KR20090082109A - Pesticide Preparation - Google Patents

Abstract

A method for producing a pesticide granule for kneading, extruding, and drying a granulated product comprising a mixture comprising an agrochemical active ingredient, a plastic microhollow, a surfactant, a binder, and calcium carbonate, the content of water in the composition obtained by kneading 15 wt% to 25 wt%, the content of calcium carbonate is 30 wt% to 90 wt% in the mixture before kneading with water, and the amount of calcium carbonate is 15 to 30 wt parts with respect to 1 wt part of the plastic microhollow; The pesticide preparation obtained by the manufacturing method of the phosphorus pesticide preparation is excellent in the floating property on the water surface, the diffusibility, etc., and is suitable for application in rice fields. Moreover, this manufacturing method can manufacture agriculturally effective pesticide industrially efficiently.

Description

Production method of pesticide preparation {PROCESS FOR PREPARING AGROCHEMICAL GRANULES}

The present invention relates to a method for producing pesticide preparation and a method for preparing pesticide preparation enclosed in a water-soluble film.

It is known to spread pesticide active ingredients throughout the paddy field by applying a pesticide granule containing a floating aid to a specific gravity of less than 1 in the paddy field and by floating and diffusing the applied pesticide paddle on the water surface.

In addition, a method of spreading a pesticide active ingredient widely throughout the paddy field is also known by introducing a packaged pesticide preparation in which the pesticide filler is encapsulated in a water-soluble film or the like.

Japanese Laid-Open Patent Publication No. 2006-257082 discloses a non-pesticide pesticide containing a condensed heterocyclic sulfonyl urea compound and pyraclonil as an active ingredient for pesticides. This causes problems such as insufficient water suspension and diffusivity of the pesticide preparation to be produced, or inability to manufacture efficiently, such as attaching granules to each other at the time of manufacture.

The present invention provides a method for industrially and efficiently producing a water-floating agrochemical pesticide excellent in water floating and diffusing properties.

The present invention relates to a process for preparing agrochemical granules for kneading, extruding and kneading a mixture comprising an agrochemical active ingredient, a plastic microhollow, a surfactant, a binder and calcium carbonate, and drying the granulated product. By adjusting the amount of use to a specific range, it is possible to efficiently produce a water-floating agrochemical pesticide excellent in water floatability and diffusivity.

That is, this invention is as follows.

1.A method for producing a pesticide preparation for kneading, extruding and drying a granulated product of a mixture comprising an agrochemical active ingredient, a plastic microhollow, a surfactant, a binder, and calcium carbonate, and obtained by kneading. The content of water in the composition is 15% by weight to 25% by weight, the content of calcium carbonate in the mixture before kneading with water is 30% by weight to 90% by weight, and the amount of calcium carbonate is contained in 1 part by weight of the plastic microhollow. The manufacturing method of the pesticide granules which is the ratio of 15-30 weight part with respect to.

2. The method for producing the pesticide preparation according to 1 above, which is dried so that the content of water in the pesticide preparation is 0.1% by weight to 2% by weight.

3. The manufacturing method of the pesticide granulation agent as described in said 1 or 2 whose surfactant is polycarboxylic acid type surfactant.

4. The manufacturing method of the pesticide granulation as described in said 1-3 whose binder is carboxymethylcellulose sodium.

5. Pesticide active ingredient, plastic micro hollow body, surfactant. A process for preparing a pesticide granule for kneading a mixture comprising a binder, calcium carbonate and bentonite with water, extruding and drying the granulated product, wherein the content of water in the composition obtained by kneading is 15% by weight to 25% by weight, and water The content of calcium carbonate in the mixture before kneading with 30% by weight to 90% by weight, the amount of calcium carbonate is a method of producing a pesticide granules in the proportion of 15 to 30 parts by weight relative to 1 part by weight of the plastic micro-hollow.

6. A method for producing a pesticide preparation for kneading, extruding and kneading a mixture comprising an agrochemical active ingredient, a plastic microhollow, a surfactant, a condensate phosphate, a binder and calcium carbonate, and drying the granulated product. The content of water in the composition is 15% by weight to 25% by weight, the content of calcium carbonate is 30% by weight to 90% by weight in the mixture before kneading with water, and the amount of calcium carbonate is 15 parts by weight of 1 part by weight of the plastic microhollow. The manufacturing method of the pesticide preparation which is the ratio of -30 weight part.

7. A method for producing a packaged pesticide preparation, which encapsulates the pesticide granules obtained by the above production methods in a water-soluble film.

The production method of the present invention comprises kneading a mixture with water containing agrochemical active ingredients, plastic microhollows, surfactants, binders and calcium carbonates, which may further contain bentonite and / or condensed phosphates ("kneading process") It is the manufacturing method of the pesticide granules which carry out extrusion granulation ("assembly process"), and dry a granulated material ("drying process").

The pesticide active ingredient is not particularly limited, and conventionally known compounds such as various herbicides, plant growth regulators, fungicides, insecticides, acaricides, nematicides and the like can be used. In addition, an agrochemical active ingredient can be used individually or in combination of 2 or more types.

Examples of the active ingredient compounds of the herbicide include (a) sulfonylurea herbicides, and (b) carbamate herbicides. (c) chloroacetanilide herbicides, (d) triazine herbicides, (e) acidamide or urea herbicides, and (f) other herbicide active compounds Can be mentioned. Herbicides can be used individually or in combination of 2 or more types.

As a representative example of the active ingredient compound of the sulfonyl urea herbicide (a), the following formula (I)

[Wherein Q is the following formula (Q1), (Q2), (Q3) or (Q4)

(Wherein R ¹ is a hydrogen atom, a halogen atom, a cyano group, a nitro group, a lower alkyl group which may be substituted with a halogen atom, a lower alkoxy group which may be substituted with a halogen atom, a lower alkylthio group, a lower alkylsulfinyl group, a lower alkyl) A sulfonyl group, an amino group, a lower alkylamino group or a lower alkylamino group, R ² represents a lower alkyl group which may be substituted with a hydrogen atom, a halogen atom or a halogen atom, and R ³ represents a hydrogen atom, a halogen atom, a cyano group or a nitro group , A lower alkyl group which may be substituted with a halogen atom, a 3-6 membered cycloalkyl group which may be substituted with a halogen atom or a lower alkyl group, a lower alkenyl group which may be substituted with a halogen atom, a lower alkynyl group optionally substituted with a halogen atom, or a halogen atom Lower alkoxy group, lower alkylthio group, lower alkyl which may be substituted A condensed heterocyclic group represented by a pinyl group, a lower alkylsulfonyl group, an amino group, a lower alkylamino group or a dialkyl alkylamino group), and Y and Z are the same or different, and lower alkyl groups and halogen atoms which may be substituted with halogen atoms. And a lower alkoxy group or halogen atom which may be substituted].

In formula (I), "lower" in a lower alkyl group, lower alkenyl group, lower alkoxy group, lower alkylthio group, etc. means that the hydrocarbon moiety has 1 or 2 to 6 carbon atoms (preferably 1 or 2 to 4 carbon atoms). It is comprised by).

Examples of the "halogen atom" include fluorine, chlorine, bromine and iodine atoms. Examples of the "lower alkyl (group)" include linear or branched alkyl groups having 1 to 4 carbon atoms, such as metel, ethyl, propyl, isopropyl, butyl, isobutyl, s-butyl and t-butyl groups. Examples of the "lower alkoxy group" include linear or branched alkoxy groups having 1 to 4 carbon atoms, such as methoxy, ethoxy, propoxy, isopropoxy and t-butoxy group. As the "lower alkenyl group", for example, ethenyl, 1-propenyl, 2-propenyl, 1,2-propadienyl, 1-butenyl, 2-butenyl, 3-butenyl, 1,3-buta A dienyl group etc. are mentioned. Examples of the "lower alkynyl group" include ethynyl, 1-propynyl, 2-propynyl, 1-butynyl, 2-butynyl group, and the like. Examples of the "3- to 6-membered cycloalkyl group" include cyclopropyl, cyclobutyl, cyclopentyl, and cyclohexyl groups.

As a condensed heterocyclic group represented by Q, the imidazo [1, 2-b] pyridazine group represented by Formula (Q1), the imidazo [1, 2-a] pyridine group represented by Formula (Q2), and formula (Q3) The pyrazolo [1, 5-a] pyrimidine group shown by the following, and the pyrazolo [1, 5-b] thiazole group shown by Formula (Q4) are mentioned.

As R ¹ , a halogen atom or a lower alkyl group which may be substituted with a halogen atom is preferable, and a chlorine atom is more preferable among them. As R <^2> , the lower alkyl group which may be substituted by the hydrogen atom, the halogen atom, or the halogen atom is preferable, and the hydrogen atom is more preferable especially. As R ³ , a lower alkyl group which may be substituted with a hydrogen atom, a halogen atom or a halogen atom, a 3-6 membered cycloalkyl group which may be substituted with a halogen atom or a lower alkyl group, a lower alkoxy group which may be substituted with a halogen atom, or a lower alkylthio group , A lower alkylsulfinyl group, a lower alkylsulfonyl group, a lower alkyl amino group or a dialkyl alkylamino group is preferable, and a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, or a 3-6 membered cycloalkyl group is particularly preferable. As Y and Z, the lower alkyl group which may be substituted by the halogen atom, or the lower alkoxy group which may be substituted by the halogen atom is preferable, and especially a methoxy group is more preferable.

Specific examples of the active ingredient compound of the sulfonyl urea herbicide (a) include bensulfuron-methyl, pyrazosulfuron-ethyl, azimsulfuron, sulfosulfuron, Imazosulfuron and the like.

Examples of active ingredient compounds of the carbamate herbicide (b) include di-allate, butylate, tri-allate, phenmedipham, chlorbufam ), Asulam, phenisopham, benthiocarb, molinate, esprocarb, pyributicarb, dimepiperate, swept (swep) etc. are mentioned.

Specific examples of the active ingredient compounds of the chloroacetanilide herbicide (c) include propachlor, metazachlor, alachlor, acetochlor, metolachlor, Butachlor, pretilachlor, tenylchlor, and the like.

Specific examples of active ingredient compounds of triazine herbicides (d) include simazine, atrazine, propazine, cyanazine, amethrin, and simetryn. ), Dimethametry (n), promethrin (prometry n) and the like.

Specific examples of the active ingredient compounds of the acid amide or urea herbicides (e) include isoxaben, diflufenican, diuron, linuron, and fluometuron. ), Difenoxuron, methyldymron, isoproturon, isouron, tebuthiuron, metabenzothiazuron, methodabenzthiazuron, propane, Mefenacet, clomeprop, naproanilide, bromobutide, dymron, cumyluron, etobenzanid, etc. Can be.

Moreover, as a specific example of the active ingredient compound of other herbicides (f), betazone, tridiphane, indanofan, amitrol, carfentrazone-ethyl , Sulfentrazone, fenchlorazole-ethyl, pentrazamide, isoxaflutole, clomazone, maleic hydrazide, pyri Pyridate, chloridazon, norflurazon, pyrithiobac, bromacil, terbacil, metrizin, metribuzin, oxazilomethone ( oxaziclomefone, cinmethylin, flumiclorac-pentyl, cinidon-ethyl, flumioxazin, fluthiacet-methyl, azaphenidine (azafenidin), benfuresate, oxadiazon, oxadiargyl, pentoxazone, Cyhalofop-butyl, carpenstrol, pyliminobac-methyl, bispyribac-sodium, pyrimisulfan, pyribenzoxim ), Pyriftalid, indanofan, quinoclamine, benzobicyolon, dithiopyr, dalapon, chlorthiamid, phenoxysullam (penoxsulam) etc. are mentioned.

As active ingredient compounds of plant growth regulators, for example, hymexazol, paclobutrazol, uniconazole-P, inabenfide, prohexadione-calcium Etc. can be mentioned.

As an active ingredient compound of a fungicide, for example, an active ingredient compound of a polyhaloalkylthio type fungicide (captan, etc.), an active ingredient compound of an organophosphorus fungicide [IBP (iprobenfos), EDDP (edifenphos), tolclophosphmethyl ( tolclofos-methyl], active ingredient compounds of benzimidazole-based fungicides [benomyl, carbendazim, thiophanate-methyl, etc.], active ingredient compounds of carboxyamide-based fungicides Mepronil, flutolanil, thifluzamide, furametpyr, tecloftalam, pencycuron, carpropamid, dichloro Diclocymet, etc.], active ingredient compounds of acylalanine fungicides (metalaxyl, etc.), active ingredient compounds of azole fungicides [triflumizole, ipconazole, peprazo Pefurazoate, prochloraz ), Etc., active ingredient compounds of methoxyacrylic acid fungicides [azoxystrobin, metominostrobin, etc.], active ingredient compounds of antibiotic fungicides [validamycin A, blastcydine S (Blastcidin-S), kasugamycin, polyoxins, etc.], and other active ingredient compounds of fungicides (phthalide, probenazole, isoprothiolane, Tricyclazole, pyroquilon, ferimlzone, acibenzolar-S-methyl, dilomezine, oxolinic acid, phenazine oxide (phenazineoxide), TPN ,: iprodione, etc.] etc. are mentioned.

As active ingredient compounds of the insecticide, for example, organophosphorus compounds (fenthion, fenitrothion, pirimiphos-methyl, diazinon, quinalphos, isoxation) (isoxathion), pyridaphenthion, chlorpyrifos-methyl, vamidothion, malathion, phenthoate, dimethoate, disulfotone (disulfoton), monocrotophos, tetrachlorvinphos, chlorfenvinphos, propaphos, acephate, trichlorfon, EPN, pyrachlor Pyraclofos, etc.], carbamate compounds (carbaryl, metolcarb, isoprocarb, BPMC, propoxur, XMC, carbofuran, carbosulphan (carbosulfan), benfuracarb, frurathioc arb), methomyl, thiodicarb, etc.], synthetic pyrethroid compounds (cycloprothrin, etofenprox, etc.), neraistoxin compounds (cartap, ben) Bensultap, thiocyclam, etc.], neonicotinoid compounds (imidacloprid, nitenpyram, acetamiprid, thiamethoxam, thiamethoxam, thiacloprid ( thicloprid, dinotefuran, clotianidin, etc.], and other active ingredient compounds of pesticides (buprofezin, tebufenozide, fipronil, Ethiprole, etc.] etc. are mentioned.

Examples of active ingredient compounds of acaricide include hexythiazox, pyridaben, fenpyroximate, tebufenpyrad, chlorfenapyr and ethoxazole. And pyrimidifen.

Examples of the active ingredient compounds of the nematicides include phosphthiazate and the like.

As an agrochemical active ingredient, the active ingredient compound of the herbicide is especially preferable.

Moreover, as an agrochemical active ingredient, the water solubility in 20 degreeC is 50 mg / ml or less normally, The thing of the range of 0.00001 mg / ml-10 mg / ml is preferable, Especially it is O.OOO1 mg / ml- Preferred is in the range of 1 mg / ml. The present invention is particularly useful for such solid pesticide active ingredients having low water solubility, that is, poorly water-soluble solid pesticide active ingredients.

The amount of the pesticide active ingredient used is usually 0.1% by weight to 45% by weight, preferably 0.2% to 40% by weight, more preferably 0.5% to 30% by weight in the mixture before kneading with water. It is enough.

The plastic microhollow body used in the present invention is a small hollow shell made of plastic. Since a plastic microhollow body is used to give buoyancy to the pesticide preparation manufactured, the external specific gravity is less than one. As a material of the outer sheath of a plastic microhollow body, vinylidene chloride- acrylonitrile resin, an acrylonitrile resin, an acryl resin, etc. are mentioned, for example, The particle diameter is about 1 micrometer-300 micrometers normally. As such a plastic microhollow body, what is normally marketed as a mixture with water can be used as it is, and as a specific example, Matsumoto micro spare F-30E (Matsumoto Oil Holding Co., Ltd. brand name, particle diameter: 20 micrometers-120 micrometers vinylidene chloride-acrylic) 10% by weight of ronitrile resin microhollow and 90% by weight of water), Matsumoto Micropair F-80E (Matsumoto Oil Holding Co., Ltd. product name, particle diameter: 20 micrometers-150 micrometers vinylidene chloride acrylonitrile resin micro hollow body 15 Wt% and a mixture of 85 wt% of water).

The amount of plastic microhollows used is usually 0.5% by weight to 5% by weight, preferably 0.5% by weight to 3% by weight, more preferably about 1% by weight to 3% by weight in the mixture before kneading with water. to be. If the amount of plastic microhollows is too small, the floating property of the water-floating pesticide agent is likely to be insufficient, and if too large, the granulation property is lowered and the amount of the pesticide active ingredient and the surfactant is relatively low. Efficacy and spreadability as pesticides fall easily.

Although the kind of surfactant is not specifically limited in this invention, A polycarboxylic acid type surfactant or a nonionic surfactant is preferable. Surfactant can be used individually or in combination of 2 or more types.

Examples of the polycarboxylic acid surfactant include salts of copolymers of maleic acid and styrenesulfonic acid, salts of copolymers of isobutylene or diisobutylene and maleic acid, salts of copolymers of maleic acid and acrylic acid, and acrylic acid polymers. And salts thereof. Examples of the salts include alkali metal salts such as sodium salts and potassium salts; Alkaline earth metal salts such as calcium salts and magnesium salts; Ammonium salt etc. are mentioned.

An acetylene glycol type surfactant is mentioned as a nonionic surfactant. As the specific example, polyoxyethylene acetylene diol (brand name "Olphin E101O" (made by Nisshin Chemical Co., Ltd.), etc.) is mentioned.

Moreover, an alkanediol derivative can also be used as a nonionic surfactant component. Alkanediol derivatives are compounds represented by the following general formula (II).

Here, X <^1> represents a C6-C14 divalent saturated hydrocarbon group, A <^1> and A <^2> respectively represent a C2-C4 alkylene group, and m and n each represent an integer. However, the sum of m and n is any one of integers 1-7, and when m is an integer of 2 or more, each A ¹ is the same or different from each other, and when n is an integer of 2 or more, each A ² is equal to each other Or different.

Examples of the divalent saturated hydrocarbon group having 6 to 14 carbon atoms in X ¹ include hexamethylene, heptamethylene, octamethylene, nonamethylene, decamethylene, and undecamethylene. C6-C14 linear alkylene group of undecamethylene, dodecamethylene, tridecamethylene, and tetradecamethylene; Carbon number such as 2-butyl-2-ethyltrimethylene, 2,4-diethylpentamethylene, 2-methyloctamethylene, etc. The branched alkylene group of -14, etc. are mentioned.

As X <^1> , a C6-C14 branched alkylene group is especially preferable. Moreover, as X <^1> , it is also preferable that it is a C9 or 10 divalent saturated hydrocarbon group.

Examples of the alkylene group having 2 to 4 carbon atoms in A ¹ and A ² include linear or branched alkylene groups such as ethylene, propylene, trimethylene, and tetramethylene groups. Can be mentioned.

The range of 6-14 is preferable and, as for HLB (Hydrophile-Lipophile Balance) of the alkanediol derivative represented by Formula (11), the range of 8-12 is more preferable.

The alkanediol derivative represented by Formula (11) can be manufactured by a well-known method. For example, a C2-C4 alkylene oxide such as ethylene oxide, propylene oxide, tetrahydrofuran, etc. is sequentially added to a C6-C14 dihydric alcohol (alkanediol or the like) in the presence of a base such as sodium hydroxide or potassium hydroxide. It can synthesize | combine by addition reaction.

The amount of the surfactant used is usually 0.1 to 10% by weight, preferably 0.2 to 8% by weight, more preferably 0.5 to 7% by weight in the mixture before kneading with water. to be.

In the present invention, it is preferable to use condensed phosphoric acid or a salt thereof to supplement the function of the surfactant as a dispersant.

Condensed phosphoric acid means linear polymeric phosphoric acid produced by dehydration condensation of orthophosphoric acid.

H _{n + 2} P _n O _{3n + 1} (n = 2, 3, 4…)

Represented by Specifically, they are polyphosphoric acid, such as diphosphoric acid (pyrophosphoric acid), triphosphoric acid (tripolyphosphoric acid), and tetraphosphoric acid. Moreover, as a salt of condensed phosphoric acid, Alkali metal salts, such as a sodium salt and potassium salt; Alkaline earth metal salts such as calcium salts and magnesium salts; Ammonium salt etc. are mentioned. As condensed phosphoric acid or its salt, especially tripolyphosphoric-acid alkali metal salts, such as sodium tripolyphosphate, are preferable. When condensed phosphoric acid or salts thereof are used, the amount thereof is usually 0.1 to 10% by weight, preferably 0.2 to 8% by weight, more preferably 0.5 to 7% in the mixture before kneading with water. It is about 2 weight%-about 6 weight% more preferably.

In the present invention, a polycarboxylic acid-based surfactant. It is preferable to use a combination of nonionic surfactants such as polyoxyethylene acetylenediol, condensed phosphoric acid or salts thereof, and the total amount thereof is usually 1% by weight to 30% by weight, preferably in a mixture before kneading with water. It is about 3 to 20 weight%, More preferably, it is about 5 to 15 weight%.

In the present invention, examples of the binder include cellulose derivatives such as salts of carboxymethyl cellulose (sodium salt and the like), polyvinyl alcohol or derivatives thereof, and water-soluble polymers such as sodium alginate, xanthan gum and gum arabic. Among these, cellulose derivatives, such as the sodium salt of carboxymethylcellulose, are preferable. The amount of the binder to be used is usually 0.1 to 10% by weight, preferably 0.2 to 8% by weight, more preferably about 1 to 8% by weight in the mixture before kneading with water.

In the present invention, the amount of calcium carbonate used is usually 30% by weight to 90% by weight, preferably 40% by weight to 80% by weight, more preferably 50% by weight to 75% by weight in the mixture before kneading with water. . Moreover, the usage-amount of calcium carbonate is 15 times-30 times, preferably 20 times-30 times of the usage-amount of a plastic micro hollow body by weight.

In the present invention, an extender may be further used in addition to calcium carbonate, and the extender may be water-soluble, such as an organic acid (citric acid, succinic acid, maleic acid, etc.) or salts thereof, urea, and saccharides (lactose, glucose, sucrose, etc.). Medium, vegetable powders (e.g. soy flour, tobacco powder, wheat flour, wood flour, etc.), mineral powders or mineral powders (e.g. kaolin, bentonite, acidic clay, clays, etc. clay, talc, feldspar, tark, diatomaceous earth, mica, Silica, alumina, sulfur, activated carbon, potassium chloride, ammonium sulfate, sodium hydrogen carbonate, sodium sulfate, magnesium carbonate and the like). Among these, bentonite is especially preferable.

In the present invention, both calcium carbonate and other extenders have a particle size of usually 1 µm to 50 µm, preferably 5 µm to 30 µm.

The total amount of extender used is usually 60% by weight to 90% by weight, preferably 65% by weight to 85% by weight in the mixture before kneading with water.

In the present invention, in addition to the above-described components, other additives such as preservatives, granulation enhancers, disintegrants, dispersants, emulsifiers, solvents, stabilizers, coloring agents, and the like may be added as necessary.

In the kneading step, a mixture containing an agricultural active ingredient, a plastic microhollower, a surfactant, a binder, calcium carbonate, which may contain bentonite and / or a condensed phosphate, and the like is kneaded with water. Here, the content of water in the composition obtained by kneading is 15% by weight to 25% by weight, the content of calcium carbonate in the mixture before kneading with water is 30% by weight to 90% by weight, and the amount of calcium carbonate is a plastic micro hollow body It is the ratio of 15-30 weight part with respect to 1 weight part.

The content of water in the composition obtained by kneading means the total amount of water contained in each component and water added in the kneading step. When there is little content of water, the water floating property of the pesticide preparation obtained will fall, and the granulation property at the time of granulation will fall. On the other hand, when there is much content of water, the problem which the granulated materials extruded from the screen adhere | attaches at the time of granulation arises, and it becomes difficult to obtain uniform kneaded material well.

Kneading can be performed using a conventional kneading apparatus, such as a stirring mixer, for example, a vertical granulator. The kneading apparatus may be added for each component, but it is preferable that the solid component is added to the kneading apparatus in advance and mixed, and the liquid component containing water is added and kneaded therein.

In the granulation step, the composition obtained by the kneading step is extrusion granulated. Extrusion granulation can be performed using a conventional extrusion granulator, for example, an extrusion granulator equipped with a screen. The extruded kneaded material is cut into suitable lengths. The screen length of the screen is usually 0.3 mm to 10 mm, preferably about 0.5 mm to 3 mm. The particle length of the extrusion granules is usually 0.5 mm to 10 mm, preferably about 2 to 5 mm.

In a drying process, a granulated material is dried. Although the granulated material obtained at the said granulation process may be provided as it is to a drying process, after granulating as needed, you may provide to the drying process.

Drying can be performed using normal drying means, such as a fluidized bed drier. You may dry under reduced pressure. The water content in the pesticide preparation obtained by drying is 0.1 weight%-2 weight% normally. After the drying step, it may be further filtered through a sieve or the like.

The pesticide granules obtained in this way are excellent in sleep floating property and diffusibility, and are particularly suitable for paddy field pesticides for rice fields. This pesticide preparation is the same as a conventional pesticide preparation, and can be sprayed by usual methods, such as manual spraying and mechanical spraying. It can also be sprayed from dung.

Said pesticide preparation can also be used as the pesticide preparation enclosed in the water-soluble film and packaged.

The water-soluble film is a film which is dissolved or dispersed in water, for example, polyvinyl alcohol or a derivative thereof, pullulan, a salt of carboxymethyl cellulose (sodium salt, etc.), a film formed from a water-soluble cellulose derivative, polyethylene oxide or a derivative thereof, or A sheet is mentioned. Among them, films or sheets molded from polyvinyl alcohol or derivatives thereof are preferable.

As a method of encapsulating the pesticide filler into a water-soluble film, conventional methods such as packaging the pesticide filler with a water-soluble film and filling the pesticide filler into a bag of the water-soluble film can be adopted. Typically, 5 g to 100 g of pesticide granules are packed per package.

The packaged pesticide preparation thus obtained is also suitable for use as paddy pesticides, and particularly suitable for being thrown into paddy fields in dung and the like.

EXAMPLES Hereinafter, although an Example demonstrates this invention still in detail, this invention is not limited by these Examples.

It is the same as the material used in the Example and the comparative example.

(Pesticide active ingredient: see the formula below)

Compound A: Imazosefuron (water solubility 0.31 mg / ml (pH7))

Compound B: 1- (2-chloro-6-n-propylimidazo [1, 2-b] pyridazin-3-ylsulfonyl) -3- (4,6-dimethoxypyrimidin-2-yl Urea (water solubility 0.15 mg / ml (pH7))

Compound C: Carfenstrol (water solubility O.OO25 mg / ml (pH7))

Compound D: benzobicycline (water solubility 0.000052 mg / ml (pH 7))

(Surfactants)

Polyoxyethylene acetylene diol (brand name "olfin E1010", product made by Nisshin Chemical Co., Ltd.)

Sodium polyacrylate (trade name "Toxanone GR-31A", manufactured by Sanyo Kasei Co., Ltd.)

(Binder)

Carboxymethyl cellulose sodium (brand name "Cellogen 7A", Dai-ichi Kogyo Pharmaceutical Co., Ltd. product)

(Plastic micro hollow body)

`` Micro spare F-80E '' (content: 15 wt%, moisture: 85 wt%), manufactured by Matsumoto Yuji Pharmaceutical Co., Ltd.

(extender)

Calcium carbonate (brand name "Tohoku tankal (# 250)", product made by Towa lime industry company)] Bentonite (brand name "Kunigel V1", product made by Kunimine industry)

(etc)

Sodium tripolyphosphate

Examples 1-5, Comparative Examples 1-6

In a ratio shown in Table 1 below, a pesticide active ingredient, sodium tripolyphosphate, a binder, a plastic microhollower, and an extender were mixed for 2 minutes using a vertical granulator (VG-25 type, manufactured by Faurek), and then a predetermined amount. The mixed solution of water, olpin E1010 and toxanone GR-31A was added and kneaded with a vertical granulator. The resulting kneaded product was assembled by a basket granulator (diameter 200 mm, screen length 1.5 mm, manufactured by Fuji Powder Co., Ltd.), and the granulated material was erected until the particle length became about 3 mm by hand. The particle | grains obtained by drying at 60 degreeC by the electric industry company were hanged on the sieve (2000 micrometer pass, 850 micrometer pass | through), and the pesticide granule was obtained.

In addition, "weight ratio" in Table 1 is a value of (weight part of calcium carbonate / weight part of a plastic micro hollow body), and "total amount of water (weight%)" is the water added for kneading | mixing, and the added micro spare F-80E. It is a ratio with respect to the whole composition obtained by kneading of the total amount of water contained. In addition, the weight% of calcium carbonate is the content rate of calcium carbonate in the mixture before kneading with water.

Evaluation test

About each pesticide granule obtained in the Example and the comparative example, granulation property, sleep levitation, and the diffusibility of particle | grains were evaluated. In addition, the water content (% by weight) in the pesticide preparation was measured. The results are shown in Table 1. In Comparative Example 5, since the granulated material which could be used for the test of the surface floating property and the particle diffusivity could not be obtained, the surface floating property and the particle diffusing property were not tested.

(Assembly)

The following criteria were evaluated about the granularity at the time of granulation.

(Double-circle): The granulated material formed in columnar shape is rapidly extruded from a screen, and there is almost no adhesion of kneaded materials.

(Circle): Although the granulated material is extruded smoothly from a screen, the part which a thin part splits is seen in a part of granulated material. There is almost no adhesion between kneaded materials.

(Triangle | delta): Extrusion from the screen of a granulated material is not smooth, and the tip part is seen in the most part of granulated material. There is almost no adhesion between kneaded materials.

X: The adhesion of the granulated materials extruded from the screen is remarkable.

(Suspension of sleep)

300 mL of 3 degree hard water of 20 degreeC is put into a 300 mL beaker, 0.5 g of each granules obtained above are put into it, and the number of the particles which settle in a few seconds is counted. This test is carried out five times to calculate the total particle number.

(Diffusion of particles)

Each granule 40g obtained above was packaged with the water-soluble film (brand name "Kuraray vinylon film VF-HP4000", the product made by Kuraray Co., Ltd.), and each packaged pesticide preparation (water-soluble pack) was obtained. This was dropped into a rice field of 1a containing water of 5 cm depth at room temperature. The diffusivity of the particles was evaluated based on the following criteria.

(Double-circle): The particle | grains disperse | distribute uniformly throughout the paddy field within 30 minutes after particle | grains start release | release from a water-soluble film.

(Circle): after particle starts to discharge | release from a water-soluble film, particle | grains disperse | distribute uniformly over the paddy field for more than 30 minutes but less than 1 hour.

(Triangle | delta): After particle | grains start to discharge | release from a water-soluble film, bonding of particle | grains arises and it takes time more than 1 hour to disperse | distribute uniformly throughout the paddy field.

X: Since the bonding of particles is remarkable, kernels are not uniformly dispersed throughout the paddy field.

(Measurement of Water Content)

The water content of each particle was measured by the following measuring apparatus and measurement conditions.

Measuring instrument: Infrared moisture meter `` FD-610 '' (Ket Science Research Institute)

Measured sample amount: about 5 grams

Measurement condition: drying loss method by heating at 60 ° C. for 10 minutes

According to the production method of the present invention, by adjusting the amount of water and calcium carbonate used in a specific range, there is no problem in the surface-floating agrochemical pesticide excellent in basic performance such as floating property and diffusivity in water surface, etc. Industrially, it can manufacture smoothly efficiently. In addition, it is possible to industrially and efficiently produce a pouch-type pesticide preparation for paddy processing in which this pesticide granule having excellent basic performance such as floating property on the water surface and diffusivity is contained in a water-soluble film.

Claims (7)

A method of producing a pesticide granule for kneading, extruding, and drying the granulated product by kneading a mixture comprising an agrochemical active ingredient, a plastic microhollow, a surfactant, a binder, and calcium carbonate, and the content of water in the composition obtained by kneading. It is 15 to 25 weight%, content of calcium carbonate in the mixture before kneading with water is 30 to 90 weight%, and the quantity of calcium carbonate is 15 to 30 weight weight with respect to 1 weight part of plastic micro hollow bodies. The manufacturing method of the pesticide preparation of a negative ratio. The method for producing a pesticide preparation according to claim 1, wherein the water content of the pesticide preparation is dried so as to be 0.1 wt% to 2 wt%. The pesticide preparation method of Claim 1 or 2 whose surfactant is a polycarboxylic-acid type surfactant. The method for producing agrochemical granules according to claim 1 or 2, wherein the binder is sodium carboxymethylcellulose. In a composition obtained by kneading, a mixture comprising a pesticide active ingredient, a plastic microhollow, a surfactant, a binder, calcium carbonate and bentonite is kneaded with water, extrusion granulated, and the granulated material is dried. The water content is 15% by weight to 25% by weight, the content of calcium carbonate in the mixture before kneading with water is 30% by weight to 90% by weight, and the amount of calcium carbonate is 15% by weight of 1 part by weight of the plastic microhollow. The manufacturing method of the pesticide preparation which is the ratio of -30 weight part. Pesticide active ingredient, plastic micro hollow body, surfactant. A method for producing a pesticide preparation comprising kneading a mixture comprising condensed phosphate, a binder, calcium carbonate and bentonite with water, extruding and drying the granulated product, wherein the content of water in the composition obtained by kneading is 15% by weight to 25% by weight. %, The content of calcium carbonate in the mixture before kneading with water is 30% by weight to 90% by weight, and the amount of calcium carbonate is 15-30 parts by weight with respect to 1 part by weight of the plastic microhollows. Way. A method for producing a packaged pesticide preparation, which encapsulates the pesticide preparation obtained in the method of claim 1 in a water-soluble film.