KR101130428B1 - Uniformly diffusible granular pesticide composition - Google Patents

Abstract

An object of the present invention is a granular pesticide which can be prepared by a simple method and exhibits the efficacy of the active pesticide active ingredient over a long period of time, and reduces the environmental load, thereby reducing or preventing the harmful effects caused by the pesticide active ingredient. It is to provide a uniformly diffusive granular pesticide formulation capable of uniformly dispersing the formulation throughout the paddy field by a simple spraying method. As a homogeneous diffusive granular pesticide preparation, it contains an acidic pesticide active ingredient, a cationic surfactant, and a basic substance, and contains a non-degradable granular pesticide composition which does not disintegrate in water within 30 minutes, and has a mass ratio of particles having a particle diameter of 3 mm or more. A granular composition having a particle size distribution of 80% by mass or more and having a floating property immediately after dropping on the water surface, but which collapses on the water surface within 30 minutes is provided. The acidic pesticide active ingredient is one of pKa 2-7, and the cationic surfactant is preferably gelled in water or exhibits swelling properties.

Description

Uniform Diffusive Granular Pesticide Formulation {UNIFORMLY DIFFUSIBLE GRANULAR PESTICIDE COMPOSITION}

The present invention relates to a uniformly diffusive granular pesticide preparation capable of exerting long-term efficacy and reducing or preventing weakening and reducing environmental load.

Conventionally, in order to reduce the weakening of the granular pesticide preparations containing an active pesticide active ingredient and to maintain the medicinal effect, various formulation methods that can control the dissolution of the pesticide active ingredient have been studied. For example, paraffin wax, thermoplastic resin or activated carbon, granular foam, clay minerals, etc. are combined and sustained release are proposed (Japanese Patent Laid-Open No. 63-35504, Japanese Patent Laid-Open). See Publication No. 63-45201 and Japanese Patent Laid-Open No. 2-288803.

However, such a conventional sustained release method is not necessarily effective, and the preparation of granular pesticide preparation is complicated, or the release of the pesticide composition is insufficient, and most of the active ingredient of the pesticide is not effectively used and remains in the pesticide composition as it is. There is a problem such that, more than necessary pesticide active ingredient is released into the environment, and as a result, the burden on the environment is increased.

In addition, for the purpose of stabilizing other active ingredients, after preparing the inner core, a method for producing granular agrochemicals for coating an active ingredient different from the inner core has also been proposed (see Japanese Patent Application Laid-Open No. 9-315903). The technique of the viable formulation which spreads the granular pesticide preparation which carried out the uniformly throughout the paddy field by spraying from the paddy field etc. is not established yet.

Under the circumstances, the present invention overcomes the problems associated with conventional granular agrochemical preparations and can be prepared by a simple method, while exhibiting the efficacy of the active pesticide active ingredient over a long period of time, and reducing environmental load, An object of the present invention is to provide a uniformly diffusive granular pesticide formulation capable of uniformly dispersing granular pesticide formulations capable of reducing or preventing the harmful effects caused by the pesticide active ingredient throughout the paddy field.

MEANS TO SOLVE THE PROBLEM As a result of earnestly researching about a uniform-diffusion granular pesticide formulation, the present inventors found that the composition contains the non-disintegrating granular pesticide which mix | blended a cationic surfactant and a basic substance with an acidic pesticide active ingredient, and has 80 mass of the particle diameter of 3 mm or more. It was found that the above problems were solved by having a particle size distribution of more than% and a property of floating on the surface and being able to disintegrate on the surface within 30 minutes. Thus, the present invention has been accomplished based on this knowledge.

That is, the present invention,

(1) A mass of particles having a particle diameter of 3 mm or more, containing an acidic pesticide active ingredient, a non-disintegrating pesticide granule which does not disintegrate in water, a surfactant, and a floating component within 30 minutes containing an active ingredient, a cationic surfactant, and a basic substance. A homogeneous diffusive granular pesticide formulation characterized by having a particle size distribution having a ratio of 80% by mass or more and a property of floating on the surface immediately after dropping on the surface, but disintegrating on the surface within 30 minutes;

(2) The uniformly diffusive granular pesticide preparation according to the above (1), wherein the acidic pesticide active ingredient is pKa 2 to 7,

(3) The uniformly diffusible granular pesticide preparation according to the above (1), wherein the acidic pesticide active ingredient is a herbicide;

(4) the uniformly diffusive granular pesticide preparation according to the above (3), wherein the herbicide is a sulfonylurea compound;

(5) herbicides of formula (I)

[Tue 1]

(Wherein R ¹ is a hydrogen atom, an alkyl group or an alkoxyalkyl group)

The uniformly diffusible granular pesticide preparation according to the above (3), which is a difluoromethanesulfonylanilide derivative or a salt thereof represented by

(6) The uniformly diffusible granular pesticide preparation according to the above (1), wherein the cationic surfactant gels in water or displays swelling properties.

(7) The uniformly diffusible granular pesticide preparation according to the above (1), wherein the basic substance is sodium hydrogen carbonate, sodium carbonate, calcium hydroxide, calcium carbonate, basic white carbon, or basic acidic clay.

(8) The uniformly diffusible granular pesticide preparation according to the above (1), wherein the floating component is an inorganic hollow body or a plastic hollow body;

(9) A non-destructive pesticide granule that does not disintegrate in water within 30 minutes containing an acidic pesticide active ingredient, a cationic surfactant, and a basic substance, together with a surfactant and a floating component, according to the granulation treatment; Method for producing a uniformly diffusive granular pesticide preparation, characterized in that the spherical shape having a particle diameter of 1 to 20 mm or a horizontally long shape having a short diameter of 1 to 20 mm and a long diameter of 3 to 40 mm,

(10) The manufacturing method according to the above (9), wherein the granulation treatment is carried out by extruding from a screen having a body diameter larger than the particle size or particle length of the non-invasive pesticide granular material,

(11) Non-destructive pesticide granules that do not disintegrate in water within 30 minutes containing an acidic pesticide active ingredient, a cationic surfactant, and a basic substance; , Spherical shape having a particle diameter of 1 to 20 mm or a horizontally long shape having a short diameter of 1 to 20 mm and a long diameter of 3 to 40 mm, and a method for producing a uniformly diffusive granular pesticide formulation, and

(12) It provides the manufacturing method as described in said (11) which performs granulation process by extruding and granulating from the screen of the body diameter larger than the particle size or particle length of a non-invasive pesticide granular material.

BRIEF DESCRIPTION OF THE DRAWINGS Explanatory drawing of the rice field pavement object of the application process of a pesticide preparation in the test example 2. FIG.

Hereinafter, the present invention will be described in detail.

The non-disintegrating pesticide granular material contained in the granular pesticide preparation of the present invention does not disintegrate in water within 30 minutes and maintains the granular prototype.

Although it does not restrict | limit especially about the acidic pesticide active ingredient used for this non-disintegrating pesticide granular material, Usually, it is a herbicide, a plant growth regulator, a fungicide, an insecticide, etc. Especially, the thing of the range of pKa 2-7 is preferable, Geometric isomers, optical isomers and the like.

Although it does not restrict | limit especially as a herbicide, The thing of pKa2-7 is preferable, Especially a sulfonylurea compound and General formula (I)

[Tue 2]

(Wherein R ¹ is a hydrogen atom, an alkyl group or an alkoxyalkyl group)

It is especially preferable that it consists of a difluoromethanesulfonylanilide derivative or its salt represented by these.

Examples of sulfonylurea compounds include 1- (4,6-dimethoxypyrimidin-2-yl) -3- [1-methyl-4- (2-methyl-2H-tetrazol-5-yl) pyra Sol-5-ylsulfonyl] urea (azimsulfuron), 1- (2-chloroimidazo [1,2-a] pyridin-3-ylsulfonyl) -3- (4,6-dimethoxypyrimidine- 2-yl) urea (imazosulfuron), ethyl = 5- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -1-methylpyrazole-4-carboxylite (pyrazosulfuron Ethyl), methyl = α- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -O-toluate (bensulfuronmethyl), 1- (4,6-dimethoxypyrimidine -2-yl) -3- (2-ethoxyphenoxysulfonyl) urea (ethoxysulfuron), 1- [2- (cyclopropylcarbonyl) anilinosulfonyl] -3- (4,6-dimethok Cypyrimidin-2-yl) urea (cyclosulfamuron), 1- (4,6-dimethoxy-1,3,5-triazin-2-yl) -3- [2- (2-methoxy Methoxy) phenylsulfonyl] urea (cynosulfuron), methyl = 3- (4-methoxy-6-methyl-1,3,5-triazine-2-ylcarbamoylsulfa Moyl) -2-tenoate (tifensulfuronmethyl), 2- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -N, N-dimethylnicotinamide (nicosulfuron), Methyl = 3-chloro-5- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -1-methylpyrazole-4-carboxylate (halosulfuronmethyl), 1- (4 , 6-dimethoxypyrimidin-2-yl) -3- (3-trifluoromethyl-2-pyridylsulfonyl) urea (furazulfuron), 1- (4,6-dimethoxypyrimidine-2 -Yl) -3- (3-ethylsulfonyl-2-pyridylsulfonyl) urea (rimsulfuron), and the like.

Moreover, as an example of a difluoromethanesulfonylanilide derivative or its salt, the compound described in Unexamined-Japanese-Patent No. 2000-44546, for example, 2-[(4,6-dimethoxypyrimidin-2-yl) hydride Oxymethyl] -N-difluoromethanesulfonylanilide, 2-[(4,6-dimethoxypyrimidin-2-yl) hydroxymethyl] -6-methoxymethyl-N-difluoromethanesulfonylanilide And 2-[(4,6-dimethoxypyrimidin-2-yl) hydroxymethyl] -6-ethyl-N-difluoromethanesulfonylanilide and the like.

Examples of other herbicides include 2-methyl-4-chlorophenoxythioacetic acid-S-ethyl (phenothiol), α- (2-naphthoxy) propionanilide (naproanilide), 5- (2,4 -Dichlorophenoxy) -2-nitrobenzoate (biphenox), S- (4-chlorobenzyl) -N, N-diethylthiocarbamate (benthiocarb), S-benzyl = 1,2-dimethyl Propyl (ethyl) thiocarbamate (esprocarb), S-ethylhexahydro-1H-azepine-1-carbothioate (morinate), S-1-methyl-1-phenylethyl = piperizine- 1-carbothioic acid (dimepiperate), O-3-tert-butylphenyl = 6-methoxy-2-pyridyl (methyl) thiocarbamate (pyrivivecarb), 2-chloro-2 ', 6'-diethyl-N- (butoxymethyl) acetanilide (butacro), 2-chloro-2 ', 6'-diethyl-N- (2-propoxyethyl) acetanilide (pretilacro ), (RS) -2-Buromo-N- (α, α-dimethylbenzyl) -3,3-dimethylbutylamide (Buromobutide), 2-benzothiazol-2-yloxy-N- Thiacetanilide (mefenacet), 1- (α, α-dimethylbenzyl) -3- (para-tril) urea (dimeron), 2-methylthio-4,6-bis (ethylamino) -s- Triazine (cymetrin), 2-methylthio-4,6-bis (isopropylamino) -s-triazine (promethrin), 2-methylthio-4-ethylamino-6- (1,2 -Dimethylpropylamino) -s-triazine (dimethamethrin), 2,4-dichlorophenyl-3'-methoxy-4'-nitrophenylether (chloromethoxyyl), 5-tert-butyl-3 -(2,4-dichloro-5-isopropoxyphenyl) -1,3,4-oxadiazol-2 (3H) -one (oxadiazone), 4- (2,4-dichlorobenzoyl) -1 , 3-dimethyl-5-pyrazoryl-p-toluenesulfonate (pyrazolate), 2- [4- (2,4-dichlorobenzoyl) -1,3-dimethylpyrazol-5-yloxy] acetphenone (Pyrazoxifen), (RS) -2- (2,4-dichloro-m-triloxy) propionanilide (chrommeprop), 2- [4- [2,4-dichloro-m-toluoyl] -1,3-dimethylpyrazol-5-yloxy] -4'-methylacetphenone (benzophenad), S, S'-dimethyl = 2-difluoromethyl-4-isobutyl-6-trifluoromethylpyridine-3,5-dicarbothioic acid (dithiophyll), 2-chloro-N- (3-methoxy-2-tenyl) -2 ' , 6'-dimethylacetanilide (tenyl chloro), butyl = (R) -2- [4- (4-cyano-2- fluorophenoxy) phenoxy] propionate (thihalohof butyl), 3- [1- (3,5-dichlorophenyl) -1-methylethyl] -2,3-dihydro-6-methyl-5-phenyl-4H-1,3-oxazin-4-one (oxazik) Romepon), 3- (4-chloro-5-cyclopentyloxy-2-fluorophenyl) -5-isopropyriden-1,3-oxazolidine-2,4-dione (pentoxazone), 1 -(Diethylcarbamoyl) -3- (2,4,6-trimethylphenylsulfonyl) -1,2,4-triazole (carpentrol), methyl = 2-[(4,6-dimethok Cipyrimidin-2-yl) oxy] -6-[(E) -1- (methoxyimino) ethyl] benzoate (pyriminobacmethyl) and the like.

Although it does not restrict | limit especially as a plant growth regulator, 4'-chloro-2 '-((alpha) -hydroxybenzyl) isonicotinanilide (inbenide), (2RS, 3RS) -1- (4-chlorophenyl) -4 , 4-dimethyl-2- (1H-1,2,4-triazol-1-yl) pentan-3-ol (paclobutrazole), (E)-(S) -1- (4-chlorophenyl ) -4,4-dimethyl-2- (1H-1,2,4-triazol-1-yl) penta-1-en-3-ol (uniconazole), calcium = 3-oxide-5- Oxo-4-propionylcyclohexa-3-enecarboxylate (prophexadione calcium salt), maleic acid hydrazide choline, etc. are mentioned. Of these, pKa 2 to 7 are particularly suitably used.

The fungicide is not particularly limited, but may be O, O-diisopropyl-S-benzylthiophosphate (IBP), 3'-isopropoxy-2-methylbenzanilide (mepronyl), α, α, α-tri Fluoro-3'-isopropoxy-O-toluanilide (flutranil), 3,4,5,6-tetrachloro-N- (2,3-dichlorophenyl) phthalamic acid (teclophthalam), 1- (4-Chlorobenzyl) -1-cyclopentyl-3-phenylurea (pencyclone), 6- (3,5-dichloro-4-methylphenyl) -3 (2H) -pyridazinone (diclomezin), methyl = N- (2-methoxyacetyl) -N- (2,6-xyryl) -DL-alanine (methacryl), (E) -4-chloro-α, α, α-trifluor-N -(1-imidazol-1-yl-2-propoxyethylidene) -o-toluidine (triflumizol), kasugamycin, varidamycin, 3-aryloxy-1, 2-benzoisothiazole- 1,1-dioxide (probenazole), diisopropyl-1,3-dithioran-2-iridene-maronate (isoprothiolane), 5-methyl-1,2,4-triazolo [ 3,4-b] benzothiazole (tricycle Sol), 1,2,5,6-tetrahydropyrrolo [3,2,1-ij] quinolin-4-one (pyroquilon), 5-ethyl-5,8-dihydro-8-oxo [1 , 3] dioxol [4,5-g] chinoline-7-carboxylic acid (oxonic acid), (Z) -2'-methylacetphenone = 4,6-dimethylpyrimidin-2-ylhydrazone-4, 5,6,7-tetrachlorophthalide (ferimzone), 3- (3,5-dichlorophenyl) -N-isopropyl-2,4-dioxoimidazolidine-1-carboxamide (if Rodion), and the like. Of these, pKa 2 to 7 are particularly suitably used.

The insecticide is not particularly limited, but may be O, O-dimethyl-O- (3-methyl-4-nitrophenyl) thiophosphate (MEP), (2-isopropyl-4-methylpyrimidyl-6) -diethylthiophosphate (Diazinone), 1-naphthyl-N-methylcarbamate (NAC), O, O-diethyl-O- (3-oxo-2-phenyl-2H-pyridazin-6-yl) phosphothio Eate (pyridapention), O, O-dimethyl-O-3,5,6-trichloro-2-pyridylphosphothioate (chlorpyriphosmethyl), dimethyldicarbetoxyethyldithiophosphate (marathon) ), O, O-dimethyl-S- (N-methylcarbamoylmethyl) dithiophosphate (dimethate), O, O-dipropyl-O-4-methylthiophenylphosphate (propaphos), O , S-dimethyl-N-acetylphosphoramide thioate (acetate), ethyl paranitrophenylthio benzene phosphonate (EPN), 2-sec-butylphenyl-N-methylcarbamate (BPMC), 2 , 3-dihydro-2,2-dimethyl-7-benzo [b] pranyl = N-dibutylaminothio-N-meth Carbamate (carbosulfan), ethyl = N- [2,3-dihydro-2,2-dimethylbenzofuran-7-yloxycarbonyl (methyl) aminothio] -N-isopropyl-β-al Raninate (benfuracarb), (RS) -α-cyano-3-phenoxybenzyl = (RS) -2,2-dichloro-1- (4-ethoxyphenyl) cyclopropanecarboxylate (cycloprop Trine), 2- (4-ethoxyphenyl) -2-methylpropyl = 3-phenoxybenzyl = ether (etfenprox), 1,3-bis (carbamoyl thio) -2- (N, N- Dimethylamino) propane hydrochloride (cartop), 5-dimethylamino-1,2,3-trioxyoxalate (thiocyclo), S, S'-2-dimethylaminotrimethylene = di (benzenethiosulfonate) (Bensultop), 2-tert-butylimino-3-isopropyl-5-phenyl-1,3,5,6-tetrahydro-2H-1,3,5-thiadiazin-4-one (part Propazine) and the like. Of these, pKa 2 to 7 are particularly suitably used.

When the acidic agrochemical active ingredient of the predetermined pKa is used, pKa of the ingredient is, for example, published on January 20, 33, Maruzen, Experimental Chemistry Course 5 (Thermal Measurement and Equilibrium) p469 to p474. It measures by the method etc. which were described.

Although it does not restrict | limit especially about the cationic surfactant used for this invention, Preferably, an amine salt system, a pyridinium salt system, a quaternary ammonium salt system, etc. are mentioned.

Examples of the amine salt-based cationic surfactant include laurylamine hydrochloride, stearylamine hydrochloride, oleylamine acetate, stearylamine acetate, stearylaminopropylamine acetate, and the like.

Examples of pyridinium salt-based cationic surfactants include laurylpyridinium chloride, myristylpyridinium chloride, cetylpyridinium chloride, and the like.

Examples of quaternary ammonium salt-based cationic surfactants include alkyldimethylbenzyl ammonium chloride, lauryltrimethylammonium chloride, cetyltrimethylammonium chloride, stearyltrimethylammonium chloride, dilauryldimethylammonium chloride, dioleyldimethylammonium chloride, and dicoyldimethylammonium. Chloride, distearyldimethylammonium chloride, lauryldihydroxyethylmethylammonium chloride, oleylbispolyoxyethylenemethylammonium chloride, stearylhydroxyethyldimethylammonium chloride, lauryldimethylbenzylammonium chloride, lauroylamino Propyl dimethyl ethyl ammonium sulphate, lauroylamino propyl dimethyl hydroxyethyl ammonium perchlorate, etc. are mentioned.

Particularly suitable as cationic surfactants are those which gelatinize in water or exhibit swelling properties, for example, dialkyldimethylammonium chlorides, the alkyl moieties of which are C8 to C22, especially dilauryldimethylammonium chloride and diol. Rail dimethylammonium chloride, dicoyldimethylammonium chloride, distearyldimethylammonium chloride and the like. These surfactants may be used alone, or may be used in combination of two or more thereof.

Although the basic substance used for this invention is not restrict | limited, Preferably, when it is set as 1 mass% aqueous solution or 1 mass% aqueous suspension, it is preferable that pH is 7.5 or more, especially 9-12. As such a thing, the hydroxide of an alkali metal or an alkaline earth metal, an alkali metal salt, an alkaline earth metal salt, the compound containing it, minerals, etc. are mentioned. Specific examples thereof include sodium hydroxide, potassium hydroxide, sodium hydrogen carbonate, sodium carbonate, calcium hydroxide, calcium carbonate, calcium oxide, basic white carbon, basic acid clay, and the like. In particular, sodium hydrogen carbonate, sodium carbonate, calcium hydroxide and calcium carbonate. Preferred are basic white carbon and basic acidic clay. These basic substances may be used independently, and may be used in combination of 2 or more type.

The surfactant used in the present invention is not particularly limited, and examples thereof include polyoxyalkylene glycol higher fatty acid esters, polyoxyalkylene alkyl ethers, polyoxyalkylene alkyl aryl ethers, polyoxyalkylene alkyl aryl phenyl ethers, Nonionic surfactants, such as sorbitan monoalkylate, acetylene glycol, and polyoxyethylene acetylene glycol, alkylaryl sulfonate, dialkyl sulfonate, alkyl sulfate ester salt, alkyl phosphate ester salt, alkylaryl phosphate, alkylaryl phosphate ester salt , Polyoxyalkylene alkyl ether sulfate ester salt, naphthalene sulfonate and its condensate, alkyl naphthalene sulfonate and its condensate, lignin sulfonate, acrylic acid-itaconic acid copolymer, methacrylic acid-itaconic acid copolymer, maleic acid Polycarboxylic acid type polymer interfaces such as -styrene copolymer, maleic acid-isobutylene copolymer, and alkali metal salts thereof Anionic surfactants, such as an active agent and polyoxyalkylene arylphenyl ether sulfate ester salt, etc. are mentioned. These may be used independently and may be used in combination of 2 or more type.

The floating material used in the present invention is not particularly limited as long as it floats on the water itself, and the inorganic material is, for example, a glassy hollow body, a foamed pearlite, a foamed fly ash, Inorganic hollow bodies such as permicurite, calcined permicurite, silas balloon, microballoon, and cenospea, and the like, are also plastics, lead, solid paraffin, starch containing foam, cork, wood chips, Organic solvents etc. which have light specific gravity, such as a plant piece, such as corn cove, and polybutene, are mentioned, respectively. In particular, inorganic hollow bodies such as glassy hollow bodies and shirasu heating foams, or plastic hollow bodies such as vinylidene chloride-acrylonitrile copolymer plastic balloons and acrylonitrile-based plastic balloons are preferable. These may be used independently and may be used in combination of 2 or more type.

The uniformly diffusive granular pesticide preparation of the present invention may contain, as necessary, additional components usually used in pesticide preparations. As this additive component, an extender, an auxiliary component, etc. are used.

As the extender, solid carriers such as mineral carriers, water-soluble salts, and the like are used. Specifically, clays, calcium carbonate, bentonite, talc, diatomaceous earth, acidic clay, silica sand, granular calcium carbonate, granular diatomaceous earth, calcium stearate, white carbon And potassium chloride, anhydrous sodium sulfate, potassium sulfate, urea, ammonium sulfate, sodium benzoate and the like. These may be used independently and may be used in combination of 2 or more type.

As an auxiliary component, for example, a binder for preparing a granular composition, specifically, carboxymethyl cellulose sodium salt, dextrin, water soluble starch, chianthac, guar gum, sucrose, polyvinylpyrrolidone, polyvinyl alcohol, poly Sodium acrylate, polyethylene glycol with an average molecular weight of 6000 to 20000, polyethylene oxide with an average molecular weight of 100,000 to 5 million, and the like. Moreover, the organic solvent used when dissolving an acidic pesticide active ingredient and a cationic surfactant, and making it adsorb | suck to a support | carrier, specifically, alkyl naphthalene, dimethylformamide, dimethyl sulfoxide, N-methyl- 2-pyrrolidone, N-jade Tilpyrrolidone, polyhydric alcohol, silicone oil, etc. are mentioned. If necessary, a stabilizer or the like may be used. These may be used independently and may be used in combination of 2 or more type.

In the uniformly diffusive granular pesticide preparation of the present invention, the composition ratio of the non-disintegrating pesticide granular product is usually 0.1-40 mass% of the acidic pesticide active ingredient, 1-40 mass% of the cationic surfactant, and 0.1-95 mass of the basic substance. It is chosen in the range of%, Preferably it adjusts so that pH of the 1 mass% aqueous suspension of a non-disintegrating pesticide granular material may be 5 or more normally, Preferably it is 7 or more, More preferably, it is 7.5-11.5.

Moreover, about the composition ratio of the uniformly diffusible granular pesticide preparation of this invention, 1-70 mass% of non-degradable pesticide granular substances, 0-50 mass% of pesticide active ingredients, 0.1-30 mass% of surfactant, and floating property 0.1-50 mass% of components, 0-95 mass% of an extender, Preferably it is 5-70 mass%, 0-50 mass% of auxiliary components, Preferably it is selected in the range of 0.1-30 mass%, More preferably, 1 The specific gravity of the particles is selected to be less than 1 and in a range sufficient to float on the water surface.

The uniformly diffusive granular pesticide preparation of the present invention disintegrates within 30 minutes after treatment in a package, and gradually precipitates the non-degradable pesticide granular material contained in itself uniformly in the package during the disintegration. It is a biocidal release-controlled pesticide that slows the elution of the pesticide active ingredient contained in water, but by incorporating the pesticide active ingredient that does not want to be sustained into the homogeneous diffuse granular pesticide preparation separately from the non-disintegrating pesticide granules. In addition, it is possible to design the dissolution properties for each active pesticide ingredient.

The present invention also includes a mixed pesticide formulation comprising a homogeneous diffusive granular pesticide formulation and a homogeneous diffusive granular pesticide formulation having neither a cationic surfactant nor a basic substance in a mass ratio of 1: 9 to 9: 1. do.

In the uniformly diffusive granular agrochemical preparation of the present invention, the size of itself is usually 1 to 20 mm in particle size, preferably 3 to 10 mm in the shape of a sphere, and is usually 1 to 20 mm in short diameter. Preferably it is 3-10 mm, long diameter 3-40 mm, Preferably it is 5-30 mm, and the size of the non-degradable pesticide granular material contained in this pesticide formulation is a spherical shape, usually 0.01- particle size 5 mm, Preferably it is 0.1-3 mm, In a horizontally long shape, Usually, short diameter 0.1-10 mm, Preferably 0.5-7 mm, Long diameter 0.3-30 mm, Preferably it is 1.5-20 mm desirable.

The method for preparing the uniformly diffusive granular pesticide preparation of the present invention and the non-disintegrating pesticide granular material contained in the formulation is not particularly limited. For example, a conventionally known rolling granulation method, extrusion granulation method, Coating assembly method and the like.

As a method for producing a uniformly diffusive granular pesticide preparation of the present invention, preferably, a non-degradable pesticide granule which does not disintegrate in water within 30 minutes containing an acidic pesticide active ingredient, a cationic surfactant and a basic substance is used as a surfactant and Along with the floating component, a method of forming a spherical shape having a particle diameter of 1 to 20 mm or a horizontally long shape having a short diameter of 1 to 20 mm and a long diameter of 3 to 40 mm can be mentioned.

(Production of Non-Destructive Pesticide Granules)

In the electric granulation method, an acidic pesticide active ingredient, a cationic surfactant, and a basic substance are added to an electric granulator together with auxiliary components such as a binder and an extender to prepare a powder granular raw material, and an appropriate amount of water or a binder is added to the powder granular raw material. It consists of the process of preparing the granular composition which has a target particle size and particle length by gradually adding melt | dissolving aqueous solution, and a process of coating this granular composition on the surface as needed, drying, and then sifting out sieve.

The extrusion granulation method is an air mill or mechanochemical milling of an acidic pesticide active ingredient, a cationic surfactant, and a basic substance together with auxiliary ingredients such as a binder and an extender to prepare a powdery raw material, and an appropriate amount for the powdery raw material. And kneading the mixture to which water is added, using a kneader, an extrusion granulator, or the like, and then extruding the granulated composition from a screen in which the diameter of the body is set so as to have a target particle size and particle length. The granular composition is formed by coating a film forming material on the surface of the granular composition as necessary, drying and sifting it out.

The coating assembly method is an air mill or mechanochemical milling process of an acidic pesticide active ingredient, a basic substance, and auxiliary components such as a cationic surfactant and an extender used as needed to prepare a powdery raw material. Into the oil-absorbing granules obtained by mixing the oil-absorbing granules having the particle length into a conical screw-type mixer and simultaneously spraying auxiliary components such as a cationic surfactant diluted with a solvent and a binder to be used, if necessary. It consists of the process of coating the powdery raw material obtained in the above, and preparing a granular composition, and drying this granular composition as needed, and then sifting it out.

(Manufacture of granular pesticide preparation)

Extrusion granulation method is a biaxial kneader with non-disintegrating pesticide granules, surfactants and floating components obtained by the above-mentioned manufacturing method together with auxiliary ingredients such as extenders, binders and stabilizers and pesticide active ingredients used as necessary. A process of preparing a granular composition by extruding the mixture obtained by adding an appropriate amount of water with the same kneading machine, an extrusion granulator, etc. from a screen having a body diameter larger than the particle size or particle length of the non-invasive pesticide granules and the granular composition If necessary, a film forming material is coated on the surface, dried, and sifted.

In the electric granulation method, the non-disintegrating pesticide granules, surfactants and floating components obtained by the above-mentioned manufacturing method are added to the electric granulator together with auxiliary ingredients such as extenders, binders and stabilizers and pesticide active ingredients used as necessary. A step of preparing a powder granular raw material, a step of gradually adding an aqueous solution in which a suitable amount of water or a binder is dissolved in the powder granular raw material to prepare a granular composition having a target particle size and particle length, and the granular composition as necessary. The film-forming material is coated on the surface, dried and sifted out.

In these production methods, the drying treatment is preferably performed by a suitable drying apparatus such as a fluidized bed drying apparatus or a vacuum drying apparatus.

In the homogeneous diffusive granular pesticide preparation of the present invention, the acidic pesticide active ingredient includes pKa 2-7, herbicide, for example, a herbicide composed of a sulfonylurea-based compound, in particular, a compound represented by general formula (I). It is preferable to use a fluoromethanesulfonylanilide derivative or a salt thereof and gelling in water as a cationic surfactant or displaying swelling property.

Hereinafter, although an Example and a test example demonstrate this invention in detail, this invention is not restrict | limited at all by these examples. In addition, in each example, a part represents a mass part.

The pesticide active ingredients used in the examples are all pKa 2 to 7, the basic substances are all 1 mass% aqueous solution or 1 mass% aqueous suspension, and the pH is 7.5 or more, and the non-disintegrating pesticide granules are all 1 mass%. The suspension had a pH above 5.

Moreover, all the cationic surfactants used in Examples 1, 7, 9-10 were gelatinized in water.

In addition, the homogeneous diffusive granular pesticide preparation obtained in each Example floated on the water immediately after dropping on the water surface, but collapsed within 30 minutes, and the non-invasive pesticide granules precipitated.

Example 1

6.25 parts of bensulfuronmethyl (pKa 5.03), 6.25 parts of distearyl dimethylammonium chloride, 6.25 parts of dilauryldimethylammonium chloride, 68.75 parts of calcium carbonate, 6.25 parts of polyvinyl alcohol, and 6.25 parts of α-starch, Pulverized with an impact mill. After kneading the obtained powder by adding an appropriate amount of water in a high speed stirrer, it is extruded from a screen having a diameter of 0.5 mm using a dome type granulator, and the granulated product is left to dry at 60 ° C. Agrochemical granules having a diameter of 0.4 to 0.6 mm and a length of 1 to 6 mm containing 6.25 mass% of bensulfuron methyl were obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 32 parts of non-disintegrating pesticide granules, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, and a plastic hollow vinylidene chloride acrylonitrile copolymer plastic balloon [Matsumoto micro spare F-30E (brand name) ), Matsumoto Yuji Pharmaceutical Co., Ltd.] 14 parts, 20 parts of anhydrous sodium sulfate, 40.9 parts of urea were kneaded with a twin-shaft kneader, and then extruded to form a screen with a diameter of 5 mm. And granulated so as to be of a target size, dried with a fluid bed dryer at a product temperature of 60 ° C., and sifted to sieve a diameter of 3 to 7 mm and a length of 3 to 20 mm. The granular material containing 2 mass% of bensulfuron methyl was obtained as a uniformly diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 2

A mixture of 6.25 parts of bensulfuronmethyl (pKa 5.03), 12.5 parts of dioleyldimethylammonium chloride, 62.5 parts of calcium carbonate and 12.5 parts of bentonite was pulverized with an impact mill. The obtained powder was kneaded by adding 12.5 parts of an acrylic emulsion containing 50% of solid content and an appropriate amount of water in a high speed stirrer, and then extrusion-assembled from a screen having a diameter of 0.5 mm using a dome type granulator, and granulating the granulated product at 60 ° C. It left still and dried and obtained the pesticide granular material of 0.4-0.6 mm in diameter and 1-6 mm in length containing 6.25 mass% of bensulfuron methyl. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 32 parts of this non-disintegrated pesticide granular material, 32 parts of mefenacet finely ground with an air mill, 1 part of dioctylsulfosuccinate, 2 parts of polyoxyethylene acetylene glycol, 3 parts of enzyme-modified dextrin, and Example 1 12 parts of the hollow plastic body, 5 parts of bentonite, 10 parts of anhydrous sodium sulfate, and 13.2 parts of urea were kneaded with a biaxial kneader, and then extruded from a screen having a diameter of 5 mm using an extrusion granulator. After assembling, sizing to a target size, drying with a fluid bed dryer at a temperature of 60 ° C., sifting and sifting, 2% by mass of bensulfuronmethyl having a diameter of 3 to 7 mm and a length of 3 to 20 mm, mefenacet The granular material containing 32 mass% was obtained as a uniformly diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 3

In the general formula (I), 10 parts of a compound in which R ¹ is an ethyl group (hereinafter referred to as compound A. pKa 6.17) and 1.7 parts of basic white carbon were mixed uniformly to prepare a compound A-containing powder finely ground with an air mill.

75 parts of diatomaceous earth having a particle size of 16 to 35 mesh (1000 to 425 μm) was added to the conical screw type mixer, and mixed separately beforehand. 10 parts of dilauryldimethylammonium chloride, 2 parts of propylene glycol, and polypropylene glycol (molecular weight: 1000) 1.3 The calcined surfactant solution prepared by heating and mixing the parts with a propeller mixer was introduced. Immediately after the end of the charge, the compound A-containing powder was added, uniformly mixed to form a granule, and the granulated material was aged with a 60 ° C borane-type drier to obtain a pesticide granule having a particle diameter of 0.4 to 1.1 mm. . The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 30 parts of this non-disintegrating pesticide granular material, 3 parts of sodium dibutylnaphthalene sulfonate, 2 parts of lauryl sulfate, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, 1 part of sodium polyacrylate, white carbon 2 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, and 34.9 parts of urea were kneaded with a biaxial kneader, and then a screen having a diameter of 5 mm using an extrusion granulator. After extrusion granulation and sizing to a target size, it is dried with a fluid bed dryer at a product temperature of 60 ° C. and sifted to contain 3% by mass of compound A having a diameter of 3 to 7 mm and a length of 3 to 20 mm. The granular material was obtained as a uniformly diffusive granular pesticide. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 4

7.5 parts of compound A (pKa 6.17), 10 parts of N-methyl-2-pyrrolidone, and 10 parts of dioleyldimethylammonium chloride were mixed with a propeller mixer to prepare a compound A containing solution. The obtained solution was made to adsorb | suck 75 parts of basic acidic clay of particle size 16-35 mesh (1000-425 micrometers) whose pH of a 1% water suspension is 7-10, and obtained the pesticide granule of the particle diameter 0.4-1.1 mm. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 40 parts of this non-disintegrating pesticide granular material, 3 parts of sodium dibutylnaphthalene sulfonate, 2 parts of lauryl sulfate, 2 parts of polyoxyethylene acetylene glycol, 0.7 parts of sodium polyacrylate, spherical hollow glass [Fuji balloon (brand name) ), Fuji Silysia Chemical Co., Ltd.] 20 parts, 15 parts of anhydrous sodium sulfate and 17.3 parts of urea are uniformly mixed in a high speed stirrer, and kneaded by adding an appropriate amount of water, and then the obtained mixture is prepared using a basket-type granulator. Compound A 3 having a diameter of 3 to 7 mm and a length of 3 to 20 mm by extrusion-assembling from a screen having a diameter of 5 mm and sizing to a target size, followed by drying with a fluid bed dryer at a temperature of 60 ° C. and sieving. The granular material containing mass% was obtained as a uniformly diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 5

In the general formula (I), R ¹ is a methoxymethyl group (hereinafter referred to as compound B. pKa 5.75) 10 parts, distearyl dimethylammonium chloride 6.7 parts, dilauryldimethylammonium chloride 6.7 parts, calcium carbonate 63.2 parts, poly The mixture which mixed 6.7 parts of vinyl alcohol and 6.7 parts of (alpha) starches uniformly was grind | pulverized by the impact grinder. After kneading the mixture obtained by adding an appropriate amount of water to the obtained powder with a high speed stirrer, using a domed granulator, extrusion granulation was carried out from a screen having a diameter of 0.5 mm. The pesticide granular material of 0.4-0.6 mm in diameter and 1-6 mm in length containing was obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 30 parts of this non-destructive pesticide granular material, 1 part of polyoxyethylene acetylene glycol, 2 parts of polyoxyethylene polyoxypropylene block polymer, 3 parts of polyoxyethylene styrylphenyl ether phosphate amine salt, 3 parts of enzyme-modified dextrin 14 parts of the plastic hollow body used in Example 1, 5 parts of bentonite, 20 parts of anhydrous sodium sulfate, and 30.9 parts of urea were kneaded with a twin-shaft kneader, and then a diameter of 5 was obtained using an extrusion granulator. 3 mass% of compound B of diameter 3-7 mm and length 3-20 mm by extrusion-granulation from the screen of mm, sizing to a target size, drying with a fluid bed drier at sieve temperature 60 degreeC, and screening. The granular material containing was obtained as a homogeneous diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 6

The mixture which uniformly mixed 6.25 parts of compound B (pKa 5.75), 12.5 parts of distearyl dimethylammonium chloride, 62.5 parts of calcium carbonate, and 12.5 parts of bentonite was grind | pulverized by the impact grinder. The mixture obtained by adding 6.25 parts of acrylic emulsion and an appropriate amount of water to the obtained powder was kneaded with a high speed stirrer, and then extruded and granulated from a screen having a diameter of 0.5 mm using a dome type granulator, and the granulated substance was left to dry at 60 ° C to give a compound. The pesticide granular material of 0.4-0.6 mm in diameter and 1-6 mm in length containing 6.25 mass% of B was obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 32 parts of this non-destructive pesticide granular material, 1 part of Compound B finely ground with an air mill, 1 part of polyoxyethylene acetylene glycol, 2 parts of polyoxyethylene polyoxypropylene block polymer, polyoxyethylene styrylphenyl ether phosphoric acid A mixture of 3 parts of amine salt, 3 parts of enzyme-modified dextrin, 14 parts of the plastic hollow body used in Example 1, 5 parts of bentonite, 20 parts of anhydrous sodium sulfate, and 30.9 parts of element was kneaded with a biaxial kneader. Then, extrusion granulation is carried out from a screen having a diameter of 5 mm using an extrusion granulator, and the granules are granulated to a target size, dried with a fluid bed drier at a temperature of 60 ° C., and sifted to sieve, diameter 3-7 mm, The granular material containing 3 mass% of compound B of length 3-20 mm was obtained as a uniformly diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 7

The mixture which mixed 10 parts of compound B (pKa 5.75), 13.3 parts of distearyl dimethylammonium chloride, 56.9 parts of calcium carbonate, and 13.3 parts of bentonite was grind | pulverized by the impact grinder. The mixture obtained by adding 13 parts of an acrylic emulsion containing 50% solids and an appropriate amount of water to the obtained powder was kneaded with a high speed stirrer, and then extruded and granulated from a screen having a diameter of 0.5 mm using a dome type granulator, and granulated material was 60 It left still to dry at degreeC, and obtained the pesticide granular material of 0.4-0.6 mm in diameter and 1-6 mm in length containing 10 mass% of compound B. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 30 parts of this non-disintegrated pesticide granular material, 8 parts of pentrazamide finely ground with an air mill, 5 parts of sodium dibutylnaphthalenesulfonate, 1 part of lauryl sulfate, 3 parts of polyoxyethylene acetylene glycol, and enzyme-modified dextrin 2 Part, 0.5 parts of sodium polyacrylate, 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, and 28.4 parts of urea were kneaded with a biaxial kneader, and then kneaded with an extrusion granulator. Compound B having a diameter of 3 to 7 mm and a length of 3 to 20 mm by extrusion-assembling from a screen having a diameter of 5 mm and sizing to a target size, followed by drying with a fluid bed dryer at a temperature of 60 ° C. and sieving. Granular material containing 3 mass% and 8 mass% of pentrazamide was obtained as a uniformly diffusive granular pesticide preparation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 8

A mixture of 6.25 parts of pyrazosulfuronethyl (pKa 3.91), 6.25 parts of cetyltrimethylammonium chloride, 68.75 parts of calcium carbonate and 18.75 parts of polyvinyl alcohol was ground by an impact mill. The obtained powder was kneaded by adding an appropriate amount of water in a high speed stirrer, and then extruded and granulated from a screen having a diameter of 0.5 mm using a dome type granulator, and the granulated substance was left to dry at 60 ° C. to yield 6.25 mass of pyrazosulfuronethyl. The pesticide granules of 0.4-0.6 mm in diameter and 1-6 mm in length containing% were obtained. The pesticide granules were dropped into water, and after 30 minutes, the disintegrated state of the particles was observed. The disintegrated particles were not identified, and were determined to be non-disintegrated.

Next, 16 parts of this non-disintegrating pesticide granular material, 5 parts of butylnaphthalene sulfonic acid formalin condensate sodium salt, 1 part of polyoxyethylene acetylene glycol, 0.5 part of sodium polyacrylate, 14 parts of the plastic hollow body used in Example 1, anhydrous 20 parts of sodium sulfate and 55.4 parts of urea were kneaded in a high speed stirrer, and then extruded and assembled from a screen having a diameter of 5 mm using an extrusion granulator. It dried with the fluidized bed drier at 60 degreeC, and sifted out, and obtained the granular material containing 1 mass% of pyrazosulfuron ethyl of diameter 3-7 mm and length 3-20 mm as a uniformly diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 9

A mixture of 20 parts of tricyclazole (pKa 1.6), 15 parts of distearyldimethylammonium chloride, 55 parts of calcium carbonate, and 10 parts of polyvinyl alcohol was pulverized with an impact mill. The obtained powder was kneaded by adding an appropriate amount of water in a high speed stirrer, and then extruded and granulated from a screen having a diameter of 0.7 mm using a dome type granulator, and the granulated substance was left to dry at 60 ° C to obtain 20% by mass of tricyclazole. The pesticide granular material of 0.6-0.8 mm in diameter and 2-9 mm in length containing was obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 40 parts of this non-disintegrating pesticide granular material, 5 parts of butylnaphthalene sulfonic acid formalin condensate sodium salt, 1 part of polyoxyethylene acetylene glycol, 0.5 part of sodium polyacrylate, an acrylonitrile-based plastic balloon [Matsumoto Micro Spare F-80E (trade name), manufactured by Matsumoto Yuji Pharmaceutical Co., Ltd.], 14 parts, 20 parts of anhydrous sodium sulfate, 31.4 parts of urea were kneaded with a high speed stirrer, and then 5 mm in diameter using an extrusion granulator. 8 mass% of tricyclazole 3-3 mm in diameter and 3-20 mm in length by carrying out the extrusion granulation from the screen of the screen, sizing to a target size, drying with a fluid bed drier at sieve temperature 60 degreeC, and sifting. The granular material containing was obtained as a homogeneous diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Example 10

The mixture which uniformly mixed 20 parts of PHC (pKa 11.6), 15 parts of distearyl dimethylammonium chloride, 55 parts of calcium carbonate, and 10 parts of polyvinyl alcohol was ground with an impact mill. After kneading the mixture obtained by adding an appropriate amount of water to the obtained powder with a high speed stirrer, the granules were extruded from a screen having a diameter of 0.7 mm using a domed granulator, and the granulated materials were left to dry at 60 ° C to contain 20% by mass of PHC. 0.6-0.8 mm in diameter and the pesticide granular material of length 2-9 mm were obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 40 parts of this non-disintegrating pesticide granular material, 5 parts of butyl naphthalene sulfonic acid formalin condensate sodium salt, 1 part polyoxyethylene acetylene glycol, 0.5 part sodium polyacrylate, 14 parts of the plastic hollow body used in Example 9, anhydrous 20 parts of sodium sulfate and 31.4 parts of urea were kneaded with a high speed stirrer, and then extruded and assembled from a screen having a diameter of 5 mm using an extrusion granulator. It dried with the fluidized bed drier at ° C, and sifted out, and the granular material containing PHC 8 mass% of diameter 3-7 mm and length 3-20 mm was obtained as a uniformly diffusive granular pesticide formulation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Comparative Example 1

The mixture which uniformly mixed 6.25 parts of bensulfuron methyl (pKa 5.03), 81.25 parts of calcium carbonate, 6.25 parts of polyvinyl alcohol, and 6.25 parts of (alpha) starch was grind | pulverized with the impact grinder. The mixture obtained by adding an appropriate amount of water to the obtained powder was kneaded with a high speed stirrer, and then extruded and granulated from a screen having a diameter of 0.5 mm using a dome type granulator, and the granulated substance was left to dry at 60 ° C. to give 6.25 mass of bensulfuronmethyl. The pesticide granules of 0.4-0.6 mm in diameter and 1-6 mm in length containing% were obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 32 parts of this non-disintegrated pesticide granular material, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, and 40.9 parts of urea are appropriate amounts of water. After kneading the mixture was added with a twin-screw kneader, and extruded from a screen having a diameter of 5 mm using an extrusion granulator, it was set to a target size, and dried by a fluid bed dryer at a temperature of 60 ℃, By sifting out, a granular material containing 2% by mass of bensulfuronmethyl having a diameter of 3 to 7 mm and a length of 3 to 20 mm was obtained as a homogeneous diffusive granular pesticide preparation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Comparative Example 2

10 parts of compound A (pKa 6.17) and 1.7 parts of basic white carbon were mixed uniformly, finely pulverized with an air mill to prepare a compound A-containing powder.

75 parts of diatomaceous earth particles having a particle size of 16 to 35 mesh (1000 to 425 μm) were added to the conical screw mixer, and 12 parts of propylene glycol and 1.3 parts of polypropylene glycol (molecular weight: 1000) were mixed beforehand by heating with a propeller mixer. The prepared solution was added. Immediately after the end of the addition, the compound A-containing powder was added thereto, mixed uniformly to form a granule, and the granular material was aged with a 60 ° C shelf-type drier to obtain a pesticide granule having a particle diameter of 0.4 to 1.1 mm. The pesticide granules were dropped into water, and after 30 minutes, the disintegrated state of the particles was observed. The disintegrated particles were not identified, and were determined to be non-disintegrated.

Next, 30 parts of this non-disintegrating pesticide granular material, 3 parts of sodium dibutylnaphthalene sulfonate, 2 parts of lauryl sulfate, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, 1 part of sodium polyacrylate, white carbon 2 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, and 34.9 parts of urea were kneaded with a biaxial kneader, and then a screen having a diameter of 5 mm using an extrusion granulator. After extrusion granulation and sizing to a target size, it is dried with a fluid bed dryer at a product temperature of 60 ° C. and sifted to contain 3% by mass of compound A having a diameter of 3 to 7 mm and a length of 3 to 20 mm. The granular material was obtained as a uniformly diffusive granular pesticide. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Comparative Example 3

A mixture of 10 parts of compound B (pKa 5.75), 6.7 parts of distearyldimethylammonium chloride, 6.7 parts of dilauryldimethylammonium chloride, 63.2 parts of clay, 6.7 parts of polyvinyl alcohol, and 6.7 parts of α-starch, was mixed. Grinding with a grinder. After kneading the mixture obtained by adding an appropriate amount of water to the obtained powder with a high speed stirrer, using a dome-type granulator, the mixture was extruded from a screen having a diameter of 0.5 mm, the granulated substance was left to dry at 60 ° C, and compound B was 10% by mass. The pesticide granular material of 0.4-0.6 mm in diameter and 1-6 mm in length containing was obtained. The pesticide granules were dropped into water, and after 30 minutes, the disintegrated state of the particles was observed. The disintegrated particles were not identified, and were determined to be non-disintegrated.

Next, 30 parts of this non-destructive pesticide granular material, 1 part of polyoxyethylene acetylene glycol, 2 parts of polyoxyethylene polyoxypropylene block polymer, 3 parts of polyoxyethylene styrylphenyl ether phosphate amine salt, 3 parts of enzyme-modified dextrin 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, and 38.9 parts of urea were kneaded with a biaxial kneader, and then extruded from a screen having a diameter of 5 mm Granulated material containing 3 mass% of compound B of 3-7 mm in diameter and 3-20 mm in length by extrusion-granulating, sizing to a target size, drying with a fluidized bed drier at sieve temperature 60 degreeC, and sifting. Was obtained as a homogeneous diffusive granular pesticide preparation. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Comparative Example 4

A mixture of 6.25 parts of pyrazosulfuronethyl (pKa 3.91), 12 parts of paraffin (melting point 68-70 ° C), 63.75 parts of calcium carbonate, and 18 parts of polyvinyl alcohol was ground by an impact mill. The mixture obtained by adding an appropriate amount of water to the obtained powder was kneaded with a high speed stirrer, and then extruded and granulated from a screen having a diameter of 0.5 mm using a dome type granulator, and the granulated substance was left to dry at 70 DEG C to form pyrazosulfuron ethyl 6.25. The pesticide granular material of 0.4-0.6 mm in diameter and 1-6 mm in length containing mass% was obtained. The obtained pesticide granules were dropped in water, and after 30 minutes, the collapsed state of the particles was observed. The disintegrated particles were not confirmed, and were determined to be non-disintegrated.

Next, 16 parts of this non-disintegrated pesticide granular material, 5 parts of butylnaphthalene sulfonic acid formalin condensate sodium salt, 1 part polyoxyethylene acetylene glycol, 0.5 part sodium polyacrylate, 14 parts of the plastic hollow body used in Example 1, anhydrous 20 parts of sodium sulfate and 55.4 parts of urea were kneaded with a high speed stirrer, and then extruded and granulated from a screen having a diameter of 5 mm using an extrusion granulator. It dried with the fluidized bed drier at ° C, and sifted out to obtain a granular material containing 1 mass% of pyrazosulfuronethyl having a diameter of 3 to 7 mm and a length of 3 to 20 mm as a uniform diffusive granular pesticide. The obtained uniformly diffusive granular pesticide preparation was dropped into water and observed. As a result, the particles of the formulation disintegrated within 30 minutes, and the non-disintegrating pesticide granules precipitated.

Test Example 1 (Underwater Dissolution Test)

8 liters of tap water was put into a 50 cm long and 40 cm wide enamel bat, and the water depth was 4 cm. This was subjected to a trial treatment so that the uniformly diffusive granular pesticide preparations of Examples 1 to 10 and Comparative Examples 1 to 4 were equivalent to 250 g per 10 ars. After 1, 3, 7, 21 and 35 days of treatment, water was collected, and HPLC concentration was used to determine the concentration of components in water as the dissolution rate in water. The results are shown in Table 1.

Herbicide active ingredient 1 day 3 days 7 days 21st 35 days Example 1  Bensulfuronmethyl 52 63 74 81 87 Example 2
 Bensulfuronmethyl 54 66 71 87 96  Mefenacet 85 92 100 97 93 Example 3  Compound A 34 41 56 59 73 Example 4  Compound A 42 54 67 82 91 Example 5  Compound B 19 21 32 47 69 Example 6  Compound B 29 38 42 53 68 Example 7
 Compound B 19 24 37 49 56  Pentrazamide 95 100 98 94 96 Example 8  Pyrazosulfuronethyl 56 59 71 83 86 Example 9  Tricyclazole 69 72 86 95 93 Example 10  PHC 59 63 72 80 83 Comparative Example 1  Bensulfuronmethyl 100 100 100 100 100 Comparative Example 2  Compound A 100 96 98 100 96 Comparative Example 3  Compound B 79 95 100 99 100 Comparative Example 4  Pyrazosulfuronethyl 6 8 3 5 7

In Table 1, the uniformly diffusive granular pesticide preparations of Examples 1 to 7 were treated with sulfonylurea-based compounds or difluoromethanesulfonylanilide derivatives or salts of herbicides of the pesticide active ingredient. In the test from 1 day to 35 days later, it turns out that it is slowed down because it is changing with respect to Comparative Examples 1-3.

In contrast to Example 8 and Comparative Example 4, the latter was changed while the water concentration was low with respect to the former, and elution of the pesticide active ingredient was only a small part of the initial stage, but not continued. It is clearly inferior in the point that most of the pesticide active ingredients remain unused.

In contrast with Example 5 and Comparative Example 3, it can be seen that the latter is changed while the water concentration is high with respect to the former, and since the basic substance is not contained, the sustained release of the pesticide active ingredient is reduced.

Test Example 2 (Packaging Diffusion)

The uniformly diffusible granular pesticide formulation of Example 5 was sprayed by hand by the spray from the upper two sides of the paddy field of 20 m short side, 50 m long side, and 5 cm depth shown in FIG. After 48 hours of spraying, water was collected and analyzed at the point (A-L) shown in Fig. 1, and theoretically, the ratio when the concentration of water in the case where the pesticide active ingredient was uniformly dispersed in water was 100%. Also, the rate of change was calculated by dividing the standard deviation of the water concentration at each point by the mean. The results are shown in Table 2.

Point Concentration of compound B
(%) A 35 B 37 C 39 D 31 E 29 F 25 G 29 H 31 I 35 J 27 K 26 L 24 Average 30.8 Change 16.2

In Table 2, when this uniformly diffusive granular pesticide preparation is applied, it can be seen that the uniformity of the active ingredient of the pesticide in water is good.

The uniformly diffusive granular pesticide preparation of the present invention can be prepared by a simple method, moderately sustained release of the pesticide active ingredient, thereby exerting the pharmacological effect of the pesticide active ingredient over a long period of time, and in the environment Plowing pesticide formulations that can reduce the environmental load by reducing the release of active ingredients and reduce or prevent weakness caused by active pesticides, for example, damage to target crops, can be prepared by simple spraying. It makes it possible to spread | diffuse uniformly, and the outstanding effect that it contributes to the vitalization of agricultural work is achieved.

Claims (12)

Mass ratio of particles having a particle size of 3 mm or more containing non-disintegrating pesticide granules, surfactants and floating components which do not disintegrate in water within 30 minutes containing an acidic pesticide active ingredient, dialkyldimethylammonium chloride and a basic substance. A uniformly diffusive granular pesticide formulation having a particle size distribution of 80% by mass or more and having a property of floating on the surface immediately after dropping on the surface, but decaying on the surface within 30 minutes. The method of claim 1, The uniformly diffusive granular pesticide preparation, characterized in that the acidic pesticide active ingredient is pKa 2-7. The method of claim 1, A uniformly diffusive granular pesticide preparation, characterized in that the acidic pesticide active ingredient is a herbicide. The method of claim 3, A homogeneous diffusive granular pesticide formulation, characterized in that the herbicide is a sulfonylurea compound. The method of claim 3, Herbicides are general formula [Tue 1]

(Wherein R ¹ is a hydrogen atom, an alkyl group or an alkoxyalkyl group) It is a difluoromethanesulfonylanilide derivative or its salt represented by the uniformly diffusible granular pesticide formulation. delete The method of claim 1, The basic substance is sodium hydrogen carbonate, sodium carbonate, calcium hydroxide, calcium carbonate, basic white carbon, or basic acidic clay. The method of claim 1, A floating diffusion granular pesticide preparation, characterized in that the floating component is an inorganic hollow body or a plastic hollow body. A non-disintegrating pesticide granule which does not disintegrate in water within 30 minutes containing an acidic pesticide active ingredient, a dialkyldimethylammonium chloride and a basic substance, together with a surfactant and a floating component, has a particle size. A method for producing a uniformly diffusive granular pesticide preparation, characterized in that it has a spherical shape of 1 to 20 mm or a horizontally long shape having a short diameter of 1 to 20 mm and a long diameter of 3 to 40 mm. The method of claim 9, A granulation process is carried out by extruding granulation from a screen having a body diameter larger than the particle size or particle length of the non-disintegrating pesticide granular material. According to the granulation treatment of the non-disintegrating pesticide granules which do not disintegrate in water within 30 minutes containing the acidic pesticide active ingredient, dialkyldimethylammonium chloride and basic substances, together with the surfactant and the floating component, A spherical shape having a particle diameter of 1 to 20 mm or a horizontally long shape having a short diameter of 1 to 20 mm and a long diameter of 3 to 40 mm. The method of claim 11, A granulation process is carried out by extruding granulation from a screen having a body diameter larger than the particle size or particle length of the non-disintegrating pesticide granular material.

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