cannot be produced by a production method including the heating and melting step as described above. On the other hand, when the fatty acid and / or fatty acid derivative and the agrochemical active ingredient are directly mixed in the solid state and extrusion granulation is carried out without passing through the heating step, the resulting particles have low hardness, and the particles are cracked or chipped during storage and transportation. By doing so, there is a possibility that the total surface area of the granule increases and the desired elution rate cannot be obtained.
An object of the present invention is to provide a pesticide granule containing a pesticide active ingredient having high water solubility, a pesticide composition capable of maintaining elution of the drug for a long time while maintaining sufficient elution efficiency of the drug, and a pesticide granule using the same Is to provide. In addition to providing a low-priced and easy-to-manufacture agricultural chemical granule that exhibits the above-described drug elution control effect when sprayed on a flooded field, such as paddy field for paddy rice cultivation, and a manufacturing process It is an object of the present invention to provide a pesticidal granule having sufficient hardness by a production method capable of avoiding decomposition of a thermally unstable pesticidal active ingredient.

  As a result of studies using various base materials, extenders and excipients that can be used in agricultural chemical granules, the present inventors have found that the agricultural chemical active ingredient (a), fatty acid and / or fatty acid derivative (b), poorly water-soluble A composition for agrochemical granules containing a polysaccharide (c) and an inorganic substance (d), and an agrochemical granule formed by granulating the composition, elutes a pesticide active ingredient with high water solubility under paddy paddy water for a long time. I found that I can control. Also, it has been found that by adding a poorly water-soluble polysaccharide (c), it is possible to form granules by extrusion granulation alone without going through a heating and melting step, and to produce agricultural chemical granules having sufficient hardness. It was. Furthermore, the present inventors have found a prescription that can more effectively suppress the floating of agricultural chemical granules caused by fatty acids to be used, and can prevent the localization of the agricultural chemical granules in paddy fields and the runoff from paddy fields. That is, it is an agrochemical granule obtained by granulating a composition for an agrochemical granule obtained by mixing an agrochemical active ingredient and other raw materials with an extrusion granulator, and further derived from a fatty acid derivative by adding a surfactant. It is an agrochemical granule which can suppress the floating of the grain to the water surface by water repellency. In addition, the poorly water-soluble polysaccharides, inorganic substances, and surfactants added in some cases have the effect of adjusting the dissolution of the agricultural chemical active ingredient into water, and depending on the type and amount of the compound, Elution characteristics can be controlled freely. The agrochemical granule according to the present application controls the elution of an agrochemical active ingredient having a high water solubility and lengthens the elution period, thereby reducing the number of spraying and enabling labor saving.

  The agrochemical composition of the present invention adjusts various types of fatty acids and / or fatty acid derivatives, poorly water-soluble polysaccharides, inorganic substances, combinations and contents of inorganic substances, and types and contents of surfactants. Can control the elution rate of various agrochemical active ingredients. As a result, it is possible to design a preparation according to the optimum concentration of the pesticidal active ingredient to be used, the target pest, the spraying time, and the action period, and as a result, the efficacy of the pesticidal active ingredient to be used is fully exhibited. Moreover, the sedimentation property to paddy water is also good, there is no runaway and localization from the paddy field, and as a result, it can be used as an excellent pesticide granule having no phytotoxicity to crops. Furthermore, the agrochemical composition according to the present application does not require a heat-melt mixing step, is a composition that can be easily mixed in the preparation of a granule, and has excellent granule moldability, while ensuring sufficient granule hardness. is there.

The agrochemical composition of the present invention, the agrochemical granule using the agrochemical composition, and the method for producing the agrochemical granule will be described in more detail below.
The pesticidal active ingredient (a) used in the pesticidal composition of the present invention may be any pesticidal active ingredient or pesticidal active ingredient, and is basically not limited. Among these, pesticidal active ingredients having high solubility in water are particularly suitable. Specifically, the water solubility at 20 ° C. is 100 ppm or more, and the water solubility is in the range of 0.01 to 50% by weight, and it can be suitably used for an agrochemical active ingredient having high water elution. Specific examples of the agrochemical active ingredient include, but are not limited to, the following.
Examples of the agrochemical insecticidal active ingredient include 1,3-dicarbamoylthio-2- (N, N-dimethylamino) -propane hydrochloride (cartap hydrochloride), 5-dimethylamino-1,2,3-trithianshu Nereistoxin insecticides such as acid salts (thiocyclam oxalate), S, S′-2-dimethylaminotrimethylene-di (benzenethiosulfonate) (bensultap); 1- (6-chloro-3 -Pyridylmethyl) -N-nitroimidazolidin-2-ylideneamine (imidacloprid), 3- (2-chloro-1,3-thiazol-5-ylmethyl) -5-methyl-1,3,5-oxadiazinan-4-ylidene ( Nitro) amine (thiamethoxam), (E) -1- (2-chloro-1,3-thiazol-5-ylmethyl) -3-methyl-2-nitrog Anidine (clothianidin), (RS) -1-methyl-2-nitro-3- (tetrahydro-3-furylmethyl) guanidine (dinotefuran), 3- (6-chloro-3-pyridylmethyl) -1,3-thiazolidine -2-Iridenecyanamide (thiacloprid), (E) -N- (6-Chloro-3-pyridylmethyl) -N-ethyl-N'-methyl-2-nitrovinylidenediamine (Nitenpyram), (E) -N -Neonicotinoid insecticides such as [(6-chloro-3-pyridyl) methyl] -N′-cyano-N-methylacetanidin (acetamipride); S-methyl-N-[(methylcarbamoyl) oxy] Carbamate insecticides such as thioacetimidate (mesomyl), 2-secondary butylphenyl-N-methyl carbamate (BPMC), and E)-4,5-dihydro-6-methyl-4- (3-pyridylmethylene amino) -1,2,4-triazine -3 (2H) - one (pymetrozine) and the like.
Examples of agricultural chemical bactericidal active ingredients include 3-allyloxy-1,2-benzisothiazole-1,1-dioxide (provenazole), 1,2,5,6-tetrahydropyrrolo [3,2,1-ij] quinoline. -4-one (pyroxylone), (E) -2-methoxyimino-N-methyl-2- (2-phenoxyphenyl) acetamide (methinostropine), 5-methyl-1,2,4-triazolo [3 4-b] benzothiazole (tricyclazole), 3′-chloro-4,4′-dimethyl-1,2,3-thiadiazole-5-carboxanilide (thiazinyl), [5-amino-2-methyl-6- (2 , 3,4,5,6-pentahydroxycyclohexyloxy) tetrahydropyran-3-yl] amino-α-iminoacetic acid (generic name: kasugamycin) It is. Among these, the present invention is suitable for preparing an elution-controlled pesticide granule for nereistoxin pesticide active ingredients. Or it is suitable also for the purpose of preparing the elution control type agricultural chemical granule of a neonicotinoid type agricultural chemical active ingredient. More preferred as the pesticidal active ingredient are thiocyclam oxalate, imidacloprid, and thiamethoxam. These agrochemical active ingredients may be used alone or in combination of two or more in the agrochemical granule of the present invention.

In addition to the nereistoxin pesticide active ingredient and the neonicotinoid pesticide active ingredient, the following pesticide active ingredients are also chemically active against the nereistoxin and neonicotinoid pesticide active ingredients in the composition of the present invention. One or more types can be used in combination as long as they do not affect the stability of the product. Specific examples include the following, but are not limited thereto. For example, pesticidal active ingredients include BPMC (2-sec-butylphenyl-N-methylcarbamate), MIPC (2-isopropylphenyl-N-methylcarbamate), NAC (1-naphthyl-N-methylcarbamate), pyraclophos (( RS)-[O-1- (4-chlorophenyl) pyrazol-4-yl] -O-ethyl-S-propyl-phosphorothioate), buprofezin (2-tert-butylimino-3-isopropyl-5-phenyl-3,4 , 5,6-tetrahydro-2H-1,3,5-thiadiazin-4-one), flucitrinate ((RS) -α-cyano-3-phenoxybenzyl- (S) -2- (4-difluoromethoxy) Phenyl) -3-methylbutyrate), mesomil (S-methyl-N-[(methylcarbamoyl)) Xy] thioacetimidate), etofenprox (2- (4-ethoxyphenyl) -2-methylpropyl-3-phenoxybenzyl-ether), XMC (3,5-xylyl-N-methylcarbamate), etc. It is done.
Bactericidal active ingredients include IBP (O, O-diisopropyl-S-benzylthiophosphate), tricyclazole (5-methyl-1,2,4-triazolo [3,4-b] benzothiazole), and fusalide (4,5 , 6,7-tetrachlorophthalide), validamycin, probenazole (3-allyloxy-1,2-benzisothiazole-1,1-dioxide), ferimzone ((Z) -2′-methylacetophenone = 4,6- Dimethylpyrimidin-2-ylhydrazine), flutolanil (α, α, α-trifluoro-3'-isopropoxy-O-toluanilide), furametopyl ((RS) -5-chloro-N- (1,3-dihydro-) 1,1,3-trimethylisobenzofuran-4-yl) -1,3-dimethylpyrazole-4-carboxamide, pe Cyclone (1- (4-chlorobenzyl) -1-cyclopentyl-3-phenylurea, dichromedin (6- (3,5-dichloro-4-methylphenyl) -3 (2H) -pyridazinone), kasugamycin monohydrochloride, etc. Is mentioned.

  The content ratio of the pesticidal active ingredient (a) in the pesticidal composition of the present invention is usually 3 to 25% by mass, preferably 4 to 15% by mass. When the content in the agrochemical composition is less than 3% by mass, sufficient efficacy of the agrochemical active ingredient cannot be expected, and when it exceeds 25% by mass, the elution of the agrochemical active ingredient into water cannot be controlled sufficiently. Therefore, long-term aftereffects cannot be expected.

In the agrochemical composition of the present invention, fatty acid and / or fatty acid derivative (b) is applied as one of the preparation bases. The fatty acids and fatty acid derivatives are excellent in processability, and can be prepared into granules having a desired particle size and length by mixing and extrusion granulation without passing through a heating step such as melting. Therefore, the agrochemical granule can be produced without going through the step of heating and melting the fatty acid and / or fatty acid derivative and the agrochemical active ingredient and other raw materials, and can be applied to the agrochemical active ingredient which is unstable to heat. The fatty acid and fatty acid derivative that can be used in the present invention can be used without particular limitation as long as they are inactive even if they are active as an agrochemical active ingredient.
Fatty acids and fatty acid derivatives suitable for the present invention are C8-C40 alkyl chain carboxylic acids and derivatives thereof. More preferred are C10-C30 alkyl chain carboxylic acids and derivatives thereof. These fatty acids and fatty acid derivatives are generally solid at room temperature and can be applied as a granule base material impregnated and held with an agrochemical active ingredient. Considering the processability in the preparation of granules, those having physical properties in which the melting point of the fatty acid and fatty acid derivative is in the range of 45 to 100 ° C. can be used particularly suitably. More preferably, it is possible to prepare granules having excellent physical properties of fatty acids and fatty acid derivatives having a melting point in the range of 50 to 90 ° C.
Examples of fatty acids include stearic acid, myristic acid, behenic acid, palmitic acid, and lauric acid. Examples of fatty acid derivatives include 12-hydroxystearic acid. Furthermore, wax-like substances obtained by hydrogenating fatty acid esters such as animal fats and vegetable oils such as cow oil, castor oil, soybean oil, palm oil, and rapeseed oil are also included. One or a mixture of two or more selected from the above can be used in any combination. Among these fatty acids and fatty acid derivatives, castor hydrogenated oil alone, a combination of beef hydrogenated oil and stearic acid, and a combination of castor hydrogenated oil and stearic acid are preferable because they exhibit good dissolution properties of the agrochemical active ingredient. Furthermore, granulation property can be improved by adding room temperature liquid vegetable oils such as castor oil, rapeseed oil, palm oil, soybean oil, cottonseed oil and linseed oil as appropriate.
The fatty acid and / or fatty acid derivative can be contained in the agrochemical granule of the present invention in a proportion of 10 to 80% by mass. Preferably it is 20-70 mass%. If it is less than 10 mass%, the elution control effect by a fatty acid and a fatty acid derivative cannot be expected, and it becomes difficult to form the shape of an agrochemical granule. On the other hand, if it exceeds 80% by mass, the pesticidal active ingredient is not sufficiently dissolved in water and remains in the granule, so that there is a possibility that sufficient effects cannot be exhibited. In the agrochemical granule according to the present invention, when the content of fatty acid and / or fatty acid derivative is increased, a granule in which the drug elution rate is controlled slowly can be prepared. On the contrary, if the content of fatty acid and / or fatty acid derivative is decreased, a granule showing a fast drug elution pattern can be prepared.

The invention according to the present application is the result of carrying out diligent studies with the object of producing and finding a granule having sufficient hardness without going through a heating and melting step, while using a fatty acid and / or a fatty acid derivative as a preparation base, It was found that a poorly water-soluble polysaccharide (c) added to an agrochemical active ingredient and a fatty acid and / or a fatty acid derivative and mixed well can be granulated with an extrusion granulator and exhibited desirable physical properties as an agrochemical granule. By adding a poorly water-soluble polysaccharide to a fatty acid and / or fatty acid derivative, a granule having sufficient hardness was obtained only by compression by extrusion granulation without giving a compression moldability and passing through a melt mixing step. . In addition, poorly water-soluble polysaccharides form a network in the agricultural chemical granules based on fatty acids and / or fatty acid derivatives to increase the hardness of the grains, and at the same time, adjust the elution of agricultural chemical active ingredients from the inside of the grains into water. There is work to do.
The poorly water-soluble polysaccharide (c) applied to the agrochemical composition of the present invention can improve the granulation properties by extrusion granulation, and impairs the stability of the agrochemical active ingredient in the agrochemical granule. Specific examples include crystalline cellulose, water-insoluble pectin, and chitin / chitosan. A poorly water-soluble polysaccharide having an average particle size of 1 μm to 45 μm is suitable for the agricultural chemical composition of the present application, and is essential for obtaining a drug elution control type granule having desirable characteristics. The average particle size is preferably 1 μm to 30 μm, and more preferably the average particle size is 5 μm to 20 μm. Usually, as the content of the poorly water-soluble polysaccharide increases, the dissolution rate of the agrochemical active ingredient in water increases. Sufficient hardness can be given to the said agrochemical granule by using 0.5-20 mass% of poorly water-soluble polysaccharides. If it is less than 0.5% by mass, the compression-forming property and hardness due to the poorly water-soluble polysaccharide cannot be provided. Moreover, when it exceeds 20 mass%, it will become difficult to shape | mold into the shape as an agrochemical granule.

The agrochemical composition of the present invention contains an inorganic substance (d). The pesticide composition has a base material of a fatty acid and / or a fatty acid derivative having a specific gravity close to 1, and floats on the water surface when sprayed on a flooded field due to the specific gravity and water repellency derived from the base material. The floating particles are not only localized in a part of the field under the influence of the wind and become non-uniform in effectiveness, but also run away from the field under the influence of the water flow and may not exhibit the expected effect. . In order to prevent a decrease in efficacy due to light specific gravity, the agrochemical composition contains an inorganic substance. When the agrochemical granule according to the present invention is sprayed on a flooded field, it is possible to greatly adjust the specific gravity of the agrochemical granule by the magnitude of the specific gravity of the inorganic substance, improving the sedimentation property in water and promptly submerging in water. The function to perform is given. In addition, the inorganic substance also has a role of appropriately adjusting the elution of the pesticidal active ingredient existing in the grain into water by roughening the internal structure of the pesticidal granule.
The inorganic substance used in the present invention is clay, silica, talc, white clay, diatomaceous earth, ashment, amorphous silicon dioxide (common name: white carbon), barium sulfate, titanium dioxide, sodium chloride, potassium chloride, dihydrate gypsum, semi-solid Although it is used by 1 type, or 2 or more types of combinations chosen from a water gypsum etc., if it does not impair the stability of an agrochemical active ingredient, it will not restrict to this. Various inorganic particle diameters can be used. Among them, those having a particle size of 20 μm to 200 μm are preferable for deriving the effect of promoting the elution of the agrochemical active ingredient in production and / or agricultural chemicals.
The said inorganic substance can be contained in the ratio of 10-60 mass% in the agrochemical granule of this invention. More preferably, it contains 20 to 50% by weight. If it is less than 10% by mass, the effect of adjusting the specific gravity cannot be expected. If it exceeds 60% by mass, it becomes difficult not only to control the elution of the pesticidal active ingredient but also to form it into a shape as an agrochemical granule.

The agrochemical composition of the present invention preferably contains a surfactant (e). As the surfactant, a nonionic and / or anionic surfactant is applied. When an anionic surfactant and / or a nonionic surfactant is sprayed with an agrochemical granule according to the present invention in a flooded field, the water repellency of the agrochemical granule of the present invention is suppressed due to its water affinity. It improves the sedimentation property and imparts a function to quickly settle in water. The surfactant used in the present invention also has a role of increasing the hydrophilicity of the agrochemical granule and appropriately adjusting the elution of the agrochemical active ingredient present in the grain into water.
Nonionic surfactants used in the present invention include polyoxyethylene alkyl ether, polyoxyethylene styryl phenyl ether, polyoxyethylene alkyl ester, polyoxyethylene phenyl ether polymer, polyoxyethylene alkylene aryl phenyl ether, polyoxyethylene poly Examples include an oxypropylene block polymer, polyoxyethylenated castor oil, polyoxyethylenated hydrogenated castor oil, glyceryl monostearate, glyceryl distearate, and polyoxyethylene sorbitan monooleate. Animates such as oxyethylene styryl phenyl ether sulfate, lignin sulfonate, alkyl aryl sulfonate, alkyl naphthalene sulfonate, etc. Emissions surfactants including but not limited to this as long as they do not impair the stability of the agrochemical active ingredient. By one or a combination of two or more selected from the group of these nonionic and anionic surfactants, an underwater sedimentation effect can be exhibited.
The form of use in which the surfactant exerts its effect may be formed by mixing with an agrochemical active ingredient and other raw materials and extrusion granulation to form an agrochemical granule, or mixing an agrochemical active ingredient and other raw materials, It is also possible to uniformly coat an underwater sedimentation-imparting agent on the surface of the agrochemical granules produced by extrusion granulation. Moreover, it is also possible to use both together.
The said surfactant can be contained in the ratio of 0.1-30 mass% in the agrochemical granule of this invention. More preferably, it is 0.1% to 10% by mass. If it is less than 0.1% by mass, it is not sufficient to exhibit a sufficient function for precipitating the agricultural chemical granules in water, and if it exceeds 30% by mass, good subsidence in water can be obtained. Since the elution rate of the active ingredient in water is greatly accelerated, elution control becomes difficult.

The poorly water-soluble polysaccharides, inorganic substances, and surfactants added in some cases according to the present invention have a role of adjusting the dissolution rate of agrochemical active ingredients in water while imparting good underwater sedimentation to the agrochemical granules. Plays. By appropriately adjusting the kind, content, and combination composition of poorly water-soluble polysaccharides, inorganic substances, and surfactants, while maintaining good moldability to granules and maintaining good sedimentation in water Agrochemical granules having a desired dissolution rate in water can be obtained. Usually, the agrochemical granule of the present invention comprises 3 to 25% by mass of an agrochemical active ingredient, 10 to 80% by mass of a fatty acid and / or a fatty acid derivative, 0.5 to 20% by mass of a poorly water-soluble polysaccharide, and 10 to 10% of an inorganic substance. It contains 60% by mass, and a desired dissolution rate in water can be obtained by appropriately adjusting within this range. In addition, the pesticide granule may contain a surfactant in a proportion of 0.1 to 10% by mass, and the water sedimentation rate of the pesticide granule and the elution rate of the pesticide active ingredient in water should be adjusted as appropriate. Can do. The surfactant is an agrochemical granule formed by granulating an agrochemical composition composed of an agrochemical active ingredient, a fatty acid and / or a fatty acid derivative, a poorly water-soluble polysaccharide and an inorganic substance, and optionally a surfactant. It can be coated on the surface of the grains, or it can be granulated by previously containing it in the agrochemical composition of the present invention. In some cases, it is also possible to coat the grain surface.
When two or more kinds of pesticidal active ingredients are contained in the pesticidal granules of the present invention, the pesticidal active ingredient may act to roughen the internal structure of the fatty acid and / or fatty acid derivative depending on the type of the pesticidal active ingredient. In this case, the pesticidal active ingredient exerts the effect of adjusting elution in water. Therefore, in order to express desired elution control, it is preferable to appropriately adjust the physical properties, solid particle diameter, and content of the pesticidal active ingredient used according to the elution rate.

There are the following two methods for producing the agrochemical granule of the present invention.
1) A method in which an agrochemical active ingredient, a fatty acid and / or a fatty acid derivative, an inorganic substance, and a poorly water-soluble polysaccharide are mixed well and then put into a granulator for granulation. Optionally, a method of coating the surface of the obtained granule with a surfactant.
2) A method in which an agrochemical active ingredient, a fatty acid and / or a fatty acid derivative, an inorganic substance, a poorly water-soluble polysaccharide, and a surfactant are mixed well and then put into a granulator for granulation. In some cases, the surface of the obtained granule is further coated with a surfactant.
When granulating the agricultural chemical composition of the present invention, the particle size is preferably 2 to 10 mm. If it is less than 2 mm, the pressure applied to the agrochemical composition is insufficient at the time of granulation, and it becomes difficult to form it into a form as a granule. Moreover, when spraying on a paddy field, there exists a possibility that it may fall to the shore etc. other than the paddy field which the said agrochemical granule aims at under the influence of a wind. When it exceeds 10 mm, not only granulation becomes difficult, but the number of sprayed particles per unit area decreases, and there may be problems such as uneven spraying and non-uniform effects.

The extrusion granulator used for production of the agrochemical granule of the present invention is preferably a vertical extrusion granulator, and the raw materials are mixed well and then put into the granulator for granulation. At this time, it is important to manufacture the granule that the die has a thickness of 10 mm or more and a particle size of 2 to 10 mm. When the thickness of the die is less than 10 mm, the pressure applied to the raw material is insufficient, and it becomes difficult to form into a shape as a granule. Moreover, when the particle size is outside the range of 2 to 10 mm, the pressure applied to the raw materials is still insufficient, and it becomes difficult to form the granules. A vertical extrusion granulator is a general name for a device that is generally granulated by extruding from a horizontally installed die by applying pressure to the composition to be granulated, and includes a disk pelleter (manufactured by Fuji Powder Co., Ltd.). It is done.
A concrete mixer, a coating pan, etc. are used for surfactant coating of the granule obtained by said method. The surfactant can be uniformly coated on the surface of the granule by adding the granule and the surfactant obtained by the above method to the mixer in this order and stirring.

  The present invention will be described in more detail with reference to the following examples, but the present invention is not limited thereto. The purity of thiocyclam oxalate used as an agrochemical active ingredient was about 89.9%. All of imidacloprid, pymetrozine and thiamethoxam had a purity of 98% or more.

Example 1
11.5 parts by weight of thiocyclam oxalate, 15.8 parts by weight of stearic acid, 37.3 parts by weight of castor oil hardened, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 30 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 2
11.5 parts by weight of thiocyclam oxalate, 12.9 parts by weight of stearic acid, 30.2 parts by weight of castor oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 40 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 3
11.5 parts by weight of thiocyclam oxalate, 9.9 parts by weight of stearic acid, 23.2 parts by weight of castor hardened oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 50 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate An agent was obtained.

Example 4
11.5 parts by weight of thiocyclam oxalate, 19.2 parts by weight of stearic acid, 36.4 parts by weight of castor hydrogenated oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle diameter: about 40 μm ) 30 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle diameter: 10 μm) 2.5 parts by weight well mixed with a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 5
11.5 parts by weight of thiocyclam oxalate, 15.7 parts by weight of stearic acid, 29.9 parts by weight of castor oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle diameter: about 40 μm ) 40 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle diameter: 10 μm) 2.5 parts by weight well mixed with a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 6
11.5 parts by weight of thiocyclam oxalate, 19.7 parts by weight of stearic acid, 37.4 parts by weight of castor hydrogenated oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 30 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) well mixed with 1.0 part by weight is a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 7
11.5 parts by weight of thiocyclam oxalate, 16.2 parts by weight of stearic acid, 30.9 parts by weight of castor oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 40 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 8
11.5 parts by weight of thiocyclam oxalate, 19.2 parts by weight stearic acid, 36.4 parts by weight castor oil, 30 parts by weight Seikolite (trade name, manufactured by Seiko Sangyo Co., Ltd., diatomaceous earth), 0. 35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) well mixed with a disk pelleter (trade name, manufactured by Fuji Powder Co., Ltd.) Put into a vertical extrusion granulator, die thickness 10mm, particle size 4.0mm), granulate, and sieved with 2mm (8.6 mesh) sieve, put into concrete mixer, Pegnol ST- 9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3) 0.3 parts by weight was coated to obtain 10.3% thiocyclam oxalate granules.

Example 9
11.5 parts by weight of thiocyclam oxalate, 12.3 parts by weight of stearic acid, 23.3 parts by weight of castor oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 50 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) well mixed with 2.5 parts by weight is a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm), granulated and sieved with 2 mm (8.6 mesh) sieve Put into a concrete mixer, coat 0.3 parts by weight of Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3), and 10.3% granules of thiocyclam oxalate Got the agent .

Example 10
11.5 parts by weight of thiocyclam oxalate, 19.2 parts by weight of stearic acid, 36.4 parts by weight of castor hydrogenated oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle diameter: about 40 μm ) 30 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle diameter: 10 μm) 2.5 parts by weight well mixed with a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10mm, particle size 4.0mm), granulated, sieved with 2mm (8.6 mesh) sieve, thiocyclam Oxalate 10.3% granules were obtained.

Example 11
11.5 parts by weight of thiocyclam oxalate, 15.7 parts by weight of stearic acid, 29.9 parts by weight of castor oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle diameter: about 40 μm ) 40 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle diameter: 10 μm) 2.5 parts by weight well mixed with a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10mm, particle size 4.0mm), granulated, sieved with 2mm (8.6 mesh) sieve, thiocyclam Oxalate 10.3% granules were obtained.

Example 12
11.5 parts by weight of thiocyclam oxalate, 12.3 parts by weight of stearic acid, 23.3 parts by weight of castor oil, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm ) 50 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemicals Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm) well mixed with 2.5 parts by weight is a disk pelleter ( Product name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10mm, particle size 4.0mm), granulated, sieved with 2mm (8.6 mesh) sieve, thiocyclam Oxalate 10.3% granules were obtained.

Example 13
11.5 parts by weight of thiocyclam oxalate, 15.7 parts by weight of stearic acid, 29.9 parts by weight of castor oil hardened, DL-clay (trade name, manufactured by Nitto Seiyaku Co., Ltd., clay, average particle size: about 25 μm) 30.0 parts by weight, castor oil 0.35 parts by weight, NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., fine crystalline cellulose, average particle size: 10 μm), 2.5 parts by weight, Riquemar S-200 (trade name, A disk pelleter (trade name, manufactured by Fuji Powder Co., Ltd., vertical extrusion granulator, die thickness 10 mm, particle size 4.0 mm) was prepared by mixing 10.1 parts by weight of Riken Vitamin Co., Ltd. (glyceryl stearate). ) And granulated with a 2 mm (8.6 mesh) sieve to obtain 10.3% thiocyclam oxalate granules.

Example 14
Imidacloprid 10.5 parts by weight, stearic acid 18.7 parts by weight, castor hydrogenated oil 35.5 parts by weight, silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm), A disk pelleter (trade name, Fuji) was prepared by mixing 0.35 parts by weight of castor oil and 5.0 parts by weight of NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm). Pourdal made, vertical extrusion granulator, put into a 10 mm die thickness, 4.0 mm particle size), granulated, and sieved with a 2 mm (8.6 mesh) sieve and put into a concrete mixer Pegnol ST-9 (trade name, manufactured by Toho Chemical Industry Co., Ltd., POE alkyl ether, HLB: 13.3) 0.3 parts by weight was coated to obtain imidacloprid 10.3% granules.

Example 15
2.0 parts by weight of imidacloprid, 15.6 parts by weight of stearic acid, 29.6 parts by weight of castor oil, 50 parts by weight of silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm), A disk pelleter (trade name, Fuji) was prepared by mixing 0.35 parts by weight of castor oil and 2.5 parts by weight of NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm). Pourdal made, vertical extrusion granulator, put into a 10 mm die thickness, 4.0 mm particle size), granulated, and sieved with a 2 mm (8.6 mesh) sieve and put into a concrete mixer , Rhedol TW-O120V (trade name, manufactured by Kao Corporation, POE sorbitan monooleate, HLB: 15) 0.3 parts by weight was coated to obtain 2.0% granules of imidacloprid.

Example 16
3.0 parts by weight of pymetrozine, 15.2 parts by weight of stearic acid, 28.9 parts by weight of castor oil, 50 parts by weight of silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm), A disk pelleter (trade name, Fuji) was prepared by mixing 0.35 parts by weight of castor oil and 2.5 parts by weight of NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm). Pourdal made, vertical extrusion granulator, put into a 10 mm die thickness, 4.0 mm particle size), granulated, and sieved with a 2 mm (8.6 mesh) sieve and put into a concrete mixer , Rhedol TW-O120V (trade name, manufactured by Kao Corporation, POE sorbitan monooleate, HLB: 15) 0.3 parts by weight was coated to obtain 3.0% pymetrozine granules.

Example 17
2.0 parts by weight of thiamethoxam, 15.6 parts by weight of stearic acid, 29.6 parts by weight of castor oil, 50 parts by weight of silt # 500 (trade name, manufactured by Marunaka Shiratosha, white clay, average particle size: about 40 μm), A disk pelleter (trade name, Fuji) was prepared by mixing 0.35 parts by weight of castor oil and 2.5 parts by weight of NP fiber (trade name, manufactured by Nippon Paper Chemical Co., Ltd., finely divided crystalline cellulose, average particle size: 10 μm). Pourdal made, vertical extrusion granulator, put into a 10 mm die thickness, 4.0 mm particle size), granulated, and sieved with a 2 mm (8.6 mesh) sieve and put into a concrete mixer , Rhedol TW-O120V (trade name, manufactured by Kao Corporation, POE sorbitan monooleate, HLB: 15) 0.3 parts by weight was coated to obtain 2.0% thiamethoxam granules.

Comparative Example 1
11.5 parts by weight of thiocyclam oxalate, 0.2 part by weight of castor oil, 20 parts by weight of stearic acid, 37.8 parts by weight of castor oil hardened, DL-clay (trade name, manufactured by Nitto Flour Mills, clay, average Particle pellet (about 25 μm) 30.0 parts by weight and Carplex # 80 (trade name, manufactured by Degussa Japan, amorphous silicon dioxide) 0.5 part by weight was mixed well with a disk pelleter (trade name, Thiocyclam oxalate 10 produced by Nipowdar Co., Ltd., vertical extrusion granulator, put into a die 10 mm thick, particle size 4.0 mm), granulated and sieved with a 2 mm (8.6 mesh) sieve A 3% granule was obtained.

Comparative Example 2
11.7 parts by weight of thiocyclam oxalate is mixed and melted in 88.3 parts by weight of stearic acid heated and melted in a melting machine, poured into a metal vat, cooled and crushed with a pelletizer. Sieving in the range of 1 mm (16 mesh) to 1.7 mm (10 mesh) gave thiocyclam oxalate 10.3% granules.

Comparative Example 3
11.7 parts by weight of thiocyclam oxalate was mixed and melted in 88.3 parts by weight of behenic acid heated and melted in a melting machine, poured into a metal bat, cooled, and crushed with a pelletizer. Sieving in the range of 1 mm (16 mesh) to 1.7 mm (10 mesh) gave thiocyclam oxalate 10.3% granules.

Comparative Example 4
11.7 parts by weight of thiocyclam oxalate was mixed and melted in 88.3 parts by weight of glycerin monostearate with a melting machine, poured into a metal bat, cooled and formed into a sheet with a pelletizer. The mixture was crushed and sieved in the range of 1 mm (16 mesh) to 1.7 mm (10 mesh) to obtain 10.3% thiocyclam oxalate granules.

Comparative Example 5
To 58.3 parts by weight of glycerol monostearate obtained by heating and melting 11.7 parts by weight of thiocyclam oxalate and 30 parts by weight of DL-clay (trade name, manufactured by Nitto Seiyaku Co., Ltd., clay, average particle size: about 25 μm) It is mixed and melted in a melting machine, poured into a metal bat, cooled and crushed with a pelletizer, sieved in the range of 1 mm (16 mesh) to 1.7 mm (10 mesh), and thiocyclam Shu An acid salt 10.3% granule was obtained.

Comparative Example 6
Beef cured by heating and melting 11.7 parts by weight of thiocyclam oxalate, 30 parts by weight of DL-clay (trade name, manufactured by Nitto Flour Mills, clay, average particle size: about 25 μm), and 10 parts by weight of glycerol monostearate 48.3 parts by weight of oil is mixed and melted with a melting machine, poured into a metal bat, cooled and formed into a sheet, and crushed with a pelletizer, in the range of 1 mm (16 mesh) to 1.7 mm (10 mesh) And thiocyclam oxalate 10.3% granules were obtained.

Comparative Example 7
Castor curing in which 11.7 parts by weight of thiocyclam oxalate, 30 parts by weight of DL-clay (trade name, manufactured by Nitto Flour Mills Co., Ltd., clay, average particle size: about 25 μm) and 20 parts by weight of glycerin monostearate are heated and melted. 38.3 parts by weight of oil is mixed and melted with a melting machine, poured into a metal bat, cooled and formed into a sheet, and crushed with a pelletizer, in the range of 1 mm (16 mesh) to 1.7 mm (10 mesh) And thiocyclam oxalate 10.3% granules were obtained.

Test Example 1 Underwater Sedimentability Test The floating state on the water surface was examined visually for the granules of the present invention and Comparative Examples 1, 6, and 7. Five granules were poured into a 1 L beaker filled with 1 L of distilled water, changes in the appearance of the grains were confirmed over time, evaluated in the following three stages, and the results are summarized in Table 1.
○: All grains are sinking △: A majority of grains are sinking
X: A majority of the grains floated on the water surface

Test Example 2 Hardness Test 100 g each of the granule of the present invention and Comparative Examples 1, 6, and 7 were put into a ball mill pot together with three magnetic balls (total of 105 g), and rotated at 75 rpm for 15 minutes. Thereafter, the contents in the ball mill pot were taken out, and the small particles passed through a sieve having an opening of 0.5 mm were weighed, and the value was taken as the hardness. The smaller the value, the higher the hardness. The results of Test Example 1 and Test Example 2 are shown in Table 1.

Table 1 Sedimentability and hardness test results of granules in water Test sample Immediately after dropping 3 hours later 6 hours later Hardness Example 1 ○ ○ ○ 3.6
Example 2 ○ ○ ○ 1.6
Example 3 ○ ○ ○ 1.6
Example 4 ○ ○ ○ 4.7
Example 5 ○ ○ ○ 4.5
Example 6 ○ ○ ○ 2.7
Example 7 ○ ○ ○ 2.8
Example 8 ○ ○ ○ 3.7
Example 9 ○ ○ ○ 2.0
Example 10 ○ △ △ 3.8
Example 11 ○ △ △ 4.0
Example 12 ○ △ △ 2.5
Example 13 Δ Δ Δ 7.4
Example 15 ○ ○ ○ 3.6
Example 16 ○ ○ ○ 4.5
Example 17 ○ ○ ○ 2.9
Comparative Example 1 ○ Δ × 29.1
Comparative Example 6 ○ ○ ○ 7.2
Comparative Example 7 ○ ○ ○ 8.5

Test Example 3 Underwater dissolution test 1
Put 0.5 g of agricultural chemical granules of Examples 1 to 9 and 13 and Comparative Examples 1 to 7 using thiocyclam oxalate as an agrochemical active ingredient into a 100 mL Erlenmeyer flask, and gently add 100 mL of distilled water. Poured (when all thiocyclam oxalate in the granules is eluted in water, it becomes 500 ppm). The amount of thiocyclam oxalate eluted in water after 1 day, 3 days, and 7 days after standing in a 25 ° C. constant temperature bath was measured by HPLC. The results of Test Example 3 are summarized in Table 2.

Table 2 Precipitation of granules in water and elution amount of thiocyclam oxalate (ppm)
Test sample 1 day later 3 days later 7 days later Example 1 69 104 136
Example 2 70 104 131
Example 3 128 209 282
Example 4 39 55 67
Example 5 75 123 165
Example 6 36 57 75
Example 7 65 108 145
Example 8 164 249 321
Example 9 107 190 270
Example 13 99 195 293
Comparative Example 1 10 16 24
Comparative Example 2 307 367 375
Comparative Example 3 405 497 484
Comparative Example 4 472 498 474
Comparative Example 5 470 491 367
Comparative Example 6 233 389 428
Comparative Example 7 220 328 369

Test Example 4 Water dissolution test 2
The agricultural chemical granules of Examples 15 to 17 were weighed so that the content of the agricultural chemical active ingredient was 50 mg, put into a 100 mL stoppered Erlenmeyer flask, and 100 mL of distilled water was gently poured (all active ingredients in the granules). Is 500 ppm in the case of elution). This was allowed to stand in a constant temperature bath at 25 ° C. for a predetermined time, and then the amount of the pesticidal active ingredient eluted in water after 2 hours, 24 hours and 96 hours was measured by HPLC. The results of Test Example 4 are summarized in Table 3.

Table 3 Sedimentability of granules in water and elution amount of active ingredients (ppm)
Test sample 2 hours later 24 hours later 96 hours later Example 15 15 52 96
Example 16 8.3 54 105
Example 17 39 117 233

Test Example 5 Insecticidal Efficacy Test 5 rice seedlings × 6 strains were planted in a 30 cm × 40 cm × 15 cm container bat and placed in a warming greenhouse. Sixteen days after planting, 33 g of the pesticidal granule of Example 17 containing thiamethoxam of the present invention as an pesticidal active ingredient was sprayed. In addition, as Comparative Example 8, 33 g of a commercially available thiamethoxam 2% granule (Digital Kola Top Actara Granule (trade name) / manufactured by Syngenta) was sprayed. After 4 days, 13 days, and 63 days after spraying, the planthoppers (Tobiro planta, white planthopper) were released. Three days after the insect release treatment, the life and death of the planthoppers were observed, and the death rate was calculated. The results are shown in Table 4.

Table 4 Results of the efficacy test of granule on planthoppers (Death rate /%)
Test sample 4 days 13 days 63 days Example 17 63 92 24
Comparative Example 8 0 89 24

As shown in Table 1, the agrochemical granule of the present invention was kept in the state of being settled in water not only immediately after being put into water but also after the time had been passed. This is because the inorganic substance contained in the pesticide granules adjusts the specific gravity of the pesticide granules to 1 or more, and the surfactant changes the physical properties of the grain surface, imparts hydrophilicity, and adheres to the grain surface. Due to the action of exfoliating foam from the surface of the grains, the granules could be continuously settled in water. Also in the hardness test, the results showed that the ball mill crushed amount was small, and the hardness was sufficient as an agrochemical granule. On the other hand, in Comparative Example 1 in which the poorly water-soluble polysaccharide component was not added, the sustained sedimentation property could not be maintained, and in the hardness test, the ball mill crushed amount was large and the granule hardness was insufficient. Comparative Examples 6 and 7 prepared by hot melting showed good water sedimentation due to the effect of containing DL-clay, but the granule hardness slightly decreased.
Moreover, as shown in Table 2 and Table 3, the agrochemical granule of the present invention has various elution characteristics by adding a poorly water-soluble polysaccharide, an inorganic substance, and a surfactant and adjusting the composition content thereof. It was possible to finish it into a granule, and it was possible to obtain a granule having a desired elution rate by suppressing initial dissolution and achieving continuous drug elution control. In addition to thiocyclam oxalate, it can provide elution control capability to imidacloprid and thiamethoxam neonicotinoid agrochemical active ingredients and pymetrozine as an agrochemical active ingredient, and it can be applied to various agrochemical active ingredients. It can be said that this is a wide range of pharmaceutical formulation technology. On the other hand, in Comparative Example 1 containing no poorly water-soluble polysaccharide, the drug elution rate was remarkably reduced, and Comparative Examples 2 to 7 prepared by hot melting did not achieve the initial elution suppression of the drug. There was a problem in the effect of maintaining the drug effect due to the sustained release.
The insecticidal efficacy test of Example 17 of the present invention showed that insecticidal efficacy can be exerted for up to 63 days after spraying. The agrochemical granule having the initial drug release control action and the sustained drug release control action of the present application exhibited an insecticidal effect that achieves both an initial insecticidal efficacy and a sustained efficacy. On the other hand, the commercially available thiamethoxam-containing granule (Comparative Example 8 Digital Collatop Actara Granule (trade name) / manufactured by Syngenta Co., Ltd.), which was Comparative Example 8, showed long-term residual effect but had insufficient initial efficacy. Therefore, the agrochemical granule according to the present application has a drug elution control action, achieves continuous drug elution over the long term from the beginning of pesticide spraying, and achieves both the initial effect and the residual effect of insecticidal efficacy by spraying once in the field. It was shown that it can be planned.

Controls the elution of pesticide active ingredients with high water solubility, prolongs the elution period, reduces the number of spraying, and saves labor. In addition, by adding and / or coating the surface of the pesticide granule obtained by adding and / or extrusion granulating a material that imparts sedimentation in water to the agrochemical granule, the specific gravity of the fatty acid derivative and the water repellent Prevents the localization of granules and the runoff from paddy fields caused by flowing water and wind, resulting in uniform effectiveness.

Claims (19)

A pesticide composition comprising a pesticide active ingredient (a), a fatty acid and / or a fatty acid derivative (b), a poorly water-soluble polysaccharide (c), and an inorganic substance (d). The agrochemical composition according to claim 1, wherein the agrochemical active ingredient (a) is an agrochemical active ingredient having a water solubility at 20 ° C of 100 ppm or more. The agrochemical composition according to claim 1 or 2, wherein the agrochemical composition contains 3 to 25% by mass of the agrochemical active ingredient (a). The agrochemical according to any one of claims 1 to 3, wherein the fatty acid and / or fatty acid derivative (b) is one or a mixture of two or more selected from C8-C40 alkyl chain carboxylic acids and derivatives thereof. Composition. The agrochemical composition according to any one of claims 1 to 4, wherein the fatty acid and / or the fatty acid derivative (b) is a mixture of castor oil, castor oil, and stearic acid. The agrochemical composition according to any one of claims 1 to 5, wherein the poorly water-soluble polysaccharide (c) is crystalline cellulose and has an average particle size of 1 µm to 45 µm. The agrochemical composition according to any one of claims 1 to 6, wherein the agrochemical active ingredient (a) includes a nereistoxin agrochemical active ingredient. Nereistoxin pesticide active ingredient is 1,3-dicarbamoylthio-2- (N, N-dimethylamino) -propane hydrochloride (hereinafter referred to as cartap hydrochloride) or 5-dimethylamino-1,2,3- The agrochemical composition according to claim 7, which is trithian oxalate (hereinafter referred to as thiocyclam oxalate). The inorganic substance (d) is at least one selected from the group consisting of clay, talc, white clay, diatomaceous earth, zeolite, barium sulfate, titanium dioxide, and amorphous silicon dioxide (white carbon). The agricultural chemical composition according to claim 1. In the agrochemical composition, the agrochemical active ingredient (a) is 3 to 25% by mass, the fatty acid and / or the fatty acid derivative (b) is 10 to 80% by mass, and the poorly soluble polysaccharide (c) is 0.5 to 20% by mass. %, And the agrochemical composition as described in any one of Claims 1-9 containing 10-60 mass% of inorganic substances (d). Furthermore, the agrochemical composition as described in any one of Claims 1-10 which contains 0.1-10 mass% of surfactant (e). The agrochemical composition according to claim 11, wherein the surfactant (e) is one or a mixture of two or more selected from nonionic surfactants and anionic surfactants. The agrochemical granule formed by granulating, after mixing the agrochemical composition as described in any one of Claims 1-12. The agrochemical granule obtained by mixing the agrochemical composition as described in any one of Claims 1-12, and granulating with a vertical extrusion granulator. The surfactant (e) according to claim 11 or 12 is coated on the mixture obtained by mixing the agrochemical composition according to any one of claims 1 to 12 and granulating with a vertical extrusion granulator. Pesticide granules. The agrochemical granule according to claim 13, wherein the particle size is 2 mm to 10 mm. The manufacturing method of the agrochemical granule granulated with a vertical extrusion granulator after mixing the agrochemical composition as described in any one of Claims 1-12. After mixing the agrochemical composition according to any one of claims 1 to 12, and then granulating with a vertical extrusion granulator, the surfactant (e) according to claim 11 or 12 is coated. To produce agrochemical granules. The method for producing an agrochemical granule according to claim 17 or 18, wherein the die used in the vertical extrusion granulator has a thickness of 10 mm or more.