WO2005029956A1

WO2005029956A1 - Uniformly diffusible granular pesticide composition

Info

Publication number: WO2005029956A1
Application number: PCT/JP2004/013776
Authority: WO
Inventors: Kiyotoshi Nishiyama; Toshio Sugimura; Tetsuo Ohkawa
Original assignee: Kumiai Chemical Industry Co., Ltd.
Priority date: 2003-09-26
Filing date: 2004-09-22
Publication date: 2005-04-07
Also published as: JPWO2005029956A1; KR20060063914A; KR101130428B1; CN1856247A; JP4919662B2; CN1856247B

Abstract

The invention aims at providing a uniformly diffusible granular pesticide preparation enabling a granular pesticide preparation which can be prepared by a simple and easy process and exert drug effects of pesticial active ingredients for a long term and is reduced in environmental load and reduced in or freed from sufferings induced by pesticidal active ingredients to be diffused uniformly over the whole of a paddy field by a simple application method. The invention provides a uniformly diffusible granular pesticide preparation which contains a non-disintegrating pesticide composition comprising an acid pesticidal active ingredient, a cationic surfactant, and a basic substance and causing no disintegration in water within 30 minutes and which has both a particle size distribution wherein the proportion of particles having diameters of 3 mm or above is 80 % by mass or above and the property of floating on water surface just after thrown onto water surface but disintegrates on water surface within 30 minutes. It is preferred that the acid pesticidal active ingredient be one having a pKa of 2 to 7, while the cationic surfactant be one having the property of gelling or swelling in water.

Description

Specification

Uniformly diffusible granular pesticide formulation

Technical field

[0001] The present invention relates to a homogeneously diffusible granular pesticide formulation that can exert its medicinal properties for a long period of time, reduce or prevent phytotoxicity, and reduce the environmental burden.

Background art

[0002] Hitherto, various formulation methods capable of controlling the dissolution of an active agricultural chemical have been studied in order to reduce the phytotoxicity and maintain the efficacy of granular agricultural chemicals containing the active agricultural chemical. For example, a method has been proposed in which paraffin wax, thermoplastic resin or activated carbon, granular foam, and clay minerals are combined and blended for slow release (Japanese Patent Application Laid-Open No. 63-35504, Japanese Patent Application Publication No. See JP-A-63-45201 and JP-A-2-288803.

[0003] However, such a conventional sustained-release method is not always effective, and the preparation method of a granular pesticide formulation is complicated, or the release of the pesticide composition is insufficient, and the pesticide active ingredient is not sufficiently released. There is a problem that most of them are not effectively used and remain in the pesticide composition as they are, so that more pesticidal active ingredients are released into the environment than necessary, resulting in a large burden on the environment. There was such a problem.

[0004] In addition, for the purpose of stabilizing different active ingredients, a method for producing a granular pesticide formulation in which an inner core is prepared and then coated with an active ingredient different from the inner core has also been proposed! 9-315903), the technology of a labor-saving formulation for uniformly dispersing a granular pesticide formulation that has been subjected to sustained release over rice paddy ridges and the like to the entire paddy field has not yet been established.

Disclosure of the invention

[0005] Under such circumstances, the present invention overcomes the problems associated with conventional granular pesticide preparations, can be prepared by a simple method, and exerts the medicinal properties of the pesticidal active ingredient for a long period of time. To provide a uniform diffusible granular pesticide formulation that can uniformly spread a granular pesticide formulation that can reduce environmental load and reduce or prevent phytotoxicity caused by pesticidal active ingredients throughout a paddy field by a simple spraying method. It is a subject.

[0006] The present inventors have conducted intensive studies on a homogeneously diffusible granular pesticide formulation, and as a result, It contains non-disintegrable granular pesticides in which an acidic pesticide active ingredient is blended with a cationic surfactant and a basic substance. Particles with a particle size of 3 mm or more have a particle size distribution of 80% by mass or more and have the property of floating on the water surface. The present inventors have found that the above-mentioned problem can be solved by making it possible to disintegrate on the water surface within 30 minutes, and have accomplished the present invention based on this finding.

That is, the present invention

(1) Contains acidic pesticide active ingredient, cationic surfactant and basic substance Within 30 minutes, contains non-disintegrable pesticide granules that do not disintegrate in water, surfactants and floating ingredients, particle size 3 mm These particles have a particle size distribution of 80% by mass or more and have the property of floating on the water surface immediately after being dropped on the water surface, but have a uniform diffusive particle characteristic of being disintegrated on the water surface within 30 minutes. Pesticide formulation,

(2) The homogeneously diffusible granular pesticide preparation according to the above (1), wherein the acidic pesticide active ingredient is pKa2-7.

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

(4) The herbicide is a sulfonylprea compound, the uniform diffusible granular pesticide formulation according to (3),

(5) Herbicide represented by general formula (I)

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

A homogeneously diffusible granular pesticide preparation according to the above (3), which is a difluoromethanesulfo-l-lide derivative or a salt thereof represented by the formula:

(6) the cationic surfactant is gelling in water, or shows a swelling property The uniform diffusible granular pesticide formulation according to the above (1),

(7) The average amount according to the above (1), wherein the basic substance is sodium hydrogen carbonate, sodium carbonate, calcium hydroxide, carbonated calcium, basic white carbon or basic acid clay. Monodisperse granular pesticide formulation,

(8) The uniform diffusible granular pesticide formulation according to (1), wherein the floating component is an inorganic hollow body or a plastic hollow body,

(9) Contains acidic pesticide active ingredient, cationic surfactant and basic substance and does not disintegrate in water within 30 minutes. ヽ Granulate non-disintegrable pesticide granules together with surfactant and floating ingredient. A method for producing a homogeneously diffusible granular pesticide formulation, characterized in that the shape is a spherical shape having a particle diameter of 11 to 20 mm or a horizontally long shape having a minor axis of 1 to 20 mm and a major axis of 3 to 40 mm.

(10) The production method according to the above (9), wherein the granulation treatment is performed by extruding and granulating from a screen having an opening diameter larger than the particle size or the particle length of the non-disintegrable pesticide granules,

(11) Non-disintegrable pesticide granules that contain acidic pesticide active ingredients, cationic surfactants and basic substances that do not disintegrate in water within 30 minutes, and pesticide active ingredients together with surfactants and floating ingredients A method for producing a homogeneously diffusible granular pesticide preparation, which is subjected to granulation treatment and has a spherical shape with a particle diameter of 11 to 20 mm, and a horizontal shape of a short diameter of 11 to 20 mm and a long diameter of 3 to 40 mm, and

(12) The production method according to the above (11), wherein the granulation treatment is carried out by extruding and granulating from a screen having an opening diameter larger than the particle size or the particle length of the non-disintegrable pesticide granules.

Is to provide.

Brief Description of Drawings

FIG. 1 is an explanatory diagram of a paddy field to which a pesticide formulation is applied in Test Example 2.

BEST MODE FOR CARRYING OUT THE INVENTION

Hereinafter, the present invention will be described in detail.

The non-disintegratable pesticide granules to be contained in the granular pesticide preparation of the present invention do not disintegrate in water within 30 minutes, and retain the original granular form.

[0010] The acidic pesticidal active ingredient used in the non-disintegrable pesticide granules is not particularly limited, but is usually a herbicide, a plant growth regulator, a bactericide, an insecticide and the like. A range is preferred, and geometric isomers, optical isomers and the like are also included.

[0011] The herbicide is not particularly limited, but pKa2-7 is particularly preferred, especially sulfol. Urea compounds and the following general formula (I)

[Formula 2]

(Wherein R ¹ is a hydrogen atom, an alkyl group or an alkoxyalkyl group), and a difluoromethanesulfo-fluoride derivative or a salt thereof is particularly preferred. Examples of the sulfolurea compound include 1- (4,6-dimethoxypyrimidin-2-yl) -3- [1-methyl-4- (2-methyl-2H-tetrazol-5-yl) pyrazole -5-ylsulfol-urea] urea (azimsulfuron), 1- (2-chloroimidazo [1,2-a] pyridine-3-ylsulfol-yl) -3--3- (4,6-dimethoxypyrimidine-2-yl) ) Urea (imazosulfuron), ethyl = 5- (4,6-dimethoxypyrimidine-2-ylcarbamoylsulfamoyl)-1-methylpyrazole-4-force ruboxylate (virazosulfuronethyl), methyl = (4, 6 -Dimethoxypyrimidine-2-ylcarbamoylsulfamoyl) -0-toluate (bensulfuronmethyl), 1- (4,6-dimethoxypyrimidine-2-yl) -3- (2-ethoxyphenoxysulfol-yl) ) Urea (Ethoxysulfuron), 1- [2- (cyclopropylcarbol) a -Rinosulfol] -3- (4,6-dimethoxypyrimidin-2-yl) urea (cyclosulfamuron), 1- (4,6-dimethoxy-1,3,5-triazin-2-y ) -3) [2- (2-Methoxyethoxy) phenylsulfol] urea (cinosulfuron), methyl 3- (4-methoxy-6-methyl-1,3,5-triazine-2-ylcarbamoylsulfur) Famoyl) -2-thenoate (thifensulfuron-methyl), 2- (4,6-dimethoxypyrimidine-2-ylcarbamoylsulfamoyl) -N, N-dimethylnicotinamide (nicosulfuron), methyl = 3- Black mouth-5- (4,6-dimethoxypyrimidine-2-ylcarbamoylsulfamoyl) -1-methylpyrazole-4-carboxylate (halosulfuronmethyl), 1- (4,6-dimethoxypyrimidine-2-y ) -3- (3-Trifluoromethyl-2-pyridylsulfol) urea (furaza sul Ron), 1 - (4, 6-dimethoxypyrimidin-- 2-I le) -3- (3-Echirusuruho - Le - 2-pyridinium Jirusuruhoniru) urea (rimsulfuron), and the like. [0013] Examples of the difluoromethanesulfo-l-lide derivative or a salt thereof include compounds described in JP-A-2000-44546, for example, 2-[(4,6-dimethoxypyrimidine-2). -Yl) hydroxymethyl] -N-difluoromethanesulfo-luarylide, 2-[(4,6-dimethoxypyrimidine-2-yl) hydroxymethyl] -6-methoxymethyl-N-difluoromethanesulfo And 2-[(4,6-dimethoxypyrimidin-2-yl) hydroxymethyl] -6-ethyl-N-difluoromethanesulfo-l-lide.

[0014] Examples of other herbicides include 2-methyl-4-chlorophenoxythioacetate-S-ethyl (phenothiol), a- (2-naphthoxy) propiona-lide (naproa-lide), 5- ( 2,4-Dichlorophenoxy) -2-nitromethyl benzoate (biphenox), S- (4-chlorobenzyl) -N, N-getylthiolbamate (benthiocarb), S-benzyl = 1,2-dimethyl Propyl (ethyl) thiocarbamate (esprocalp), S-ethylhexahydro-1H-azepine-1-carbothioate (molinate), S-1-methyl-1--1-phenyl-piperidine-1-carbothioate (dimipeperitate) ), O-3-tert-Butylphenol = 6-methoxy-2-pyridyl (methyl) thiocarbamate (pyributicarb), 2-chloro-2 ', 6'-ethyl-N- (butoxymethyl) acetate-lide (pig Roll), 2-chloro-2 ', 6'-Getyl-N- (2-propoxyshetyl) aceto-Lide (pretilachlor), (RS) -2-bromo-N- (a, α-dimethylbenzyl) -3,3-dimethylbutyramide (promobutide), 2-benzothiazole-2-yloxy-Ν-methylaceto-lide (mephenacet), 1- (α, α-dimethylbenzyl) -3- (para-tolyl) urea ( Daimlon), 2-methylthio-4,6-bis (ethylamino) -s-triazine (simetrine), 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 (chromomethoxyel), 56 -Butyl-3- (2,4-dichloro-5-isopropoxy- -1,3,4-oxaziazol-2 (3Η) -one (oxaziazone), 4- (2,4-dichlorobenzoyl) -1,3-dimethyl-5-pyrazolyl-ρ-toluenesulfonate ( Pyrazolate), 2- [4- (2,4-dichlorobenzoyl) -1,3-dimethylbiazole-5-yloxy] acetophenone (virazoxifene), (RS) -2- (2,4- Dichloro-m-tolyloxy) propiona-lido (clomeprop), 2- [4- [2,4-dichloro-m-toluoyl] -1,3-dimethylbiazo Le-5-yloxy] -methylacetophenone (benzophenap), S, S'-dimethyl = 2-difluoromethyl-4-isobutyl-6-trifluoromethylpyridine-3,5-dicarbothioate (dithiopyr), 2-chloro-N- (3-methoxy-2-tur) -2 ', 6'-dimethylaceto-lido (turchlor), butyl = (R) -2- [4- (4-cyano-2- Fluorophenoxy) phenoxy] propionate (hop butyl butyl), 3- [1- (3,5-dichlorophenyl) -1-methylethyl] -2,3-dihydro-6-methyl-5-phenyl-4H -1,3-oxazine-4-one (oxadicromemefone), 3- (4-chloro-5-cyclopentyloxy-2-fluorophenyl) -5-isopropylidene-1,3-oxazolidine -2, 4-dione (pentoxazone), 1- (ethyl carbamoyl) -3- (2, 4, 6-trimethylphenol sulfol) -1, 2, 4-to Azol (cafuentrol), methyl = 2-[(4,6-dimethoxypyrimidine-2-yl) oxy] -6-[(E) -1- (methoxyimino) ethyl] benzoate (pyriminoback methyl) Etc.

[0015] The plant growth regulator is not particularly limited, but may be 4'-cloth-2 '-(hi-hydroxybenzyl) isonicotinylide (inavenfide), (2RS, 3RS) -1- (4 -Black mouth ferrule)-

4,4-dimethyl-2- (1Η-1,2,4-triazol-1-yl) pentan-3-ol (paclobutrazol), (E)-(S) -l- (4- yl) -4, 4-dimethyl-2-(1 [Eta]-1, 2, 4-tri Azoru - 1 - I le) penta -丄- E emissions - ₃ - ol (© - conazole), calcium 3- O key Sid-5-oxo-4-propionylcyclohexa-3-enecarboxylate (prohexadione calcium salt); hydrazidecholine maleate; Among them, those having pKa27 are particularly preferably used.

[0016] The fungicide is not particularly limited, but includes O, 0-diisopropyl-S-benzylthiophosphate (ΙΒΡ), 3'-isopropoxy-2-methylbenza-lide (meprole), a, a, α-Trifluoro-3'-isopropoxy-0-toluide (flutoral), 3,4,5,6-tetrachloro --- (2,3-dichlorophenol) phthalamic acid ), 1- (4-chlorobenzyl) -1-cyclopentyl-3-phenylurea (pencyclone), 6- (3,5-dichloro-4-methylphenyl) -3 (2Η) -pyridazinone (Diclomedin), methyl = Ν- (2-methoxyacetyl) -Ν- (2,6-xylyl) -DL-araninate (metalaxyl), (Ε) -4-chloro-a, a, a ~ b Rifluo Mouth-N- (1-imidazole-1-yl-2-propoxyshetilidene) -0-toluidine Flumizole), kasugamycin, noridamycin, 3-aryloxy-1,2-benzisothiazole-1,1-dioxide (probenazole), diisopropyl-1,3-dithiolan-2-ylidene-malonate (isoprothiolane), 5- Methyl-1,2,4-triazolo [3,4-b] benzothiazonole (tricyclazonole), 1,2,5,6-tetrahydropyro [3,2,1-ij] quinolin-4-one (Pyroquilon), 5-ethyl-5, 8-dihydro-8-oxo [1, 3] dioxolo [4, 5-g] quinoline-7-carboxylic acid (oxolinic acid), (Ζ) -2'-methyl Acetofphenone = 4,6-dimethylpyrimidine-2-ylhydrazone -4,5,6,7-tetraclomouth phthalide (pheliminzone), 3- (3,5-dichlorophenyl) -Ν-isopropyl-2,4 -Dioxoimidazolidine-1-carboxamide (iplodione) and the like. Among them, those having pKa2-7 are particularly preferably used.

Although the insecticide is not particularly limited, O, 0-dimethyl-0- (3-methyl-4-nitrophenyl) thiophosphate (MEP), (2-isopropyl-4-methylpyrimidyl-6) -getyl thiophosphate ( Diazinon), 1-naphthyl-N-methylcarbamate (NAC), O, O-getyl-0- (3-oxo-2-phenyl-2H-pyridazine-6-yl) phosphorothioate (pyridafentione) ), O, O-dimethyl-O-3,5,6-trichloro-2-pyridyl phosphorothioate (chloropyrifosmethyl), dimethyldicarbethoxyxethyl thiophosphate (marathon), O, 0-dimethyl -S- (N-methylcarbamoylmethyl) dithiophosphate (dimethoate), O, 0-dipropyl-0-4-methylthiophene-phosphate (propaphos), O, S-dimethyl-N-acetylphosphoramide Chooate (acephate) , Ethyl para-trophylthionobenzenephosphonate (EPN), 2-sec-butylphenyl-N-methylcarbamate (BPMC), 2,3-dihydro-2,2-dimethyl-7-benzo [b] fura -Le =? ^-Dibutylaminothio -N-methylcarbamate (carbosulfan), ethyl = N- [2,3-dihydro-2,2-dimethylbenzofuran-7-yloxycarbonyl (methyl) aminothio]- N-isopropyl-13-araninate (benfuracarb), (RS) -a-cyano-3-phenoxybenzyl = (RS) -2,2-dichloro-1- (4-ethoxyphenyl) cyclopropanecarboxylate (Cycloprothrin), 2- (4-ethoxyphenyl)-2-methylpropyl = 3-phenoxybenzyl = ether (ethofenprox), 1,3-bis (potumbamoylthio) -2- (N , N-dimethylamino) propane hydrochloride (cartap), 5-dimethyl Amino - 1, 2, 3 Torichianshiyuu salt ( Thiocyclam), S, S'-2-dimethylaminotrimethylene di (benzenethiosulfonate)

) (Bensultap), 2-tert-butylimino-3-isopropyl-5-phenyl-1,3,5,6-tetrahydro-2H-1,3,5-thiadiazin-4-one (buprofezin) No. Among them, those having pKa2-7 are particularly preferably used.

When an acidic pesticidal active ingredient having the above-mentioned predetermined pKa is used, the pKa of the ingredient can be determined, for example, by referring to Experimental Chemistry Lecture 5 (thermal measurement and equilibrium), p469-p474, published on January 20, 1958, Maruzen Co., Ltd. It is measured by the method described.

The cationic surfactant used in the present invention is not particularly limited, but preferably includes an amine salt, a pyridium salt, and a quaternary ammonium salt.

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

[0021] Examples of the pyridinium salt-based cationic surfactant include lauryl pyridinium chloride, myristyl pyridin-dum chloride, cetyl pyridin-dum chloride and the like.

[0022] Examples of the quaternary ammo-pum salt cationic surfactant include alkyl dimethyl benzylammonium-pum chloride, lauryltrimethylammo-pumchloride, cetyltrimethylammonium-pumchloride, stearyltrimethylammonium-pumchloride, dilauryldimethylammonium-pumchloride, Dioleyldimethylammonium chloride, dicocoyldimethylammonium chloride, distearyldimethylammonium chloride, lauryldihydroxyethylmethylammonium chloride, oleylbispolyoxyethylenemethylammonium chloride, stearylhydroxyethyldimethylammonium chloride Peryldimethylbenzylammonium -Phamchloride, lauroylaminopropyldimethylethylammonium Arm ethosulfate, lauroyl § amino propyl dimethyl hydroxyethyl E chill § Nmo - such Umupaku opening rate and the like.

Particularly preferred cationic surfactants are those which gel or swell in water, for example, dialkyldimethylammonium-dimethyl chlorides whose alkyl moiety is C8-C22, Among them, dilauryl dimethylammonium-pum chloride, Dioleyldimethylammonium chloride, dicocoyldimethylammonium chloride and distearyldimethylammonium chloride. These surfactants may be used alone or in combination of two or more.

[0024] The basic substance used in the present invention is not particularly limited, but preferably has a pH of 7.5 or more, especially 9 to 12 when a 1% by mass aqueous solution or 1% by mass aqueous suspension is used. Some are preferred. Examples of such compounds include hydroxides of alkali metals and alkaline earth metals, alkali metal salts and alkaline earth metal salts, and compounds and minerals containing the same. More specifically, sodium hydroxide, potassium hydroxide, sodium hydrogencarbonate, sodium carbonate, calcium hydroxide, calcium carbonate, calcium oxide, basic white carbon, basic acid clay and the like can be mentioned. Particularly preferred are sodium hydrogen carbonate, sodium carbonate, calcium hydroxide, calcium carbonate, basic white carbon and basic acid clay. These basic substances may be used alone, or two or more kinds may be used in combination.

The surfactant used in the present invention is not particularly limited, and examples thereof include polyoxyalkylene glycol higher fatty acid ester, polyoxyalkylene alkyl ether, polyoxyalkylene alkylaryl ether, polyoxyalkylene alkylaryl ether, Non-ionic surfactants such as sorbitan monoalkylate, acetylene glycol, polyoxyethylene acetylene glycol, alkylaryl sulfonates, dialkyl sulfonates, alkyl sulfates, alkyl phosphates, alkyl aryl phosphates , Alkyl aryl phosphate, polyoxyalkylene alkyl ether sulfate, naphthalene sulfonate and its condensate, alkyl naphthalene sulfonate and its condensate, rig- Polycarboxylic acid-type polymer interfaces such as sulfonic acid salt, acrylic acid itaconic acid copolymer, methacrylic acid-itaconic acid copolymer, maleic acid styrene copolymer, maleic acid isobutylene copolymer, and alkali metal salts thereof Surfactants such as polyoxyalkylene aryl phenyl ether sulfate salts and the like. These may be used alone, or

, Or two or more of them may be used in combination.

[0026] When the floating substance used in the present invention is dropped on the surface of water, the substance itself floats on the surface of water. The inorganic substance is not particularly limited as long as it is a substance, and examples of the inorganic substance include an inorganic hollow body such as a glassy hollow body, expanded pearlite, expanded fly ash, vermiculite, calcined vermiculite, shirasu balloon, microballoon, and cenosphere. Isopotency Examples of the organic substances include plastic hollow bodies, waxes, solid paraffins, foam-containing starch, cork, wood chips, plant pieces such as cotton bean, polybutenes and other specific light substances, and organic solvents. Can be In particular, an inorganic hollow body such as a glassy hollow body and a heated Shirasu foam, or a plastic hollow body such as a Shiridani vinylidene.acrylonitrile copolymer plastic balloon and an acrylonitrile-based plastic balloon are preferable. These may be used alone, or

Two or more types may be used in combination.

[0027] The homogeneously diffusible granular pesticide preparation of the present invention can contain, as necessary, an additive component usually used in pesticide preparations. As the additional components, extenders, auxiliary components, and the like are used.

[0028] As the extender, a solid carrier such as a mineral carrier, a water-soluble salt, or the like is used. Specific examples include clays, calcium carbonate, bentonite, talc, diatomaceous earth, acid clay, silica sand, and granular carbonate. Examples include calcium, granular diatomaceous earth, calcium stearate, white carbon, potassium chloride, anhydrous sodium sulfate, potassium sulfate, urea, ammonium sulfate, and sodium benzoate. These may be used alone or in combination of two or more.

[0029] As the auxiliary component, for example, a binder for preparing a granular composition, specifically, carboxymethylcellulose sodium salt, dextrin, water-soluble starch, xanthan gum, guar gum, sucrose, polybutylpyrrolidone, polybutyl alcohol , Sodium polyacrylate, polyethylene glycol having an average molecular weight of 6000 to 20000, and polyethylene oxide having an average molecular weight of 100,000 to 5,000,000. Organic solvents used for dissolving the acidic pesticide active ingredient and the cationic surfactant and adsorbing them on the carrier, specifically, alkylnaphthalene, dimethylformamide, dimethylsulfoxide, N-methyl-2-pyrrolidone, N- Octylpyrrolidone, polyhydric alcohol, silicone oil and the like. In addition, if necessary, a stabilizer or the like may be used. These may be used alone or in combination of two or more. [0030] In the homogeneously diffusible granular pesticide formulation of the present invention, the composition ratio of the non-disintegrable pesticide granules is usually 0.1 to 40% by mass of an acidic pesticide active ingredient, and 140 to 100% by mass of a cationic surfactant. The basic substance is selected in the range of 0.1 to 95% by mass, and the pH of a 1% by mass aqueous suspension of the non-disintegrating pesticide granules is usually 5 or more, preferably 7 or more, more preferably 7. Adjusted to be 5—11.5.

[0031] The composition ratio of the homogeneously diffusible granular pesticide preparation of the present invention is usually 1 to 70% by mass of non-disintegrable pesticide granules, 0 to 50% by mass of pesticidal active ingredient, and surface activity. 0.1 to 30% by mass, floating component 0.1 to 50% by mass, extender 0 to 95% by mass, preferably 5 to 70% by mass, auxiliary component 0 to 50% by mass, preferably 0.1 to 30% %, More preferably one having a specific gravity of less than 1 and sufficient for floating on the water surface.

[0032] The uniformly dispersible granular pesticide preparation of the present invention disintegrates within 30 minutes after being treated in the field, and gradually disperses the non-disintegrable pesticide granules contained therein into the field during the disintegration. This is a labor-saving controlled-release pesticide formulation that has been settled down and has a slow release of the pesticide active ingredient contained in the pesticide granule. It is also possible to design a dissolution property suitable for each pesticide active ingredient by including a non-disintegrable pesticide granular material in a homogeneously diffusible granular pesticide formulation.

[0033] The present invention also relates to the homogeneously diffusible granular pesticide formulation and a homogeneously diffusible granular pesticide formulation having neither a cationic surfactant nor a basic substance in a ratio of 1: 9-9: 1. It also includes mixed pesticide preparations mixed by mass ratio.

[0034] In the homogeneously diffusible granular pesticide preparation of the present invention, the size itself is usually in the form of a sphere, usually having a particle diameter of 11 to 20 mm, preferably 3 to 10 mm, and in the case of a horizontally long shape, usually having a minor diameter of 1 to 20 mm, preferably. The size of non-disintegrable pesticide granules contained in this pesticide formulation is usually 3 to 10 mm, major axis is 3 to 40 mm, and preferably 5 to 30 mm. 0.1 to 3 mm, preferably 0.1 to 10 mm, preferably 0.5 to 7 mm, preferably 0.5 to 7 mm, major axis 0.3 to 30 mm, preferably 1.5 to 20 mm for a horizontally long shape. The power of doing it!

[0035] There is no particular limitation on the method for preparing the homogeneously diffusible granular pesticide preparation of the present invention and the non-disintegrable pesticide granules contained in the preparation. Method, extrusion granulation method, coating granulation method and the like are used. [0036] The method for producing the homogeneously diffusible granular pesticide preparation of the present invention is preferably a non-disintegrable pesticidal granule which contains an acidic pesticide active ingredient, a cationic surfactant and a basic substance and does not disintegrate in water within 30 minutes. A method of subjecting the product to a granulation treatment together with a surfactant and a buoyant component to obtain a spherical shape having a particle diameter of 120 mm or a horizontally long shape having a minor axis of 120 mm and a major axis of 3 to 40 mm can be mentioned.

(Production of non-disintegrable pesticide granules)

In the tumbling granulation method, a step of preparing a powdery granular material by adding an acidic agricultural chemical active ingredient, a cationic surfactant and a basic substance together with auxiliary components such as a binder and a bulking agent to a tumbling granulator, A step of preparing a granular composition having a target particle size and grain length by gradually adding an appropriate amount of water or an aqueous solution in which a binder is dissolved to the granular material, and, if necessary, applying a film to the surface of the granular composition. It consists of coating the forming substance, drying and then sieving.

[0038] In the extrusion granulation method, an acidic pesticide active ingredient, a cationic surfactant, and a basic substance are pulverized with an air mill or mechanochemical pulverized together with auxiliary ingredients such as a binder and a bulking agent to prepare a powdery raw material. Process: After kneading a mixture obtained by adding an appropriate amount of water to this powdery raw material using a twin-screw extruder, extruder, etc., the mixture is adjusted to have the target particle size and grain length. Extruding and granulating from a screen with a set aperture diameter to prepare a granular composition, and coating the granular composition with a film-forming substance on its surface, if necessary, drying, and sieving. Power.

[0039] In the coating granulation method, an acidic pesticide active ingredient, a basic substance, and auxiliary ingredients such as a cationic surfactant and a bulking agent used as needed are pulverized by an air mill or mechanochemical to prepare a powdery raw material. Process, oil-absorbing granules having the target particle size and target length are put into a conical screw-type mixer, and auxiliary components such as a cationic surfactant diluted with a solvent and a binder used as necessary are sprayed simultaneously. The oil-absorbing granular material obtained by mixing while mixing is coated with the powdery raw material obtained in the previous step, and the process of preparing the granular composition and drying the granular composition as necessary, and then sieving. Become. (Manufacture of granular pesticide formulations)

In the extrusion granulation method, the non-disintegrable pesticide granules, surfactants, and floating components obtained by the above-mentioned production method are combined with auxiliary components such as extenders, binders, stabilizers, and the like, which are used as necessary. The mixture is kneaded with an appropriate amount of water using an extrusion granulator or the like, and the resulting mixture is subjected to particle size and particle size of non-disintegrable pesticide granules. A step of preparing a granular composition by extruding and granulating a screen having a larger opening diameter, and coating the granular composition with a film-forming substance on its surface, if necessary, and drying it. The sieving process power is also increased.

In the tumbling granulation method, the non-disintegrable pesticide granules, surfactants and floating components obtained by the above-mentioned production method are mixed with auxiliary components such as a bulking agent, a binder and a stabilizer, which are used as necessary. A process of preparing a granular material by placing it in a tumbling granulator together with the pesticidal active ingredient, and gradually adding an aqueous solution in which an appropriate amount of water or a binder is dissolved to the granular material, and a granular composition having a target particle size and particle length. The step of preparing the product and the step of coating the particulate composition with a film-forming substance on its surface, if necessary, drying and sieving.

[0042] In these production methods, the drying treatment is preferably performed by an appropriate drying device such as a fluidized bed drying device or a vacuum drying device.

[0043] In the homogeneously diffusible granular pesticide preparation of the present invention, an acidic pesticide active ingredient having a pKa of 17 and, among others, a herbicide such as a herbicide composed of a sulfonylprea compound, particularly a compound represented by the general formula (I) It is preferable to use the difluoromethanesulfo-fluoride derivative or a salt thereof to be used, and a cationic surfactant which is a gel that gels in water or has a swelling property.

Hereinafter, the present invention will be described in detail with reference to Examples and Test Examples, but the present invention is not limited to these Examples. In addition, in each example, a part represents a mass part.

[0045] The pesticidal active ingredient used in the Examples had a deviation of pKa2-7, and the basic substance was a 1% by mass aqueous solution or a 1% by mass aqueous suspension having a pH of 7.5 or more. Each of the non-disintegrable pesticide granules was a 1% by mass aqueous suspension having a pH of 5 or more.

In addition, the cationic surfactants used in Examples 1, 7, 9 and 10 were all capable of gelling in water. [0047] Furthermore, the homogeneously diffusible granular pesticide formulation obtained in each example floated on the water surface immediately after being dropped on the water surface, but was disintegrated within 30 minutes, and the non-disintegrable pesticide granular material settled out.

Example 1

Bensulfuron methyl (pKa 5.03) 6.25 parts, distearyl dimethyl ammonium chloride 6.25 parts, dilauryl dimethyl ammonium chloride 6.25 parts, calcium carbonate 68.75 咅, polyvinylinoleanol 25 咅 ^ Hidani starch 6. The mixture obtained by uniformly mixing 25 咅 was pulverized with an impact pulverizer. The obtained powder is kneaded by adding an appropriate amount of water in a high-speed stirrer, and then extruded using a dome-type granulator through a screen having an aperture of 0.5 mm, and the granulated material is statically held at 60 ° C. After drying, pesticide granules containing 6.25% by mass of bensulfuron-methyl and having a diameter of 0.4-0.6 mm and a length of 16 mm were obtained. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and the particles were determined to be non-disintegrated.

[0049] Next, 32 parts of non-disintegrable pesticide granules, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, and a plastic hollow body made of Shiridani biylidene 'acrylonitrile copolymer plastic balloon [Matsumoto Microsphere F —30E (trade name, manufactured by Matsumoto Yushi Seiyaku Co., Ltd.) 14 parts, 20 parts of anhydrous sodium sulfate, 40.9 parts of urea, and a mixture of 40.9 parts of urea and an appropriate amount of water are kneaded in a twin-screw type, followed by extrusion granulation. Extruded and granulated from a screen with an opening diameter of 5 mm using a stirrer, sized to reach the target size, dried at 60 ° C with a fluidized bed drier, and sieved to obtain a 3-mm diameter. A granule containing 2% by mass of benzulfuron methyl having a length of 7 mm and a length of 3 to 20 mm was obtained as a uniform diffusible granular pesticide preparation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide particulates settled out.

Example 2

6.25 parts of bensulfuron methyl (pKa 5.03), 12.5 parts of dioleyl dimethylammonium-pum chloride, 62.5 parts of calcium carbonate, and 12.5 parts of bentonite are uniformly mixed. Crushed with a machine. The obtained powder was kneaded in a high-speed stirrer with 12.5 parts of an acrylic emulsion containing 50% solids and an appropriate amount of water, and then kneaded. Extruded and granulated from screen, and granulated product was dried at 60 ° C. After drying, pesticide granules containing 6.25% by mass of bensulfuron-methyl and having a diameter of 0.4 to 0.6 mm and a length of 16 mm were obtained. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and it was determined that the particles were not disintegrated.

[0051] Next, 32 parts of the non-disintegrating pesticide granules, 32 parts of mefenacet finely pulverized by an air mill, 1 part of dioctyl sulfosuccinate, 2 parts of polyoxyethylene acetylene glycol, 3 parts of enzyme-modified dextrin, A mixture of 12 parts of the plastic hollow body used in Example 1, 5 parts of bentonite, 10 parts of anhydrous sodium sulfate and 13.2 parts of urea mixed with an appropriate amount of water was kneaded in a twin-screw type and extruded. Extruded and granulated from a screen with an opening diameter of 5 mm using a granulator, sized to the target size, dried at 60 ° C with a fluidized-bed dryer, and sieved to obtain a diameter of 3 mm. Granules containing 2% by weight of vensulfuron methyl and 7% by length and 32% by mass of mefenacet, 3 to 20mm in length, were obtained as a uniform diffusible granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide particulates settled out.

Example 3

Compound A of the general formula (I) in which R ¹ is an ethyl group (hereinafter referred to as Compound A. _P Ka 6.17) 10 parts and basic white carbon 1.7 parts are uniformly mixed and pulverized with an air mill. A contained powder was prepared.

[0053] 75 parts of diatomaceous earth having a particle size of 16-35 mesh (1000-425 µm) is put into a conical screw mixer, and while mixing, separately 10 parts of dilauryl dimethylammonium-dimethyl chloride, 2 parts of propylene glycol, Polypropylene glycol (molecular weight: 1000) 1. A cationic surfactant solution prepared by heating and mixing 3 parts with a propeller mixer was charged. Immediately after completion of the charging, the compound A-containing powder is charged, uniformly mixed and granulated, and the granulated material is aged in a tray dryer at 60 ° C to obtain a pesticide particle having a particle size of 0.4 to 1.1 mm. I got something. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed, and no disintegrated particles were observed.

Next, 30 parts of the non-disintegrable pesticide granules, 3 parts of sodium dibutylnaphthalenesulfonate, 2 parts of lauryl sulfate, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, 1 part of sodium polyacrylate Parts, 2 parts of white carbon, A mixture of 14 parts of a plastic hollow body, 20 parts of anhydrous sodium sulfate, and 34.9 parts of urea mixed with an appropriate amount of water is kneaded in a twin-screw type, and then extruded using a granulator. After extrusion granulation and sizing to the target size, the product is dried at a product temperature of 60 ° C with a fluid bed dryer and sieved to obtain a compound with a diameter of 3-7 mm and a length of 3-20 mm. A particulate matter containing 3% by mass of the substance A was obtained as a uniform diffusible granular pesticide preparation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Example 4

7.5 parts of compound A (pKa6.17), 10 parts of N-methyl-2-pyrrolidone and 10 parts of dioleyldimethylammonium-dum chloride were mixed with a propeller-type mixer to prepare a solution containing compound A. The obtained solution is adsorbed on 75 parts of a basic acidic clay having a particle size of 16-35 mesh (1000-425 / zm), in which the pH of a 1% aqueous suspension is 7-10. 4--1 1mm pesticide granules were obtained. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and the particles were determined to be non-disintegrated.

Next, 40 parts of the non-disintegrating pesticide granules, 3 parts of sodium dibutylnaphthalenesulfonate, 2 parts of lauryl sulfate, 2 parts of polyoxyethylene acetylene glycol, 0.7 parts of sodium polyacrylate, and spherical hollow glass [Fuji Balloon (trade name), manufactured by Fuji Silicon Chemical Co., Ltd.] 20 parts, 15 parts of anhydrous sodium sulfate, and 17.3 parts of urea were uniformly mixed in a high-speed stirrer, and an appropriate amount of water was added and kneaded. Then, the obtained mixture is extruded and granulated from a screen with an opening diameter of 5 mm using a basket type granulator, and sized to the target size, and then a fluidized bed dryer at a product temperature of 60 ° C. By drying and sieving, a granular material containing 3% by mass of the compound A having a diameter of 3 to 7 mm and a length of 3 to 20 mm was obtained as a uniform diffusible granular pesticide preparation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Example 5

In the formula (I), R ¹ is a methoxymethyl group (hereinafter, referred to as compound B. _P Ka5.7.5) 10 parts, distearyl dimethylammonium chloride 6.7 parts, dilauryldimethylammonium chloride 6 7 parts, calcium carbonate 63.2 parts, polybutyl alcohol 6.7 parts, The mixture obtained by uniformly mixing 6.7 parts of arsenic starch was pulverized with an impact pulverizer. A mixture obtained by adding an appropriate amount of water to the obtained powder is kneaded with a high-speed stirrer, and then extruded using a dome-type granulator through a screen having an opening diameter of 0.5 mm, and the granulated material is heated at 60 ° C. After standing and drying, pesticide granules containing 10 mass% of compound B and having a diameter of 0.4 to 0.6 mm and a length of 16 mm were obtained. The obtained pesticidal granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and it was determined that the particles were not disintegrated.

Next, 30 parts of the non-disintegrable pesticide granules, 1 part of polyoxyethylene acetylene glycol, 2 parts of polyoxyethylene polyoxypropylene block polymer, 3 parts of polyoxyethylene styryl ether ether phosphate amine salt, enzyme modification A mixture of 3 parts of 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 and an appropriate amount of water was kneaded in a biaxial type. After that, it is extruded and granulated through a screen with an opening diameter of 5 mm using an extrusion granulator, sized to the target size, and dried at a product temperature of 60 ° C by a fluidized bed dryer and sieved. As a result, a granular material containing 3% by mass of the compound B having a diameter of 3 to 7 mm and a length of 3 to 20 mm was obtained as a uniform diffusible granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Example 6

Compound B (pKa 5.75) 6.25 parts, distearyl dimethylammonium chloride 12.5 parts, calcium carbonate 62.5 parts, bentonite 12.5 parts A uniformly mixed mixture was ground with an impact mill. . A mixture of 6.25 parts of acrylic emulsion and an appropriate amount of water in the obtained powder was kneaded with a high-speed stirrer, and the mixture was extruded and granulated through a screen having an aperture of 0.5 mm using a dome-type granulator. The granulated material was allowed to stand at 60 ° C. and dried to obtain a pesticide granule containing 6.25% by mass of compound B, having a diameter of 0.4 to 0.6 mm and a length of 16 mm. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were recognized, and it was determined that the particles were not disintegrated.

Next, 32 parts of the non-disintegrable pesticide granules, 1 part of the conjugated product B finely pulverized by an air mill, 1 part of polyoxyethylene acetylene glycol, 2 parts of polyoxyethylene polyoxypropylene block polymer, and 2 parts of polyoxyethylene Styryl ether ether phosphate amine salt 3 parts, yeast 3 parts of denatured dextrin, 14 parts of hollow plastic body used in Example 1, 5 parts of bentonite, 20 parts of anhydrous sodium sulfate, 30.9 parts of urea and a mixture of 30.9 parts of urea mixed with appropriate amount of water and kneaded in a twin-screw type After that, it is extruded and granulated from a screen with an opening diameter of 5 mm using an extrusion granulator, sized to the target size, dried at 60 ° C in a fluidized bed dryer and sieved. As a result, a granular material containing 3% by mass of compound B having a diameter of 3 to 7 mm and a length of 3 to 20 mm was obtained as a uniform diffusible granular pesticide formulation. The obtained homogeneously diffusible granular pesticide product was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Example 7

A mixture obtained by uniformly mixing 10 parts of Compound B (pKa 5.75), 13.3 parts of distearyldimethylammonium chloride, 56.9 parts of calcium carbonate, and 13.3 parts of bentonite was ground with an impact mill. A mixture obtained by adding 13 parts of an acrylic emulsion containing 50% solids to the obtained powder and an appropriate amount of water is kneaded with a high-speed stirrer, and then, using a dome-type granulator, a screen having an aperture of 0.5 mm. The mixture is extruded and granulated, and the granulated product is allowed to stand at 60 ° C. and dried to obtain a pesticide granule containing 10% by mass of compound B and having a diameter of 0.4 to 0.6 mm and a length of 16 mm. Obtained. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and the particles were determined to be non-disintegrated.

Next, 30 parts of the non-disintegrable pesticide granules, 8 parts of fentorazamide finely pulverized by an air mill, 5 parts of sodium dibutylnaphthalenesulfonate, 1 part of lauryl sulfate, 3 parts of polyoxyethylene acetylene glycol, 3 parts of enzyme-modified dextrin 2 Part, 0.5 part of sodium polyacrylate, 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, 28.4 parts of urea, and a mixture obtained by adding an appropriate amount of water to a biaxial type-dapper. After kneading, the mixture is extruded and granulated through a screen with a mesh size of 5 mm using an extrusion granulator, sized to the target size, and dried at 60 ° C in a fluidized bed dryer. By sieving, a granular material containing 3% by mass of compound B and 3% by mass of fentrazamide having a diameter of 3 to 7 mm and a length of 3 to 20 mm was obtained as a homogeneously diffusible granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out. Example 8

6. Birazosulfronethyl (pKa 3.91) 6. 25 parts, cetyltrimethylammonium chloride 6. Canoresium carbonate 68. Posivininoleanolecone olecole 18. Mix uniformly mixed 75. And crushed. The obtained powder is kneaded by kneading an appropriate amount of water in a high-speed stirrer, and then extruded using a dome-type granulator through a screen with an aperture of 0.5 mm, and the granulated material is cooled at 60 ° C. After standing and drying, pesticide granules containing 6.25% by mass of birazosulfronethyl and having a diameter of 0.4 to 0.6 mm and a length of 16 mm were obtained. The pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. No disintegrated particles were observed, and the particles were judged to be non-disintegrated.

Next, 16 parts of the non-disintegrating pesticide granules, 5 parts of sodium salt of butyl naphthalenesulfonic acid formalin condensate, 1 part of polyoxyethylene acetylene glycol, 0.5 part of sodium polyacrylate, Example 1 A mixture of 14 parts of the plastic hollow body used in the above, 20 parts of anhydrous sodium sulfate, and 55.4 parts of urea and an appropriate amount of water was kneaded in a high-speed stirrer, and then a 5 mm screen with an extrusion granulator was used. After extrusion granulation, sizing to the target size, drying at 60 ° C with fluidized bed dryer and sieving, villas of 3-7 mm in diameter and 3-20 mm in length the granules containing Brazosport iodosulfuron E chill 1 mass ^_0/0 was obtained as a uniform one diffusible granular pesticide formulations. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Example 9

A mixture obtained by uniformly mixing 20 parts of tricyclazole (pKal. 6), 15 parts of distearyl dimethylammonium-dimethyl chloride, 55 parts of calcium carbonate, and 10 parts of polybutyl alcohol was pulverized with an impact pulverizer. The obtained powder is kneaded by adding an appropriate amount of water in a high-speed stirrer, and then extruded using a dome-type granulator through a screen having an aperture of 0.7 mm, and the granulated material is heated at 60 ° C. After standing and drying, pesticide granules containing 20% by mass of tricyclazole and having a diameter of 0.6 to 0.8 mm and a length of 2 to 9 mm were obtained. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed, and no disintegrated particles were observed. Next, 40 parts of the non-disintegrating pesticide granules, 5 parts of sodium salt of butyl naphthalenesulfonic acid formalin condensate, 1 part of polyoxyethylene acetylene glycol, 0.5 part of sodium polyacrylate, and a plastic hollow body Acrylonitrile plastic balloon [Matsumoto Microsphere F-80E (trade name), manufactured by Matsumoto Yushi Seiyaku Co., Ltd.] 14 parts, anhydrous sodium sulfate 20 parts, urea 31.4 parts, and a mixture obtained by adding an appropriate amount of water After kneading with a high-speed stirrer, the mixture is extruded and granulated through a screen with an opening diameter of 5 mm using an extrusion granulator, and sized to the target size. By drying and sieving, a granule having a diameter of 3 to 7 mm and a length of 3 to 20 mm and containing 8% by mass of tricyclazole was obtained as a uniform diffusible granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Example 10

A mixture obtained by uniformly mixing 20 parts of PHC (pKall.6), 15 parts of distearyl dimethylammonium chloride, 55 parts of carbonated calcium carbonate, and 10 parts of polybutyl alcohol was pulverized with an impact pulverizer. A mixture obtained by adding an appropriate amount of water to the obtained powder is kneaded with a high-speed stirrer, and then extruded and granulated from a screen having an opening diameter of 0.7 mm using a dome-type granulator. To obtain a pesticide granule containing 20% by mass of PHC and having a diameter of 0.6 to 0.8 mm and a length of 2 to 9 mm. The obtained pesticide granules were dropped into water, and after 30 minutes, the collapse state of the particles was observed. As a result, no disintegrated particles were observed, and the particles were judged to be non-disintegrated.

Next, 40 parts of the non-disintegrable pesticide granules, 5 parts of sodium salt of formalin condensate of butyl naphthalenesulfonic acid, 1 part of polyoxyethylene acetylene glycol, 0.5 part of sodium polyacrylate, Example 9 A mixture of 14 parts of the plastic hollow body, 20 parts of anhydrous sodium sulfate, and 31.4 parts of urea to which an appropriate amount of water was added was kneaded with a high-speed stirrer, and the mixture was extruded through a 5 mm screen with an extrusion granulator. Extruded and granulated, sized to the target size, dried at 60 ° C with fluidized bed dryer and sieved to obtain PHC8 mass of 3-7 mm in diameter and 3-20 mm in length. % Was obtained as a homogeneously diffusing granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out. [0069] Comparative Example 1

A mixture obtained by uniformly mixing 6.25 parts of bensulfuron-methyl (pKa5.03), 81.25 parts of calcium carbonate, 6.25 parts of polybutyl alcohol, and 6.25 parts of pregelatinized starch was pulverized with an impact mill. A mixture obtained by adding an appropriate amount of water to the obtained powder is kneaded with a high-speed stirrer, and then extruded using a dome-type granulator through a screen having an opening diameter of 0.5 mm, and granulated at 60 ° C. To obtain a pesticide granule containing 6.25% by mass of bensulfuron-methyl and having a diameter of 0.4 to 0.6 mm and a length of 16 mm. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and the particles were judged to be non-disintegrated.

Next, 32 parts of the non-disintegrable pesticide granules, 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, urea After kneading the mixture obtained by adding an appropriate amount of water to 40.9 parts in a biaxial type, extruding it through a screen with an opening diameter of 5 mm using an extrusion granulator to obtain the target size. After sizing, the dried in a fluid-bed dryer at product temperature 60 ° C, by kicking sieve fraction, granular and containing not Nsu bensulfuron methyl 2 mass ^_0/0 mentioned diameter 3- 7 mm, length 3- 20 mm The product was obtained as a homogeneously diffusing granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-collapsible pesticide particulates settled out.

[0071] Comparative Example 2

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

[0072] Into a conical screw type mixer, 75 parts of diatomaceous earth particles having a particle size of 16-35 mesh (1000-425 µm) are put, and while mixing, 12 parts of propylene glycol and polypropylene dalicol (molecular weight: 1000) are separately added. A solution prepared by heating and mixing 3 parts with a propeller mixer was charged. Immediately after the completion of the charging, the above-mentioned powder containing compound A is charged, uniformly mixed and granulated, and the granulated material is aged in a tray dryer at 60 ° C to obtain a pesticide having a particle size of 0.4 to 1.1 mm. Got. The pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and the particles were judged to be non-disintegrated. Next, 30 parts of the non-disintegrable pesticide granules, 3 parts of sodium dibutylnaphthalenesulfonate, 2 parts of lauryl sulfate, 3 parts of polyoxyethylene acetylene glycol, 2 parts of enzyme-modified dextrin, 1 part of sodium polyacrylate Parts, 2 parts of white carbon, 14 parts of the plastic hollow body used in Example 1, 20 parts of anhydrous sodium sulfate, and 34.9 parts of urea, and a mixture obtained by adding an appropriate amount of water to the mixture. After extruding and granulating from a screen with a mesh size of 5 mm using an extrusion granulator, sizing to the target size, drying at 60 ° C with a fluidized bed dryer and sieving. As a result, a granular material containing 3% by mass of the compound A having a diameter of 3 to 7 mm and a length of 3 to 20 mm was obtained as a uniform diffusible granular pesticide formulation. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

[0074] Comparative Example 3

Compound B (pKa 5.75) 10 parts, distearyl dimethylammonium chloride 6.7 parts, dilauryldimethylammonium chloride 6.7 parts, clay 63.2 parts, polybutyl alcohol 6.7 parts, pregelatinized starch 6. The mixture obtained by uniformly mixing 7 parts was pulverized with an impact pulverizer. A mixture obtained by adding an appropriate amount of water to the obtained powder is kneaded with a high-speed stirrer, and then extruded and granulated through a screen having an opening diameter of 0.5 mm using a dome-type granulator. To obtain a pesticide granule containing 10% by mass of compound B and having a diameter of 0.4 to 0.6 mm and a length of 16 mm. The pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. No disintegrated particles were observed, and the particles were judged to be non-disintegrated.

Next, 30 parts of the non-disintegratable pesticide granules, 1 part of polyoxyethylene acetylene glycol, 2 parts of polyoxyethylene polyoxypropylene block polymer, 3 parts of polyoxyethylene styryl ether ether phosphate amine salt, enzyme modification A mixture of 3 parts of dextrin, 14 parts of the hollow plastic body used in Example 1, 20 parts of anhydrous sodium sulfate, and 38.9 parts of urea and an appropriate amount of water was kneaded in a twin-screw type, and then extruded. Extruded through a screen with an opening diameter of 5 mm, granulated to a target size, dried at 60 ° C with a fluidized-bed dryer, and sieved to obtain a 3-diameter. A granular material containing 3% by mass of compound B having a size of 7 mm and a length of 3 to 20 mm was obtained as a homogeneously diffusible granular pesticide formulation. The obtained homogeneously diffusible particulate pesticide formulation was dropped into water and observed. The particles of the agent disintegrated, and the non-disintegrating pesticide granules settled.

Comparative Example 4

6.25 parts of Birazosulfronethyl (pKa 3.91), 12 parts of 《raffine (melting point 68-70.C), 63.75 parts of calcium carbonate, 18 parts of polybutyl alcohol It was crushed by a pulverizer. A mixture obtained by adding an appropriate amount of water to the obtained powder is kneaded with a high-speed stirrer, and then extruded and granulated through a screen having an opening diameter of 0.5 mm using a dome-type granulator, and the granulated material is heated at 70 ° C. After standing and drying, pesticide granules containing 6.25% by mass of birazosulfronethyl and having a diameter of 0.4 to 0.6 mm and a length of 16 mm were obtained. The obtained pesticide granules were dropped into water, and after 30 minutes, the disintegration state of the particles was observed. As a result, no disintegrated particles were observed, and it was determined that the particles were not disintegrated.

Next, 16 parts of the non-disintegrable pesticide granules, 5 parts of sodium salt of butyl naphthalenesulfonic acid formalin condensate, 1 part of polyoxyethylene acetylene glycol, 0.5 part of sodium polyacrylate, Example 1 A mixture of 14 parts of the plastic hollow body used in the above, 20 parts of anhydrous sodium sulfate, and 55.4 parts of urea and an appropriate amount of water was kneaded with a high-speed stirrer, and then extruded using a granulator with a screen having an aperture of 5 mm. After extrusion granulation and sizing to the target size, the product is dried at 60 ° C in a fluidized bed drier and sieved to obtain virazos with a diameter of 3-7 mm and a length of 3-20 mm. the granules containing Rufuronechiru 1 mass ^_0/0 was obtained as a uniform one diffusible granular pesticide formulations. The obtained homogeneously diffusible granular pesticide formulation was dropped into water and observed. As a result, the particles of the formulation were disintegrated within 30 minutes, and the non-disintegrated pesticide granules settled out.

Test Example 1 (Dissolution test in water)

Eight liters of tap water was placed in an enamel bat 50 cm long and 40 cm wide to a depth of 4 cm. The homogeneously diffusible granular pesticide preparations of Examples 1-110 and Comparative Examples 1-4 were applied thereto so as to be equivalent to 250 g per 10 ares. Water was sampled 1, 3, 7, 21, and 35 days after treatment, and the concentration of the components in the water was determined as the dissolution rate in water by HPLC analysis. The results are shown in Table 1.

[table 1]

[0079] From Table 1, it can be seen that the homogeneously diffusible granular pesticide preparation of Example 17 is characterized in that the pesticidal active ingredient is a herbicide sulfolureurea-based compound or difluoromethanesulfo-lua-lide derivative or a salt thereof. The dissolution rate in water was lower than that in Comparative Example 13 in the test from 1 day to 35 days after the treatment, indicating that the drug was controlled to be released gradually.

[0080] Further, comparing Example 8 with Comparative Example 4, the latter has a lower concentration in water than the former, and the elution of the pesticidal active ingredient is only a small portion at the initial stage and does not continue. Many of the pesticidal active ingredients in the uniform diffusible granular pesticide formulation remain unused! /, Clearly inferior.

[0081] Further, when Example 5 and Comparative Example 3 are compared, the latter has a higher water concentration than the former, and the sustained release of the pesticide active ingredient is reduced due to the absence of a basic substance. You can see.

[0082] Test Example 2 (Field diffusibility)

From the two windward sides of a paddy field having a short side of 20 m, a long side of 50 m, and a water depth of 5 cm shown in FIG. 1, the uniformly diffusible granular pesticide preparation of Example 5 was sprayed by hand. Forty-eight hours after spraying, water is collected from point (A-L) shown in Fig. 1 and analyzed. Was calculated, and the standard deviation of the concentration in water at each point was divided by the average to calculate the fluctuation rate. The results are shown in Table 2.

[Table 2]

[0083] From Table 2, it can be seen that when this homogeneously diffusible granular pesticide preparation is applied, the uniformity of the pesticide active ingredient in water is good.

Industrial applicability

[0084] The homogeneously diffusible granular pesticidal preparation of the present invention can be prepared by a simple method, and moderately releases the dissolution of the pesticidal active ingredient, whereby the efficacy of the pesticidal active ingredient can be maintained for a long period of time. Spray a granular pesticide formulation that can exert its effect and reduce the environmental burden by reducing the release of pesticide active ingredients into the environment, and reduce or prevent harm caused by the pesticide active ingredients, for example, harm to target crops. The method enables uniform diffusion throughout the paddy field, and has a remarkable effect of contributing to labor saving in agricultural work.

Claims

The scope of the claims

[1] Contains no acidic pesticide active ingredient, cationic surfactant and basic substance. Does not disintegrate in water within 30 minutes! し Contains non-disintegrable pesticide granules, surfactant and floating component, It has a particle size distribution in which the mass ratio of particles with a particle diameter of 3 mm or more is 80% by mass or more and has the property of floating on the water surface immediately after being dropped on the water surface, but is characterized by collapse on the water surface within 30 minutes Uniformly diffusible granular pesticide formulation.

[2] The homogeneously diffusible granular pesticide preparation according to claim 1, which has an acidic pesticide active ingredient power of Ka2-7.

[3] The homogeneously diffusible granular pesticide preparation according to claim 1, wherein the acidic pesticide active ingredient is a herbicide.

[4] The uniformly dispersible granular pesticide preparation according to claim 3, wherein the herbicide is a sulfonyliderea compound.

[5] herbicide is a general formula

[Chemical 1]

(Wherein R ¹ is a hydrogen atom, an alkyl group or an alkoxyalkyl group), or a difluoromethanesulfo-l-lide derivative or a salt thereof. Granular pesticide formulation.

[6] The homogeneously diffusible granular pesticide preparation according to claim 1, wherein the cationic surfactant exhibits a gelling property or swelling property in water.

[7] The uniform diffusivity according to claim 1, wherein the basic substance is sodium hydrogencarbonate, sodium carbonate, calcium hydroxide, calcium carbonate, basic white carbon or basic acid clay. Granular pesticide formulation.

[8] The homogeneously diffusible granular pesticide preparation according to claim 1, wherein the floating component is an inorganic hollow body or a plastic hollow body.

[9] Contains acidic pesticide active ingredient, cationic surfactant and basic substance, and does not disintegrate in water within 30 minutes. ヽ Non-disintegrable pesticide granules can be granulated together with surfactant and floating ingredient. A method for producing a homogeneously diffusible granular pesticide formulation, comprising a spherical shape with a particle diameter of 11 to 20 mm or a horizontally long shape with a short diameter of 1 to 20 mm and a long diameter of 3 to 40 mm.

10. The production method according to claim 9, wherein the granulation treatment is performed by extruding and granulating the non-disintegrable pesticide granules from a staline having an opening diameter larger than the particle diameter or the particle length.

[11] Do not disintegrate in water within 30 minutes containing the acidic pesticide active ingredient, cationic surfactant and basic substance! を Non-disintegrable pesticide granules and pesticide active ingredient Uniformly diffusible granular pesticide formulation that has been subjected to granulation together with a playful component and has a spherical shape with a particle diameter of 11 to 20 mm! /, A horizontal shape of a short diameter of 11 to 20 mm and a long diameter of 3 to 40 mm Manufacturing method.

12. The production method according to claim 11, wherein the granulation treatment is carried out by extruding and granulating the non-disintegrable pesticide granules from a staline having an opening diameter larger than the particle diameter or the particle length.