JP2006281199A - Manufacturing method of particle mixtures - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide the manufacturing method of more homogeneous particle mixtures of a plurality of kinds by using a container rotary mixer or a mechanically stirring mixer. <P>SOLUTION: Highly homogeneous particle mixtures of two kinds or more can be obtained by the manufacturing method of the mixtures of particles A and particles B comprising a step for injecting the particles A consisting of a plurality of components and the particles B consisting of a plurality of components into a container, a step for humidifying the interior of the container, and a step for rotating the container or rotating stirring blades provided in the container. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a particle mixture composed of two or more components.

In the fields of medicines, agricultural chemicals, dyes, polymer additives, etc., multiple types of particles with different active ingredients and different characteristics (for example, release characteristics of active ingredients) without changing the shape of the particles before mixing , It may be necessary to mix uniformly. As a device for mixing particles, generally used are power mixers such as cylindrical mixers, V-type mixers, double cone mixers, ribbon-type mixers, etc. The particles are mixed by charging in a container and rotating the container itself or rotating a stirring blade in the container.
In such a batch type mixing method, it is required that a plurality of types of particles be uniformly mixed by a short time stirring. Patent Document 1 discloses an apparatus that can perform mixing by measuring the mixing homogeneity of particles in a mixer.

JP 2003-522635 A

  To provide a method for producing a mixture of particles capable of efficiently and uniformly mixing two or more kinds of particles.

  The present inventor has found that uniform mixing can be achieved in a short time by mixing two or more kinds of particles composed of a plurality of components in a humidified container using a power mixer, The present invention has been completed.

That is, the present invention
[Invention 1]
A step of putting particles (A) composed of a plurality of components and particles (B) composed of a plurality of components into a container;
Humidifying the interior of the container; and
A method for producing a mixture of particles (A) and particles (B), comprising a step of rotating the vessel or rotating a stirring blade provided in the vessel;
[Invention 2]
A step of putting particles (A) composed of a plurality of components and particles (B) composed of a plurality of components into a container;
Humidifying the interior of the container; and
A method for producing a mixture of particles (A) and particles (B), comprising the step of rotating the container;
[Invention 3]
The production method according to [Invention 1] or [Invention 2], wherein the particles (A) and the particles (B) are particles containing a surfactant;
[Invention 4]
The particle (A) and the particle (B) are particles having a particle diameter of 0.3 to 10 mm and a volume resistivity of 10 ¹⁰ Ω · m or more [Invention] 1] to [Invention 3] according to any one of the production methods;
[Invention 5]
The production method according to any one of [Invention 1] to [Invention 4], wherein the particles (A) are particles containing particles containing a pharmaceutical ingredient, an agrochemical ingredient or a fertilizer ingredient;
[Invention 6]
The production method according to any one of [Invention 1] to [Invention 5], wherein the particles (A) are particles coated with a resin.

  The method for producing a particle mixture using a container rotating mixer includes a step of putting particles to be mixed into a container and a step of rotating the container. Moreover, the manufacturing method of the particle mixture by a mechanical stirring type mixer includes the process of putting the particle | grains to be mixed in a container, and the process of rotating the stirring blade provided in this container.

  The mixture of particles (A) and particles (B) obtained by the method of the present invention is a mixture in which the particles (A) and the particles (B) each remain in the form of particles.

  Examples of the power mixer used in the method for producing a mixture of particles according to the present invention include a container rotating mixer and a mechanical stirring mixer from the method of imparting momentum to particles.

  Examples of the container rotating mixer include a horizontal cylindrical mixer, an inclined cylindrical mixer, a V mixer, and a double cone mixer. The container rotation type mixer is suitable for use in mixing particles having a small fluidity difference between particles to be mixed and having good fluidity and particles easily broken by friction.

  Examples of the mechanical stirring mixer include a ribbon mixer, a conical screw mixer, a high-speed fluid mixer, a rotating disk mixer, and a stirring mixer. The mechanical stirring mixer is suitable for use in mixing particles having a large difference in physical properties.

  The particle | grains which consist of multiple components in this invention mean the particle | grains in which 1 or more types of components different from this solid component are contained in a solid component. The particles include particles in which different components are uniformly dispersed in the solid component and particles in which different components are unevenly distributed around the solid component.

  In the present invention, the particle (A) composed of a plurality of components and the particle (B) composed of a plurality of components are different from each other. Here, the particles are different from each other (a) when the types of components contained in the particles are different, or (b) when the content of a specific component contained in the particles is twice or more different. In addition, the case where only the shape of particle | grains or a particle diameter differs is not included.

  Here, the “component” contained in the particle means a substance having a content of 0.1% by weight or more in the particle. The components contained in the particles do not have a chemical bond with each other, and are held in the particles by a physical force such as a cohesive force.

  The method for producing a particle mixture of the present invention comprises (i) a step of putting particles (A) consisting of a plurality of components and different particles (B) consisting of a plurality of components into a container, (ii) a step of humidifying the inside of the container, and (Iii) A step of rotating the container or rotating a stirring blade provided in the container. The steps (i) and (ii) may be performed in parallel, and the steps (ii) and (iii) may be performed in parallel.

  In the step (i), the particles (A) and the particles (B) are put in a container, but particles different from the particles (A) and the particles (B) may be further added.

  The mixing ratio of the particles (A) and the particles (B) is usually 50:50 to 5:95 by weight, and preferably 50:50 to 75:25.

  Step (ii) is performed, for example, by sending high-humidity air into the container or sending fine water droplets (mist). Humid air or fine water droplets can be generated by a humidifier. As a humidifier, there are a plurality of types such as a heating type (steam type) that generates water vapor by heating water, an ultrasonic type that generates fine water droplets (mist) by an ultrasonic vibrator, and a combination thereof. There are types.

  The relative humidity in the container is raised by 10% or more, preferably 20% or more with respect to the relative humidity outside the container in step (ii). The relative humidity in the container is usually preferably 50% or more.

  The relative humidity is a value obtained by dividing the water vapor partial pressure in the measurement air by the saturated water vapor partial pressure at the measurement temperature × 100, and is expressed in%.

  In the step (iii), the particles (A) and the particles (B) are rotated by rotating the container itself containing the particles (A) and the particles (B) or by rotating the stirring blade provided in the container. It is a process of mixing.

  Step (iii) is usually performed in the range of −10 to 50 ° C. When the particle (A) or the particle (B) contains a pharmaceutical component, an agrochemical component or a fertilizer component, it is preferably performed in the range of −5 to 40 ° C. from the viewpoint of the stability of the component.

  In the present invention, the number of particles per 1 g of particles (A) and particles (B) is usually 50 to 5000, preferably 200 to 3000. The apparent specific gravity of the particles is usually 0.3 to 1.5 g / cc, preferably 0.7 to 1.2 g / cc. The apparent specific gravity of the particles can be measured by the whole farming method. The difference in apparent specific gravity between the particles (A) and the particles (B) is preferably 0.3 g / cc or less, more preferably 0.2 g / cc or less. The shape of the particles is usually a cubic shape, a rectangular parallelepiped shape, a triangular pyramid shape, a conical shape, a cylindrical shape, a spherical shape, a dumbbell shape, an elliptical shape, an egg shape, a convex lens shape, a concave lens shape, a plate shape, and the like.

The particles (A) and particles (B) used in the present invention are usually charged particles, that is, the volume resistivity determined by measuring the electrical resistance of the particles is 10 ¹⁰ Ω · m or more. Is a particle. The volume resistivity of the particles is determined by, for example, packing a particle in a container of 150 mmφ × 10 mm, placing 10 mm in the sample thickness direction, and installing 80 mmφ electrodes at both ends. Can be calculated by obtaining the resistance value using R8340A type manufactured by Advantest Corporation).

  The particles (A) and the particles (B) preferably contain a surfactant as a constituent component of a particle composed of a plurality of components. Furthermore, examples of the constituent components of the particles include pharmaceutical components, agricultural chemical components, fertilizer components, dye components, and polymer additive components in addition to the surfactant.

  Examples of the surfactant include nonionic surfactants, anionic surfactants, cationic surfactants, and amphoteric surfactants. When the surfactant contained in the particles is contained, the amount thereof is 0.1 to 70% by weight, preferably 0.5 to 30% by weight, based on the weight of the particles.

Examples of nonionic surfactants include sugar ester type nonionic surfactants, fatty acid ester type nonionic surfactants, vegetable oil type nonionic surfactants, alcohol type nonionic surfactants, and alkylphenol type nonionic surfactants. Agent, polyoxyethylene / polyoxypropylene block polymer type nonionic surfactant, bisphenol type nonionic surfactant, polyaromatic ring type nonionic surfactant, silicon type nonionic surfactant and fluorine type nonionic surfactant An agent can be mentioned.
Examples of the sugar ester type nonionic surfactant include sorbitan fatty acid ester, polyoxyethylene sorbitan aliphatic ester, and sucrose fatty acid ester.
Examples of the fatty acid ester type nonionic surfactant include polyoxyethylene fatty acid esters, polyoxyethylene resin acid esters, and polyoxyethylene fatty acid diesters.
Examples of the vegetable oil type nonionic surfactant include polyoxyethylene castor oil and polyoxyethylene hydrogenated castor oil.
Examples of the alcohol type nonionic surfactant include polyoxyethylene alkyl ether.
Examples of the alkylphenol type nonionic surfactant include polyoxyethylene alkylphenyl ether, polyoxyethylene dialkylphenyl ether, and polyoxyethylene alkylphenyl ether / formalin condensate.
Polyoxyethylene / polyoxypropylene block polymer type nonionic surfactants include, for example, polyoxyethylene / polyoxypropylene block polymer, alkylpolyoxyethylene / polyoxypropylene block polymer ether and alkylphenyl polyoxyethylene / polyoxy A propylene block polymer ether is mentioned.
Examples of the bisphenol type nonionic surfactant include polyoxybisphenyl ether. Examples of the polyaromatic nonionic surfactant include polyoxyalkylene benzyl phenyl ether and polyoxyalkylene styryl phenyl ether.
Examples of silicon-type nonionic surfactants include polyoxyethylene ether type silicon surfactants and polyoxyethylene ester type silicon surfactants.

Examples of the anionic surfactant include sulfate type anionic surfactant, anionic surfactant, sulfonate type anionic surfactant, phosphate type anionic surfactant and carboxylic acid type anionic surfactant. be able to.
Examples of the sulfate type anionic surfactant include alkyl sulfate, polyoxyethylene alkyl ether sulfate, polyoxyethylene alkyl phenyl ether sulfate, polyoxystyryl phenyl ether sulfate, and polyoxyethylene / polyoxypropylene block polymer sulfate. .
Examples of the sulfonate type anionic surfactant include paraffin sulfonate, dialkyl sulfosuccinate, alkylbenzene sulfonate, monoalkyl naphthalene sulfonate, dialkyl naphthalene sulfonate, naphthalene sulfonate / formalin condensate, Examples include alkyl diphenyl ether disulfonate and polyoxyethylene alkyl phenyl ether sulfonate.
Examples of the phosphate type anionic surfactant include polyoxyethylene alkyl ether phosphate, polyoxyethylene monoalkyl phenyl ether phosphate, polyoxyethylene dialkyl phenyl ether phosphate, polyoxyethylene styryl phenyl ether phosphate, polyoxyethylene alkyl ether phosphate Examples thereof include oxyethylene / polyoxypropylene block polymer phosphates and alkyl phosphates.
Examples of the carboxylic acid type anionic surfactant include fatty acid sodium, fatty acid potassium, fatty acid ammonium, N-methyl-sarcosinate, sodium resinate and potassium resinate.

Examples of the cationic surfactant include an ammonium type cationic surfactant and a benzalkonium type cationic surfactant.
Examples of ammonium-type cationic surfactants include alkyltrimethylammonium chloride, methylpolyoxyethylene alkylammonium chloride, alkyl N-methylpyridinium bromide, mono- or dialkylmethylated ammonium chloride, and alkylpentamethylpropylenediamine chloride. .
Examples of the benzalkonium-type cationic surfactant include alkyldimethylbenzalkonium chloride, benzethonium chloride, and octylphenoxyethoxyethyldimethylbenzylammonium chloride.

  Examples of amphoteric surfactants include betaine-type amphoteric surfactants. Examples of betaine-type amphoteric surfactants include dialkyldiaminoethyl betaine and alkyldimethylbenzyl betaine.

  In the present invention, when the particle (A) is a particle containing an agrochemical component, the particle usually contains an agrochemical component, a surfactant, and further a carrier as a solid component, and if necessary, a binder, Solvents, stabilizers, colorants, coating agents and the like are further contained. Usually, agrochemical ingredients, surfactants, carriers as solid ingredients, and if necessary, binders, solvents, stabilizers, colorants, coating agents, etc. are mixed, granulated and molded, and then the particles are formed. Can be manufactured.

  Examples of the agrochemical component include insecticides, fungicides, herbicides, insect growth regulators, plant growth regulators, and the like. Specific examples include the following compounds.

  O, O-dimethyl-O- (3-methyl-4-nitrophenyl) phosphorothioate, O, O-dimethyl-O- (3-methyl-4- (methylthio) phenyl) phosphorothioate, O, O-diethyl-O- 2-isopropyl-6-methylpyrimidin-4-yl phosphorothioate, O, O-diethyl-O-3,5,6-trichloro-2-pyridyl phosphorothioate, O, S-dimethylacetyl phosphoramide thioate, S-2, 3-dihydro-5-methoxy-2-oxo-1,3,4-thiadiazol-3-ylmethyl O, O-dimethyl phosphorodithioate, O, O-diethyl S-2-ethylthioethyl phosphorodithioate, 2,2-dichlorovinyldimethylphosphate, O-ethyl-O-4- (methylthio) phenyl S-propyl phosphate Forodithioate, O-4-cyanophenyl O, O-dimethyl phosphorothioate, 2-methoxy-4H-1,3,2-benzodioxaphosphorin-2-sulfide, O, O-dimethyl-S- (N-methylcarbamoyl) Methyl) dithiophosphate, ethyl 2-dimethoxyphosphinothioylthio (phenyl) acetate, diethyl (dimethoxyphosphinothioylthio) succinate, dimethyl 2,2,2-trichloro-1-hydroxyethylphosphonate, S-3,4 -Dihydro-4-oxo-1,2,3-benzotriazin-3-ylmethyl O, O-dimethyl phosphorodithioate, dimethyl-{(E) -1-methyl-2- (methylcarbamoyl) vinyl} phosphate, O, O, O ′, O′-tetraethyl-S, S′-methylenebi (Phosphorodithioate) organophosphorus compounds such as,

  2-sec-butylphenylmethylcarbamate, ethyl N- {2,3-dihydro-2,2-dimethylbenzofuran-7-yloxycarbonyl (methyl) aminothio} -N-isopropyl-β-alaninate, 2-isopropoxyphenyl -N-methyl carbamate, 2,3-dihydro-2,2-dimethyl-7-benzo (b) furanyl N-dibutylaminothio-N-methyl carbamate, 1-naphthyl-N-methyl carbamate, S-methyl-N -(Methylcarbamoyloxy) thioacetimidate, 2- (ethylthiomethyl) phenylmethylcarbamate, 2-methyl-2- (methylthio) propionaldehyde O-methylcarbamoyloxime, N, N-dimethyl-2-methylcarbamoyloxy Imino-2- (methylthio) ace Carbamate compounds such as toamide, S-4-phenoxybutyl-N, N-dimethylthiocarbamate,

  2- (4-Ethoxyphenyl) -2-methyl-1- (3-phenoxybenzyl) oxypropane, (RS) -α-cyano-3-phenoxybenzyl (RS) -2- (4-chlorophenyl) -3- Methyl butyrate, (S) -α-cyano-3-phenoxybenzyl (S) -2- (4-chlorophenyl) -3-methylbutyrate, (RS) -α-cyano-3-phenoxybenzyl 2,2, 3,3-tetramethylcyclopropanecarboxylate, (RS) -α-cyano-3-phenoxybenzyl (1RS) -cis, trans-3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropanecarboxy Rate, 3-phenoxybenzyl (1RS) -cis, trans-3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropanecal Boxylate, (RS) -α-cyano-3-phenoxybenzyl (1RS, 3Z) -cis-3- (2-chloro-3,3,3-trifluoroprop-1-enyl) -2,2-dimethylcyclo Propanecarboxylate, (S) -α-cyano-3-phenoxybenzyl (1R) -cis-3- (2,2-dibromovinyl) -2,2-dimethylcyclopropanecarboxylate, (RS) -α-cyano -3-phenoxybenzyl (RS) -2,2-dichloro-1- (4-ethoxyphenyl) cyclopropanecarboxylate, α-cyano-3-phenoxybenzyl N- (2-chloro-α, α, α-tri Fluoro-p-tolyl) -D-valinate, 2-methyl-3-phenylbenzyl (1RS, 3Z) -cis-3- (2-chloro-3,3,3-trifluoro Oro-1-propenyl) -2,2-dimethylcyclopropanecarboxylate, 2- (4-bromodifluoromethoxyphenyl) -2-methyl-1- (3-phenoxybenzyl) methylpropane, (S) -α-cyano -3-phenoxybenzyl (1R) -cis-3- (1,2,2,2-tetrabromoethyl) -2,2-dimethylcyclopropanecarboxylate, (4-ethoxyphenyl)-{3- (4- Fluoro-3-phenoxyphenyl) propyl} dimethylsilane, 3-phenoxybenzyl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (RS)- α-cyano-3-phenoxybenzyl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1) -Propenyl) cyclopropanecarboxylate, 5-benzyl-3-furylmethyl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (S)- α-Cyano-3-phenoxybenzyl (1R, 3Z) -cis- (2,2-dimethyl-3- {3-oxo-3- (1,1,1,3,3,3-hexafluoropropyloxy) Propenyl} cyclopropanecarboxylate, (RS) -α-cyano-4-fluoro-3-phenoxybenzyl 3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropanecarboxylate, 2,3,5 6-tetrafluoro-4-methylbenzyl (1RS, 3Z) -cis-3- (2-chloro-3,3,3-trifluoro-1-propenyl -2,2-dimethylcyclopropanecarboxylate, 2,3,5,6-tetrafluorobenzyl (1R) -trans-3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropanecarboxylate, 3 , 4,5,6-tetrahydrophthalimidomethyl (1RS) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (RS) -2-methyl-4- Oxo-3- (2-propenyl) -2-cyclopenten-1-yl (1RS) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (S) -2-methyl-4-oxo-3- (2-propynyl) -2-cyclopenten-1-yl (1R) -cis, trans-2,2 -Dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (RS) -1-ethynyl-2-methyl-2-pentenyl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, 2,5-dioxo-3- (2-propynyl) imidazolidin-1-ylmethyl (1R) -cis, trans-2,2-dimethyl-3- ( 2-methyl-1-propenyl) cyclopropanecarboxylate, 5- (2-propynyl) furfuryl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate , Pyrethro such as 5- (2-propynyl) furfuryl 2,2,3,3-tetramethylcyclopropanecarboxylate De-based compounds,

  Thiadiazine derivatives such as 2-tert-butylimino-3-isopropyl-5-phenyl-1,3,5-thiadiazin-4-one, nitroimidazolidine derivatives, S, S ′-(2-dimethylaminotrimethylene) bis (thiocarbamate) ), N, N-dimethyl-1,2,3-trithian-5-ylamine, S, S′-2-dimethylaminotrimethylenedi (benzenethiosulfonate) and other nereistoxin derivatives, N-cyano- N-cyanoamidine derivatives such as N′-methyl-N ′-(6-chloro-3-pyridylmethyl) acetamidine, 6,7,8,9,10,10-hexachloro-1,5,5a, 6, 9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepine oxide, 1,2,3,4,5,6-hexachloro Cyclohexane, 1,1-bis (4-chlorophenyl) -2,2,2-trichloroethanol) chlorinated hydrocarbon compounds such as,

1- {3,5-dichloro-4- (3-chloro-5-trifluoromethylpyridin-2-yloxy) phenyl} -3- (2,6-difluorobenzoyl) urea, 1- (3,5-dichloro -2,4-difluorophenyl) -3- (2,6-difluorobenzoyl) urea, 1- {4- (2-chloro-4-trifluoromethylphenoxy) -2-fluorophenyl} -3- (2, 6-difluorobenzoyl) urea and other benzoylphenylurea compounds,

  Formamidine derivatives such as N, N ′-{(methylimino) dimethylidyne} -di-2,4-xylidine, N ′-(4-chloro-2-methylphenyl) -N, N-dimethylmethinimidamide, N— Thiourea derivatives such as (2,6-diisopropyl-4-phenoxyphenyl) -N′-t-butylcarbodiimide, N-phenylpyrazole compounds, 5-methoxy-3- (2-methoxyphenyl) -1,3, 4-oxadiazol-2- (3H) -one, isopropyl 4,4′-dibromobenzylate, 4-chlorophenyl 2,4,5-trichlorophenylsulfone, S, S-6-methylquinoxaline-2,3- Diyldithiocarbonate, 2- (4-tert-butylphenoxy) cyclohexylprop-2-ylsulfite, bis {tris (2- Til-2-phenylpropyl) tin} oxide, (4RS, 5RS) -5- (4-chlorophenyl) -N-chlorohexyl-4-methyl-2-oxo-1,3-thiazolidine-3-carboxamide, 3, 6-bis (2-chlorophenyl) -1,2,4,5-tetrazine, 2-tert-butyl-5- (4-tert-butylbenzylthio) -4-chloropyridazin-3 (2H) -one, tert -Butyl (E) -4-[(1,3-dimethyl-5-phenoxypyrazol-4-yl) methyleneaminooxymethyl] benzoate, N- (4-tert-butylbenzyl) -4-chloro-3-ethyl -1-methyl-5-pyrazolecarboxamide, 5-chloro-N- [2- {4- (2-ethoxyethyl) -2,3-dimethylphenoxy} ethyl -6-ethylpyrimidin-4-amine, 5-methyl (1,2,4) triazolo (3,4-b) benzothiazole, methyl 1- (butylcarbamoyl) benzimidazole-2-carbamate, 6- (3 5-Dichloro-4-methylphenyl) -3 (2H) -pyridazinone, 1- (4-chlorophenoxy) -3,3-dimethyl-1- (1H-1,2,4-triazol-1-yl) butanone , (E) -4-chloro-2- (trifluoromethyl) -N- [1- (imidazol-1-yl) -2-propoxyethylidene] aniline, 1- [N-propyl-N- [2- ( 2,4,6-trichlorophenoxy) ethyl] carbamoyl] imidazole, (E) -1- (4-chlorophenyl) -4,4-dimethyl-2- (1H-1,2,4-triazole -1-yl) -1-penten-3-ol, 1- (4-chlorophenyl) -4,4-dimethyl-2- (1H-1,2,4-triazol-1-yl) pentan-3-ol (E) -1- (2,4-dichlorophenyl) -4,4-dimethyl-2- (1H-1,2,4-triazol-1-yl) -1-penten-3-ol, 1- ( 2,4-dichlorophenyl) -4,4-dimethyl-2- (1H-1,2,4-triazol-1-yl) pentan-3-ol, 4- [3- (4-tert-butylphenyl)- 2-methylpropyl] -2,6-dimethylmorpholine, 2- (2,4-dichlorophenyl) -1- (1H-1,2,4-triazol-1-yl) hexan-2-ol, O, O- Diethyl O-2-quinoxalinyl phosphorothioe , O- (6-ethoxy-2-ethyl-4-pyrimidinyl) O, O-dimethyl phosphorothioate, 2-diethylamino-5,6-dimethylpyrimidin-4-yl dimethylcarbamate, 4- (2,4-dichloro Benzoyl) -1,3-dimethyl-5-pyrazolyl p-toluenesulfonate, 4-amino-6- (1,1-dimethylethyl) -3-methylthio-1,2,4-triazine-5 (4H)- ON, 2-chloro-N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl) aminocarbonyl] benzenesulfonamide, 2-methoxycarbonyl-N-[(4,6- Dimethoxypyrimidin-2-yl) aminocarbonyl] benzenesulfonamide, 2-methoxycarbonyl-N-((4,6-dimethylpyrimidine 2-yl) aminocarbonyl) benzenesulfonamide, 2-methoxycarbonyl-N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl) aminocarbonyl] benzenesulfonamide, 2-ethoxy Carbonyl-N-[(4-chloro-6-methoxypyrimidin-2-yl) aminocarbonyl] benzenesulfonamide, 2- (2-chloroethoxy) -N-[(4-methoxy-6-methyl-1,3 , 5-Triazin-2-yl) aminocarbonyl] benzenesulfonamide, 2-methoxycarbonyl-N-[(4,6-dimethoxypyrimidin-2-yl) aminocarbonyl] phenylmethanesulfonamide, 2-methoxycarbonyl-N -[(4-Methoxy-6-methyl-1,3,5-triazin-2-yl) aminocal Bonyl] thiophene-3-sulfonamide, 4-ethoxycarbonyl-N-[(4,6-dimethoxypyrimidin-2-yl) aminocarbonyl] -1-methylpyrazole-5-sulfonamide, 2- [4,5- Dihydro-4-methyl-4- (1-methylethyl) -5-oxo-1H-imidazol-2-yl] -3-quinolinecarboxylic acid, 2- [4,5-dihydro-4-methyl-4- ( 1-methylethyl) -5-oxo-1H-imidazol-2-yl] -5-ethyl-3-pyridinecarboxylic acid, methyl 6- (4-isopropyl-4-methyl-5-oxoimidazolin-2-yl) -M-toluate, methyl 2- (4-isopropyl-4-methyl-5-oxoimidazolin-2-yl) -p-toluate, 2- (4-isopropyl-4-me Til-5-oxoimidazolin-2-yl) nicotinic acid, N- (4-chlorophenyl) methyl-N-cyclopentyl-N′-phenylurea, (RS) -2-cyano-N-[(R) -1 ( 2,4-dichlorophenyl) ethyl] -3,3-dimethylbutyramide, N- (1,3-dihydro-1,1,3-trimethylisobenzofuran-4-yl) -5-chloro-1,3-dimethyl Pyrazole-4-carboxamide, N- [2,6-dibromo-4- (trifluoromethoxy) phenyl] -2-methyl-4- (trifluoromethyl) -5-thiazolecarboxamide, 2,2-dichloro- N- [1- (4-chlorophenyl) ethyl] -3-methylcyclopropanecarboxamide, methyl (E) -2-2-2-6- (2-cyanophenoxy) pyrim N-4-yloxy-phenyl-3-methoxyacrylate, 5-methyl-1,2,4-triazolo (3,4-b) benzothiazole, 3-allyloxy-1,2-benzisothiazole-1,1 -Dioxide, diisopropyl = 1,3-dithiolane-2-ylidene-malonate, O, O-dipropyl-O-4-methylthiophenyl phosphate and the like.

Examples of the carrier as the solid component include a mineral carrier, a vegetable carrier, a moving substance carrier, a synthetic carrier, and the like.
Examples of mineral carriers include kaolinite, kaolinite, dickite, nacrite, kaolin minerals such as halloysite, chrysotile, lizardite, and antigolite. Montmorillonite minerals such as (antigorite), amesite, serpentinite, sodium montmorillonite, calcium montmorillonite, magnesium montmorillonite, saponite, hectorite hectorite, sauconite, beidellite, smectite, pyrophyllite, talc, agalmatolite, muscovite, phengite, cereal Hydrous magnesium silicate such as sericite, illite, mica, cristobalite, quartz, silica, attapulgite, sepiolite, etc. ), Dolomite, calcium carbonate fine powder, calcium carbonate, gypsum, sulfate minerals such as plaster, zeolite (zeolite), boiling stone, Examples include tuff, vermiculite, laponite, pumice, diatomite, acidic clay, and activated clay. Examples of plant carriers include cellulose, hull, wheat flour, wood flour, starch, bran, wheat bran, soybean flour ( soy bean flour).
Synthetic carriers include, for example, wet silica, dry silica, calcined product of wet silica, surface modified silica, modified starch ( Matsutani Chemical Pine Flow etc.) [processed starch (ex. Pineflow manufactured by Matsutani Kagaku KK (Japan))] and the like.
These carriers are usually contained in the granular material in an amount of 0.5 to 99.9% by weight, preferably 25 to 99.5% by weight.

  In the present invention, when the particles (A) and / or particles (B) are particles containing a fertilizer component, the particles usually contain a fertilizer component and a surfactant, and if necessary, a coloring agent (coloring agent), coating material, and the like.

  As fertilizer components, urea (urea), ammonium sulfate, ammonium chloride, ammonium phosphate, ammonium nitrate, lime nitrogen, sodium nitrate ), Acetaldehyde condensed urea, calcined phosphate, processed phosphate fertiliaer, conc. Superphosphate, mixed phosphate fertilizer mixture, potassium chloride ( potassium chloride), potassium sulfate magnesia, potassium bicarbonate, potassium silicate, potassium phosphate, potassium phosphate, potassium nitrite, etc. .

  In the present invention, the particles (A) and / or the particles (B) may be coated with a resin or the like. Examples of the resin in this case include water-soluble polymers, waxes, thermoplastic resins, and thermosetting resins.

  Examples of the water-soluble polymer include sugars and alginate.

  Examples of the wax include, for example, synthetic waxes such as carbowax, hoechst wax, sucrose ester, fatty acid ester, carnauba wax, beeswax, Examples thereof include natural waxes such as wood wax, petroleum waxes such as paraffin wax and petrolactam.

  Examples of thermoplastic resins include polyolefins such as polyethylene, polypropylene, polybutene, and polystyrene, polyvinyl acetate, polyvinyl chloride, polyvinylidene chloride, polyacrylic acid, polymethacrylic acid, polyacrylic acid ester, and polymethacrylic acid ester. Vinyl polymers, butadiene polymers, isoprene polymers, chloroprene polymers, butadiene-styrene copolymers, ethylene-propylene-diene copolymers, diene polymers such as styrene-isoprene copolymers, ethylene-propylene copolymers Polymer, butene-ethylene copolymer, butene-propylene copolymer, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid copolymer, ethylene-methacrylic acid ester copolymer , Ethylene Carbon oxide copolymer, polyolefin copolymer such as ethylene-vinyl acetate-carbon monoxide copolymer, vinyl chloride copolymer such as vinyl chloride-vinyl acetate copolymer, vinylidene chloride-vinyl chloride copolymer, etc. Can be mentioned.

  Examples of the thermosetting resin include urethane resin, epoxy resin, alkyd resin, unsaturated polyester resin, phenol resin, urea resin ( Examples include urea resin, melamine resin, silicon resin, and the like.

  The urethane resin is usually produced by reacting a polyisocyanate and a polyol in the presence of a curing agent such as an organic metal or an amine. Polyisocyanate and polyol, which are monomers of a urethane resin, are usually used in the form of a monomer alone, a solution, a water-based emulsion, an organic solvent-based emulsion, or the like. Such polyisocyanates include toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), naphthalene diisocyanate, tolidine diisocyanate, hexamethylene diisocyanate, isophorone. Diisocyanate, xylylene diisocyanate, 4,4-methylenebis (cyclohexylisocyanate), trimethylhexamethylenediisocyanate, 1,3- (isocyanatomethyl) Cyclohexane (1,3- (isocyanatemethyl) cyclohexane), triphenylmethanetriisocyanate, tris (isocyanate) Phenyl) thiophosphate (tris (isocyanataphenyl) thiophosphate), and, and mixtures thereof.

  In addition, it can replace with said polyisocyanate monomer and can also use these modified bodies and oligomers. Examples of the modified body include an adduct modified body, a biuret modified body, an isocyanurate modified body, a block modified body, a prepolymer modified body, and a dimerized modified body. Examples of the polyol include a condensed polyester polyol, a polyether polyol, a poly (meth) acrylic acid polyol, a lactone type polyether polyol, Examples thereof include polycarbonate polyol, natural polyol, and modified products thereof. The condensed polyester polyol is usually obtained by a condensation reaction between a polyol and a dibasic acid, and the polyether polyol is usually obtained by a polymerization reaction of a cyclic oxide. Poly (meth) acrylic acid polyol is usually obtained by condensation reaction of poly (meth) acrylic acid and polyol, condensation reaction of (meth) acrylic acid and polyol, or polymerization reaction of (meth) acrylic acid ester monomer. It is done. The lactone polyester polyol is obtained by ring-opening polymerization of ε-caprolactam using a polyhydric alcohol as an initiator. Polycarbonate polyol is usually obtained by the reaction of glycol and carbonate. As polyol, methylene glycol, ethylene glycol, propylene glycol, tetramethylene glycol, hexamethylene glycol, Methylene diol, trimethylol propane, poly (tetramethylene glycol), glycerin, pentaerythritol, sorbitol, sucrose, and , And these oligomers. Examples of the dibasic acid include adipic acid and phthalic acid. As (meth) acrylic acid, acrylic acid, methacrylic acid and the like are generally used.

  Epoxy resin is usually a reaction of phenol or alcohol with epichlorhydrin in the presence of a curing agent, a reaction of carboxylic acid with epichlorohydrin in the presence of a curing agent, a curing agent. Reactions of amines, cyanuric acid or hydantoin with epichlorohydrin in the presence of alcohol, and aliphatic cyclic epoxy compounds in the presence of curing agents such as peracetic acid ) And the like. Epoxy resins include bisphenol A type, bisphenol F type, brominated bisphenol A type, hydrogenated bisphenol A type, bisphenol S type, bisphenol AF type, biphenyl type, naphthalene type, fluorin glycidyl amines such as (fluorene) type, phenol novolac type, orthocresol novolac type, DPP novolac type, trishydroxyphenylmethane type, tetraphenylolethane type, etc. Ether type epoxy resin, tetraglycidyldiaminodiphenylmethane type, triglycidylisocyanurate type, hydantoin type, aminophenol type, aniline type, toluidi (Toluidine) type glycidyl amine type epoxy resins such as alicyclic epoxy resin (alicyclic type epoxy resins) and the like.

The alkyd resin may be, for example, a modifying agent such as natural vegetable oil or animal fat, a metal soap, Produced by performing in the presence of an antiskinning agent.
Examples of the polybasic acid include phthalic anhydride and maleic anhydride, and examples of the polyhydric alcohol include pentaerythritol and glycerin.
Examples of the modifying agent include soybean oil, linseed oil, tung oil, safflower oil, coconut oil, palm oil, Dehydrated castor oil, etc.
As the metal soap, usually, metal salts of naphthenic acid or octylic acid such as manganese, cobalt, zirconium, nickel, iron, lead and the like, for example, Zirconium octylate, manganese naphthenate, cobalt octylate, and mixtures thereof. Examples of the anti-skinning agent include dipentene, methoxyphenol, cyclohexanone oxime, methyl ethyl ketone oxime, and mixtures thereof.

Unsaturated polyester resins are usually obtained by reacting unsaturated dibasic acid and divalent alcohol in the presence of vinyl monomer.
Examples of the unsaturated dibasic acid include phthalic anhydride, isophthalic acid, terephthalic acid, succinic acid, adipic acid, and azelaic acid. ), Sebacic acid, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, tetrabromophthalic anhydride, tetrachlorophthalic anhydride, het anhydride ( HET acid anhydride) (ie, chlorendic anhydride), endomethylenetetrahydrophthalic anhydride, etc.
Examples of the dihydric alcohol include ethylene glycol, propylene glycol, 1,3-butylene glycol, 1,6-hexanediol, Diethylene glycol, dipropylene glycol, neopentyl glycol, triethylene glycol, hydrogenated bisphenol A, bisphenol dihydroxypropyl ether, etc. Is mentioned.
Examples of the vinyl monomer include styrene, vinyltoluene, chlorostyrene, dially phthalate, trially cyanurate, methyl metacrylate, and the like. .

A phenolic resin is produced by reacting a phenolic compound with an aldehyde in the presence of a catalyst such as hydrochloric acid, oxalic acid, hexamethylenetetramine and the like. . Examples of the phenol compound include phenol, o-cresol, m-cresol, p-cresol, xylenol, and pt-butylphenol ( p-tert-butylphenol), resorcinol and the like.
In this reaction, a novolac type phenol resin is obtained under acidic catalyst conditions, and a resol type phenol resin is obtained under basic catalyst conditions.
Urea resins or melamine resins are usually produced by the reaction of urea or melamine with formaldehyde such as formalin in the presence of a basic catalyst.

  Urea / melamine resins are usually produced by the reaction of urea or melamine with formalin in the presence of a basic catalyst.

  Next, the production method of the present invention will be described with reference to a mixing test example of two kinds of particles using the production method of the present invention.

[Particles used in test examples]
・ Particle a
2 parts by weight of polyoxyethylene styryl phenyl ether, 3 parts by weight of a binder, 13.5 parts of a water-soluble carrier and 73.5 parts of a mineral carrier were mixed and kneaded with water. The kneaded product is granulated and dried by an extrusion granulator, and the obtained particles are further coated with a urethane resin obtained from an aromatic polyisocyanate and a polyether polyol, and a circle having a particle size of 500 to 1190 μm. Columnar particles a were obtained.
・ Particle b
6 parts by weight of an agrochemical active ingredient, 2 parts by weight of polyoxyethylene styryl phenyl ether, 5 parts by weight of a binder, 1 part by weight of a stabilizer, and 86 parts by weight of a mineral carrier were mixed and kneaded with water. The kneaded product was granulated with an extrusion granulator and dried to obtain cylindrical particles b having a particle size of 500 to 1190 μm.

[Mixing device used in test example]
As a container for containing particles, a cylindrical container made of SUS304 having a volume of 450 ml (diameter: about 7 cm, height: about 10 cm) was used. The cylindrical container has a removable lid at the top of the cylinder. The power mixer used was a tumbler shaker mixer (manufactured by Willy et Bacchofen (WAB), TURBULA Type T2C) having a container holding part rotatably attached to two different axes, and the rotational speed was It was operated at 42 rpm.

[Comparative Example 1]
In a 450 ml container (made of SUS304 with a diameter of about 7 cm and a height of about 10 cm) having a removable lid at the top, 150 g of particles a are placed in an atmosphere of an air temperature of 20 ° C. and a relative humidity of 30%. I put it in. The container lid was then closed.
At 20 ° C., the container charged with the particles was attached to the above-mentioned tumbler shaker mixer (manufactured by Willy et Bacofen (WAB), TURBULA Type T2C). Next, the cylindrical container was rotated at a rotation speed of 42 rpm for 5 minutes.
Thereafter, the cylindrical container was removed from the tumbler, shaker, and mixer, and the container was allowed to stand with its lid on top. The particles in the container were taken out from the upper part by 30 g in 10 parts (layers), and the contents of the agrochemical components in each part were analyzed. The standard deviation and the average value were calculated from the content analysis values. Furthermore, the degree of mixing (CV% = standard deviation ÷ average value × 100) was determined. The results are shown in Table 1.

Examples 1 to 3
In a 450 ml container (made of SUS304 with a diameter of about 7 cm and a height of about 10 cm) having a removable lid at the top, 150 g of particles a are placed in an atmosphere of an air temperature of 20 ° C. and a relative humidity of 30%. I put it in. Next, the container was transferred into a glass container humidified to a predetermined humidity, and left for a time sufficient to replace the interior of the container with humidified air. Thereafter, the lid of the container was closed.
At 20 ° C., the cylindrical container charged with the particles was attached to the above-described tumbler shaker mixer (manufactured by Willy et Bacofen (WAB), TURBULA Type T2C). Next, the cylindrical container was rotated at a rotation speed of 42 rpm for 5 minutes.
Thereafter, the cylindrical container was removed from the tumbler, shaker, and mixer, and the container was allowed to stand with its lid on top. The particles in the container were taken out from the upper part by 30 g in 10 parts (layers), and the contents of the agrochemical components in each part were analyzed. The standard deviation and the average value were calculated from the content analysis values. Furthermore, the degree of mixing (CV% = standard deviation ÷ average value × 100) was determined. The results are shown in Table 1.

  In any of Comparative Example 1 and Examples 1 to 3, there was no increase in fine powder due to particle breakage, that is, no change in the shape of particles a and particles b was observed.

  By the method for producing a particle mixture of the present invention, two or more types of particle mixtures with high uniformity can be obtained.

Claims (6)

A step of putting particles (A) composed of a plurality of components and particles (B) composed of a plurality of components into a container;
Humidifying the interior of the container; and
A method for producing a mixture of particles (A) and particles (B), comprising a step of rotating the vessel or rotating a stirring blade provided in the vessel. A step of putting particles (A) composed of a plurality of components and particles (B) composed of a plurality of components into a container;
Humidifying the interior of the container; and
A method for producing a mixture of particles (A) and particles (B), comprising a step of rotating the container.   The production method according to claim 1 or 2, wherein the particles (A) and the particles (B) are particles containing a surfactant. The particle (A) and the particle (B) are particles having a particle diameter in the range of 0.3 to 10 mm and a volume resistivity of 10 ¹⁰ Ω · m or more. The manufacturing method described in any one of 1-3.   The production method according to any one of claims 1 to 4, wherein the particles (A) are particles containing a pharmaceutical ingredient, an agrochemical ingredient or a fertilizer ingredient.   6. The production method according to claim 1, wherein the particles (A) are particles coated with a resin.