KR100766754B1 - Floating solid pesticide preparations - Google Patents

Abstract

The present invention relates to a sleep-floating pesticide solid preparation containing one or two or more sleep expanding agents and pesticide active ingredients selected from C ₂ to C ₄ alkylene oxide adducts and derivatives thereof of C ₄ to C ₁₀ alkyl alcohols. will be.

Description

Sleep-Floating Pesticide Solids {FLOATING SOLID PESTICIDE PREPARATIONS}

The present invention relates to a sleep-floating pesticide solid preparation containing one or two or more sleep expanding agents and pesticide active ingredients selected from C ₂ to C ₄ alkylene oxide adducts and derivatives thereof of C ₄ to C ₁₀ alkyl alcohols. The present invention relates to a pesticide preparation for rice paddy divided into a pack of water-soluble films and a method for controlling harmful organisms generated in rice paddies using the same.

Conventionally, pesticides used in paddy fields have been formulated in various formulations, such as powders, hydrating agents, milk agents and granules, for the convenience of their use, and have been spread over water or rice. However, in recent years, for example, in view of the aging of farmers, the diversification of labor, and the increase in the labor burden of women, the labor force savings of pesticide dispersion have been required.

As a result, a lot of flooring agents which can be processed without using a machine, or so-called 1 kg granules, which increase the amount of the active ingredient in the formulation and reduce the amount of dispersion as the formulation, are used. However, the floorables have problems such as flying to the sprayer at the time of treatment depending on the wind direction and the problem of empty bottle treatment, and the 1kg granules have disadvantages such as the need for a spray mechanism and uniform dispersion, for example.

Recently, a labor-saving pesticide formulation (ie, a pesticide formulation for non-feeding) that can be processed by dividing the solid preparation of pesticides into a pack of water-soluble films and throwing the pack out of the rice paddies without being put into the paddy field has been proposed (Japan Japanese Patent Laid-Open No. 3-173802), which is commercialized, and these are also called jumbo or pack agents.

Such non-feeding preparations include, for example, 1) large-sized expanded tablets as they are put into the paddy field (JP-A 6-107503), 2) small-sized expanded tablets in a pack of water-soluble film, and put into the paddy fields. (Japanese Patent Application Laid-Open No. 5-339106), (3) A water-soluble carrier such as potassium chloride is assembled with a water-soluble film-forming polymer, containing the active ingredient of a pesticide, divided into a pack of water-soluble film, and put into a rice paddy. (Japanese Patent Application Laid-open No. Hei 5-78207), ④ Pour a pesticide solid preparation prepared to be suspended on the water in a pack of water-soluble films, and put it into rice paddies (Japanese Patent Laid-Open No. 6-336403) and ⑤ It is known to fill a water-soluble container with oil having sleep stability and put it into rice paddies (Japanese Patent Laid-Open No. 5-339103).

Such a pesticide preparation for non-injection has a high content of the pesticide active ingredient in the formulation and is applied locally, so if the active ingredient does not diffuse rapidly at the point where it is injected, the effect of weakness or effect due to unevenness of the pesticide active ingredient Non-uniformity tends to occur, and in some cases, there is a concern that the remaining crops may be affected by the residual of the active ingredient of the pesticide.

On the other hand, as a pesticide solid preparation formulated to proliferate on the surface of the water for the purpose of spreading the active ingredient of pesticides, for example, (1) floating with a water-soluble carrier (Japanese Patent Publication No. 48-15613, Japanese Patent Publication 47-1240), (2) using pumice or vermiculite having specific absorption capacity (Japanese Patent Publication No. 44-8600), (3) Granules using volatile insecticide compounds (Japanese Patent Publication No. 49-11421) ), (4) A carbamate-based pesticide active ingredient and an organic compound having a distribution coefficient of 10 ² or more fixed to a solid carrier (Japanese Patent Laid-Open No. 2-174702), and (5) fungicides A composition comprising an active ingredient, a solid carrier and an oil that is a herbicide or a plant growth regulator (JP-A-3-193705) is disclosed.

However, when these pesticide solid preparations are treated under conditions where the rice is small and there are no obstacles such as bucho, algae and oil film on the surface of the water, the particles spread widely on the surface with the help of the wind, so they do not enter the rice fields and are scattered on the rice fields. The so-called edge scattering, however, has a high effect, but when the rice grows and becomes unable to use the force of the wind, or when it is treated in the presence of obstacles such as bucho, algae, and oil film on the surface, the particles are less likely to spread by magnetic force. In some cases, a sufficient biological effect cannot be exhibited, or a weakness may occur due to the local presence of the active ingredient. In such a case, since it is necessary to enter and distribute rice fields like conventional granules, it is not preferable from the point of reducing labor.

In order to solve these drawbacks, an acetylene-based surfactant is used as a sleep expanding agent, and an attempt is made to divide it into a pack of water-soluble film having a sleep expansion, or a silicone-based, fluorine-based surfactant, or dialkyl sulfosuccinate as a sleep expanding agent. Attempts have been made to use sinates (Japanese Patent Laid-Open No. 6-336403, Japanese Patent Laid-Open No. 8-99802, and Japanese Patent Laid-Open No. 2766973). However, even with such a technique, sufficient diffusion may not be expected in the conditions where obstacles exist in the above water surface and in the treatment after rice is grown.

The present inventors, the surface accuracy is superior conductive surface suspended agrochemicals a result of extensive studies for solid preparations, of C ₄ ~C ₁₀ alkyl, C ₂ ~C ₄ alcohol alkylene oxide adducts, and one or two or more selected from the derivatives The present invention has been completed by finding that the surface-floating pesticide solid preparation containing the sleep expanding agent exhibits excellent sleep integrity even in the treatment of rice paddies with obstacles in the surface of the water and after the rice is grown.

The present invention relates to a sleep-floating pesticide solid preparation containing one or two or more sleep expanding agents and pesticide active ingredients selected from C ₂ to C ₄ alkylene oxide adducts and derivatives thereof of C ₄ to C ₁₀ alkyl alcohols. The present invention provides a pesticide preparation for paddy feeding in water-soluble films and a method for controlling harmful organisms generated in paddy fields using them.

In the present invention, "C ₄ -C ₁₀ alkyl alcohol" is a straight or branched chain alcohol having 4 to 10 carbon atoms, for example, butanol, pentanol, hexanol, heptanol, octanol, nonanol, isononanol, Decanol or ethylhexanol, preferably a straight or branched alcohol having 6 to 10 carbon atoms, more preferably octanol, ethylhexanol or isononanol, still more preferably ethylhexanol Isononanol.

In the present invention, "C ₂ -C ₄ alkylene oxide" is a linear or branched alkylene oxide of 2 to 4 carbon atoms, for example, may be ethylene oxide, propylene oxide or butylene oxide, preferably ethylene oxide Or propylene oxide.

In the present invention, the "C ₄ ~C ₁₀ alkyl alcohol C ₂ ~C ₄ alkylene oxide adduct" is, the "C ₄ ~C ₁₀ alkyl alcohol" to the hydroxy group of the "C ₂ ~C ₄ alkylene oxides." In addition, when adding several alkylene oxide, the order of addition is arbitrary.

"C ₄ ~C ₁₀ alkyl alcohol of C ₂ ~C ₄ alkylene oxide addition product" in the present invention, preferably the following general formula (I):

R ¹ O- (AO) _m- (BO) _n -H

[Wherein, R ¹ represents a C ₄ to C ₁₀ alkyl group, A represents a group represented by the formula -CH ₂ -CH _2- , B represents a group represented by the formula -CH ₂ -CH (CH ₃ )-, m represents 0-30, n represents 0-30, provided m and n are not 0 at the same time, when n is 0, m is 2 or more, and when m and n are not all 0, m AO The order in which the groups and the n BO groups combine is arbitrary]

It is a compound represented by.

In the above formula, "m" and "n" represent the number of ethylene oxide and propylene oxide added to one compound (I), respectively, and the number of ethylene oxide and propylene oxide added to the plurality of compounds (I). It is also possible to represent the average of.

In the present invention, "C ₄ ~C ₁₀ alkyl alcohol of C ₂ ~C ₄ alkylene oxide adduct derivative" is, for example, the "C ₄ ~C ₁₀ alkyl alcohol of C ₂ ~C ₄ alkylene oxide adduct" phosphate Esters, salts of phosphate esters, sulfate esters, salts of sulfate esters or C ₁ -C ₁₀ alkyl ethers, preferably phosphoric acid esters or salts thereof.

"Phosphate ester" in this invention contains all the monoester, diester, and triester, Preferably it is a mixture thereof.

In the present invention, the "salt" is not particularly limited as long as it is usually used as a pesticide, for example, alkali metal salts such as sodium salts, potassium salts and lithium salts; Amine salts such as ammonium salts, triethanolamine salts and isopropylamine salts; Or alkaline earth metal salts such as calcium and barium salts, preferably ammonium salts or alkali metal salts, and more preferably ammonium salts, sodium salts or potassium salts.

"C ₁ ~C ₁₀ alkyl ether" in the present invention, wherein the oxygen atoms of the terminal hydroxyl group of the "C ₄ ~C ₁₀ alkyl alcohol of C ₂ ~C ₄ alkylene oxide adducts", having from 1 to 10 linear Or branched chain alkyl groups, for example methyl ether, ethyl ether, propyl ether, isopropyl ether, butyl ether, pentyl ether, hexyl ether, heptyl ether, octyl ether, ethylhexyl ether, nonyl ether, isononyl ether or decyl Ether, preferably ethylhexyl or isononylether.

The "C ₂ -C ₄ alkylene oxide adduct of C ₄ -C ₁₀ alkyl alcohol" of the present invention is more preferably the compound (Ia) represented by the following in the compound (I):

R ¹ is a C ₆ -C ₁₀ alkyl group (more preferably an octyl, ethylhexyl or isononyl group, still more preferably an ethylhexyl or isononyl group),

A is a group represented by the formula -CH ₂ -CH _2- ,

B is a group represented by the formula -CH ₂ -CH (CH ₃ )-,

When m is 0-15 (more preferably 0-10), n is 0-15 (more preferably 0-10), provided that m and n are not 0 at the same time and n is 0, m is 2 As mentioned above, when m and n are not all 0, the order which m AO groups and n BO groups combine is arbitrary.

The sleep expanding agent of the present invention is particularly preferably in the compound (I), wherein R ¹ is an ethylhexyl or isononyl group, m is 0 to 10, n is 0 to 10, provided that m and n Is not 0 at the same time and when n is 0, m is two or more compounds (Ib), its phosphate ester or its ammonium salt, sodium salt or potassium salt, most preferably in the compound (I), R ¹ It is an ethylhexyl or isononyl group, m is 2-8, n is 0-8, The compound (Ic), its phosphate ester, or the sodium salt of this phosphate ester.

The sleep expanding agent of the present invention can be used as it is, and even if it is not commercially available, it can be produced according to the method described in, for example, a new surfactant (Horiguchi Hiroshi, Sankyo Publishing, 50 years of digestion). have.

The amount of the water spreading agent to be used is usually 0.1 to 50% by mass, preferably 0.5 to 30% by mass, and more preferably 1 to 20% by mass in the agrochemical solid preparation.

The active ingredient of the pesticide in the present invention is not particularly limited as long as it is a pesticide capable of sleeping treatment, and may be a liquid or a solid, for example, an insecticide, a fungicide, a herbicide or a plant regulator.

Pesticides used are, for example, isoxathione, diazinone, disulfotone, propaphos, trichlorphone, formothione, dimethoate, monoclotophosphate, acetate, carbofuran, carbosulfane, thioxik Infiltrating insecticides such as ram, carptop, bensultop, benfuracarb, furathiocarb, bupropezin, phenobucarb, metholcarb, propoxya, imidacloprid, nitenpyram and acetamiprid; Or synthetic pyrethroids effective for insects that live in or near water, such as rice water weevil or rice leaf beetle, such as cycloprotrin, etofenprox and silafluorophene. And preferably imidacloprid, nitenpyram, acetamiprid, cycloprotrin, etofenprox or silafluorophene.

The fungicides used are, for example, probenazole, isoprothiolane, isprobenfos, tricyclazole, pyroquilon, carpropamide, oribright, azoxystrobin and 7-fluoro-1,2,5,6- Thermal diseases such as tetrahydro-4H-pyrrolo [3.2.1-ij] quinolin-4-one; Flutolanyl, mepronyl, tifluzamide, furamepyr and 2- (4-fluorophenyl) -1- (1H- 1,2,4-triazol-1-yl) -3-trimethylsilyl Leaf blight blight agents such as propan-2-ol; Teclophthalam; Or benomyl, preferably propenazole, isoprothiolane, pyroquilon, carpropamide, oribright, azoxystrobin, 7-fluoro-1,2,5,6-tetrahydro-4H- Pyrrolo [3.2.1-ij] quinolin-4-one, flutolanyl, tifluzamide, furamepyr, 2- (4-fluorophenyl) -1- (1H-1,2,4-tria Zol-1-yl) -3-trimethylsilyl-propan-2-ol or teclophthalam.

Herbicides used are, for example, pyrazolates, benzophenads, pyrazoxifenes, pyributycarbs, bromobutides, butamifos, mefenacet, bensulfuron-methyl, anilofos, butachlor, pretilachlor , Thiobencarb, chlornitropen, clomethoxyphene, dimuron, biphenox, naproanilide, oxadione, oxadiargyl, ventazone, molinate, piperophosph, dimepiperate, espro Salts such as carb, dithiopyr, imazosulfuron, benfuresate, quinoclamine, cinnamethylline, MCPA or its sodium salt, potassium salt or esters of MCPA, 2,4-D or its sodium salt, Salts such as potassium salt or esters of 2,4-D, MCPB or its sodium salt, salts such as potassium salt or esters of MCPB, quinclolac, pyrazosulfuronethyl, pentoxazone, tenylchlor, cumyluron, Cynosulfuron, cymetrine, dimethamethrin, sihalopopbutyl, eto Zanide, carfenstrol, ethoxysulfuron, azimsulfuron, cyclosulfamuron, indanophane, pyriminobacmethyl, oxazilomepon, 4- (2-chlorophenyl) -N-cyclohexyl-4,5- Dihydro-N-ethyl-5-oxo-1H-tetrazol-1-carboxyamide (pentrazamide, NBA061), [3- (2-chloro-4-methylsulfonylbenzoyl) -4-phenylthio] ratio Cyclo [3.2.1] oct-3-en-2-one (benzobicyclo, SB500), methyl = N- [4- (benzothiazol-2-ylmethoxy) -2-methyl phenyl] carbamate and Non herbicides such as methyl = N- [4- (benzooxazol-2-ylmethoxy) -2-methylphenyl] carbamate, preferably pyrazolate, benzophene, pyrazoxifene, pyributy Carb, Bromobutide, Mefenacet, Bensulfuron-methyl, Anilophos, Butachlor, Pretilachlor, Dimuron, Oxadiagil, Imazulfuron, Pirazosulfuron-ethyl, Pentoxazone, Tenylchlor , Dimethacrylate, sihalopopbutyl, carfenstrol, ethoxy Sulfuron, azimsulfuron, indanophan, pentrazamide (NBA061), benzobicyclo, methyl N- [4- (benzothiazol-2-ylmethoxy) -2-methylphenyl] carbamate or methyl N- [ 4- (benzooxazol-2-ylmethoxy) -2-methylphenyl] carbamate.

The plant control agents used may be, for example, inabenfeed, paclobutrazole, uniconazole or triaptenenol, preferably inbenpide or paclobutrazole.

Pesticide solid preparations of the present invention, in addition to the sleep enhancer and the active ingredient pesticides, for example, sleep resuscitants, other sleep enhancers, disintegrating and dispersing agents, wetting agents, binders, extenders, granulation enhancers, solvents, emulsifiers, stabilizers and grinding aids, etc. It may contain other auxiliaries.

The pesticide solid preparation of the present invention may contain a sleeping flotation agent in order to improve sleep flotation. The sleep resuscitation agent may be one that floats a pesticide solid preparation on the surface of the water, and includes, for example, minerals such as foamed shirasu, expanded pearlite, foamed pumice and calcined vermiculite; Plant material such as cork, wood meal and cellulose; Foamed synthetic resins such as foamed styrol; Synthetic resin powders such as polyvinyl chloride powder; Plastic hollow bodies such as Matsumoto micro spare F30E; Granular material of synthetic resin; Or mixtures thereof, preferably foamed shirasu, foamed pearlite, foamed pumice, calcined vermiculite, cork, wood mill, foamed synthetic resin, synthetic resin powder or plastic hollow body.

The amount of the sleep suspension used depends on the type of the sleeping suspension used, the formulation, and the size of the pesticide solid preparation. The amount of the sleep suspension used should be sufficient to float the surface of the pesticide solid preparation, and usually 0.01 to 90% by mass in the pesticide solid preparation. It is preferably from 0.1 to 70% by mass, more preferably from 0.5 to 60% by mass.

The present invention may contain various surfactants as an adjuvant, and the surfactants used may act as other sleep expanding agents, disintegrating and dispersing agents, wetting agents, binders, granulation enhancers or emulsifiers, depending on their properties. Moreover, a polymer and an organic solvent can also be used for several objectives according to the property.

The pesticide solid preparation of the present invention may further contain another sleep expanding agent together with the above sleeping extender in order to improve sleep stability. Other sleep extenders used are sodium, potassium and ammonium salts of, for example, copolymers of styrenesulfonic acid and vinyl with (co) polymers of carboxylic acids such as acrylic acid and maleic acid, carboxylic acids such as acrylic acid and maleic acid. Polycarboxylic acid type polysorbs such as polymer salts, etc .; Soaps such as sodium oleate and potassium stearate; Other anionic surfactants such as sodium dialkylsulfosuccinate, sodium dodecylbenzenesulfonate, sodium lauryl sulfate and perfluoroalkylcarboxylates; Other nonionic surfactants such as polyoxyethylene alkylaryl ether, polyoxyethylene alkyl ether having 11 or more carbon atoms, polyoxyethylene alkyl ester and alkyl ester of sorbitan; Silicone based nonionic surfactants, acetylene based nonionic surfactants and pluronic type nonionic surfactants; Surfactants which made these nonionic surfactants the ester of phosphoric acid or sulfuric acid, and neutralized them with appropriate alkali in some cases; Fluorine-containing surfactants; Mineral oils such as liquid paraffin, naphthenic and aromatic high boiling point solvents, low viscosity polybutene and machine oil; Silicone oils; Various vegetable oils; Resins such as rosin; Camphor white milk; αpinene; camphor; Or naphthalene, preferably an acetylene-based nonionic surfactant or various mineral oils.

The amount of other sleep enhancers used depends on the type and amount of the sleep extender and the method of addition, the type or amount of active pesticide active ingredient or sleep suspension, and the type or amount of other supplements. It is 0.01-50 mass% in the inside, Preferably it is 0.1-40 mass%, More preferably, it is 0.2-30 mass%.

The pesticide solid preparation of the present invention may contain a disintegrating and dispersing agent in order to disintegrate the particles in water and to suspend and disperse the pesticide active ingredient in water. The disintegrating and dispersing agents used are often anionic surfactants, for example, lignin sulfonates, (alkyl) naphthalene sulfonates and their condensates, phenol sulfonates and their condensates, condensates of styrene sulfonates, maleic acid and styrene sulfonic acids Salts of condensates, salts of carboxylic acid condensates such as acrylic acid and maleic acid, polyacrylates, salts of acrylic acid and maleic acid copolymers, salts of maleic anhydride and methylvinyl ether copolymers, alkylbenzenesulfonates, dialkylsulfosuccinic acids Salts, salts of lauryl sulfate, polyoxyethylene alkyl aryl ether sulfate, polyoxyethylene aryl aryl ether sulfate, polyoxyethylene alkyl aryl ether phosphate ester, polyoxyethylene aryl aryl ether phosphate ester or these sulfate esters or phosphoric acid Anionic surfactants, such as salts which neutralized the ester with a suitable cation, are preferably ligated Ninsulfonate, condensates of (alkyl) naphthalenesulfonates, condensates of phenolsulfonates, condensates of styrenesulfonates, salts of condensates of maleic acid and styrenesulfonic acids, salts of carboxylic acid condensates such as acrylic acid and maleic acid, polyacrylates Acid salts, salts of acrylic acid and maleic acid copolymers, salts of maleic anhydride and methylvinyl ether copolymers or dialkylsulfosuccinate salts. Surfactants used in these disintegrating and dispersing agents are often effective as wetting agents. Moreover, phosphate, such as sodium phosphate and sodium hexametaphosphate; Suitable among nonionic, cationic or amphoteric surfactants; And starch, carboxymethylcellulose, carboxymethylated starch, and salts thereof, crosslinked products of polyvinylpyrrolidone, microcrystalline cellulose and superabsorbent resins and the like that have the property of absorbing and expanding water can be used as disintegrating and dispersing agents. .

The amount of the disintegrating and dispersing agent or the disintegrating and dispersing agent and the wetting agent to be used is usually from 0.01 to 30% by mass, preferably from 0.03 to 20% by mass, more preferably from 0.05 to 10% by mass in the agrochemical solid preparation.

The pesticide solid preparation of the present invention may contain a binder for imparting hardness to the particles or for coating the surface of the particle nucleus with the active ingredient in the case of granulating the powder raw material to prepare granules.

The binder used for the former purpose includes water-soluble starch derivatives such as relatively low molecular weight dextrin and α-ized starch; Water-soluble polymer materials such as polyvinylpyrrolidone, salts of polyacrylic acid, salts of carboxymethylcellulose, polyvinyl alcohols having a relatively low molecular weight and low saponification rate, salts of lignin sulfonic acid and gum arabic; Or montmorillonite-based mineral fine powder such as bentonite.                 

The amount of the binder to be used for the former purpose depends, for example, on the formulation composition, the granulation method, and the size of the particles, but is usually 0.1 to 30% by mass, preferably 0.5 to 20% by mass, in the agrochemical solid preparation.

The binder used for the latter purpose may be, in addition to the solid binder, an oily binder which is difficult to volatilize. In the present invention, by dissolving these binders in a solvent such as water or a volatile organic solvent, the pesticide active ingredient may be coated on the surface of the particle nucleus, and then the solvent may be evaporated. And may be left in the pesticide solids without evaporating the binder. The method of leaving the binder in the pesticide solid preparation is an advantageous method since the drying step can be omitted.

In the case of coating and evaporating the binder, the amount of the binder used is preferably smaller in consideration of economical efficiency, and is usually 0.01 to 20% by mass, preferably 0.1 to 10% by mass, more preferably in agrochemical solids. It is 0.2-5 mass%. Water is preferable as the solvent for dissolving the binder.

The binder used in the case of leaving the binder in the pesticide solid preparation should be one capable of uniformly coating the pesticide active ingredient on the surface of the particle nucleus, and the pesticide active ingredient should be in an oil state which does not adversely affect, for example, particle growth and decomposition. Preferably, for example, a solvent having high boiling point, low toxicity, low flammability and low viscosity, and having a specific gravity of less than 1 and difficult to dissolve the active ingredient of agrochemicals is preferable. Such binders include, for example, mineral oils such as low viscosity liquid paraffin, chlorinated paraffin, isoparaffin, machine oil, polybutene, paraffinic, naphthenic and aromatic high boiling solvents; Vegetable oils such as palm oil, soybean oil, and rapeseed oil; Animal oils such as whale oil and sardine oil; Silicone oils and derivatives thereof; Plasticizers such as esters of monocarboxylic acids such as oleic acid and palm oil fatty acids, esters of dicarboxylic acids such as maleic acid, fumaric acid, phthalic acid and adipic acid, and phosphoric acid esters such as tributylphosphate and triethylphosphate; Glycols such as ethylene glycol, diethylene glycol, polyethylene glycol, propylene glycol, butanediol and hexylene glycol; lactones such as ε-caprolactone and γ-butyrolactone; N-alkylpyrrolidone; Various liquid surfactants; Or mixtures thereof, preferably relatively inexpensive and not adversely affecting the active ingredient, the binder itself being stable and having low volatility, more preferably mineral oils such as liquid paraffin, machine oil and polybutene, mono Carboxylic acid ester or dicarboxylic acid ester.

The amount of binder used when leaving the binder in the pesticide solid preparation varies depending on the type of binder, the type or physical properties of the active ingredient of the pesticide, and the type or amount of the other auxiliary agent, which is usually 1 to 50% by mass in the pesticide solid preparation, Preferably it is 3-40 mass%, More preferably, it is 5-35 mass%.

The extender used in the pesticide solid preparation of the present invention is not particularly limited as long as it is generally used as a carrier of the pesticide, and includes, for example, minerals such as clay, calcium carbonate, diatomaceous earth, amorphous silicon dioxide and talc; Or vegetable powders such as starch, wood mill, sawdust, coffee bean powder, tabuk powder (Makko (Machilus thunbergii) base powder), cellulose powder, microcrystalline cellulose, chaff powder, rice bran, bran and palm husk powder, Preferably amorphous silicon dioxide, talc or wood mill.

The amount of extender used varies depending on the type and amount of other auxiliaries, but is usually 0.1 to 80% by mass, preferably 1 to 50% by mass, and more preferably 2 to 40% by mass in the agrochemical solid preparation.

The pesticide solid preparation of the present invention may contain a cohesiveness improving agent in order to improve the cohesiveness of the pesticide granules. The coarse enhancer to be used is not particularly limited as long as it imparts plasticity to the surfactant or composition generally used as coarse enhancer in agrochemical granules, and for example, polyoxyethylene alkylaryl ether, polyoxyethylene alkyl ester and polyoxyethylene Nonionic surfactants such as arylaryl ethers; Anionic surfactants such as sodium salt of dialkylsulfosuccinate and sodium salt of alkylbenzenesulfonic acid; Mineral fines such as bentonite; Starch derivatives such as dextrin and α-ized starch; Natural rubber such as arabic rubber; Cellulose derivatives such as sodium salt of carboxymethylcellulose; Or a water-soluble synthetic polymer such as sodium salt of polyvinyl alcohol or polyacrylic acid, and preferably sodium salt of bentonite or carboxymethylcellulose.

The amount of the granularity improving agent to be used varies depending on the type of granularity improving agent and the type and amount of other auxiliary agents, but is usually 0.01 to 30% by mass, preferably 0.05 to 25% by mass, more preferably in agrochemical solids. 0.1-20 mass%.

The pesticide solid preparation of the present invention may contain a solvent in order to dilute the liquid pesticide active ingredient or to make a low melting point pesticide active ingredient into a liquid phase. The solvents used for this purpose are high boiling point, low toxicity and high flash point.When the specific gravity of the pesticide active ingredient is 1 or more, the specific gravity is less than 1 and low viscosity to keep the emulsified particles in water for as long as possible and to spread widely in rice fields. Phosphorus solvents are preferable, for example, paraffinic, aromatic and naphthenic high boiling point solvents; Esters such as fatty acids, phthalic acid, adipic acid and phosphoric acid obtained from various animals and plants such as oleic acid, maleic acid, fumaric acid and palm oil; Vegetable oils such as palm oil and rapeseed oil; Or animal oils such as whale oil and sardine oil. Preferably, they are liquid paraffin or low molecular weight polybutene.

The amount of solvent that dilutes or dissolves the active pesticide active ingredient varies depending on the type and physical properties of the active pesticide active ingredient.As long as possible, as long as it does not affect the stability and physical properties of the pesticide solid preparation over time, it is usually diluted or It is 0.1-50 parts with respect to 1 part of pesticide active ingredients to melt | dissolve, Preferably it is 0.2-10 parts.

In addition, C ₄ ~C ₁₀ also a C ₂ ~C _4, the alkylene oxide addition compounds to the alkyl alcohol can be used as solvent to dilute or dissolve the agricultural chemical active ingredient.

The pesticide solid preparation of the present invention may contain an emulsifier in order to emulsify the pesticide active ingredient in water, and such emulsifier may be selected according to the type or physical properties of the pesticide active ingredient or solvent, similarly to the emulsifier of the emulsion. However, unlike conventional emulsifiers, since they are not artificially stirred at the time of use of agrochemical solid preparations, the self-emulsification property is as good as possible, and fine emulsification is preferably performed.                 

The amount of the emulsifier to be used is usually 0.01 to 10 parts, preferably 0.03 to 3 parts, with respect to 1 part of the liquid to be emulsified, which consists of a liquid pesticide active ingredient or a pesticide active ingredient diluted or dissolved in a solvent.

The pesticide solid preparation of the present invention may contain a stabilizer as necessary for the stabilization of the active pesticide active ingredient or the stabilization of physical properties in the formulation. The stabilizers used may be, for example, pH adjusters, antioxidants, light stabilizers, volatilization inhibitors, solid acid activity inhibitors, pigments or drying agents.

The pesticide solid preparation of the present invention may contain a grinding aid, if necessary, in order to improve the grindability or to prevent adhesion to the device when the active ingredient is dry milled. The grinding aid used may be, for example, amorphous synthetic silica, talc or various particulate minerals and the like, preferably amorphous synthetic silica or talc.

When the pesticide active agent of the present invention is a solid pesticide active ingredient, if necessary, the powder premix obtained by pulverizing with a sleep expanding agent, disintegrating and dispersing agent, wetting agent, extender, stabilizer and grinding aid, etc. is suspended in water. It can be produced by coating the particle nucleus with an appropriate binder, and if the pesticide active ingredient is a liquid, it is dissolved in a suitable solvent as it is or as a liquid or if the pesticide active ingredient is a solid or liquid as needed. Can also be prepared by adding other auxiliaries such as a suitable disintegrating / dispersing agent, wetting agent, emulsifying agent and stabilizer and absorbing it in the particle nucleus suspended in water.

The pesticide solid preparation of the present invention can be obtained by the following method.                 

When the pesticide active ingredient of the present invention is a solid, if the particle size of the pesticide active ingredient is thick, it causes the thickening of the pesticide active ingredient at the point of rice paddy, and when the pesticide active ingredient is present locally for a long time, the effect is insufficient. Or problems may occur. Since the active ingredient of the pesticide of the present invention should be dissolved and diffused into the paddy field and water quickly after being put into the paddy field, it is effective. Therefore, even if the solubility in water is high, the fine pesticide active ingredient of the solid may be crushed to some extent. Both, and low solubility in water requires particularly fine grinding. Therefore, the active ingredient of the solid may be, if necessary, combined with the grinding aid or other auxiliary agents, for example, dry grinding by hammer mill, jet mill or the like; Or it can grind | pulverize by wet grinding by a sand mill, an attritor, etc.

The dry-pulverized pesticide active ingredient tends to be classified according to the difference in particle size or weight ratio with the sleeping floc and other auxiliary agents, and nonuniformity of the pesticide active ingredient is likely to occur in the pesticide solid preparation. In this regard, as described later, the method of kneading and assembling the slurry containing the wet-pulverized pesticide active ingredient with other auxiliaries is likely to produce nonuniformity of the pesticide active ingredient as described above. It is preferable not to do it.

The wet-pulverized pesticide active ingredient is dried and then pulverized by spray drying or the like, or absorbed into a carrier having a suitable oil absorption ability such as amorphous synthetic silica, diatomaceous earth, calcium silicate, and a super absorbent polymer, and dried and if necessary. It can be pulverized and handled in the same manner as the dry pesticide active ingredient. In addition, during wet granulation, the slurry containing the wet milled pesticide active ingredient is used together with kneaded water, whereby the pesticide granules of the present invention can be prepared by mixing and granulating.

In the case of using a liquid pesticide active ingredient, a liquid pesticide active ingredient or a low melting point pesticide active ingredient, it may be dissolved in a solvent or an emulsifier, if necessary, and absorbed into the surface-sustaining carrier or the surface-floating particle nucleus, or With other auxiliaries, such as resins, chemicals or other solid pesticide actives, which are absorbed or compatible with carriers having oil absorption such as amorphous synthetic silica, diatomaceous earth, calcium silicate, superabsorbent resins and superabsorbent dextrins A solid solution can be formed and treated in the same manner as the solid pesticide active ingredient.

These pesticide active ingredients can be made into the pesticide solid preparation of this invention through processes, such as mixing, grinding | pulverization, kneading, granulation, drying, sizing, coating, or absorption, with other adjuvant.

In the case of powder formulations, the pesticide solid preparation of the present invention may be prepared by mixing an active pesticide active ingredient, a sleep expanding agent, and other auxiliaries, if necessary, by pulverizing using a suitable mill such as a hammer mill and an air mill.

When the pesticide solid preparation of the present invention is a granule, for example, a method of assembling a raw material powder using a suitable granulator (assembly method), or a method of coating an active pesticide active ingredient with a suitable binder on a floating particle nucleus prepared in advance (coating Method) or a pesticide active ingredient in a suitable solvent, and can be manufactured by the method (absorption method) which absorbs this in the floating particle nucleus prepared previously.

In the case of producing granules by the granulation method, the agrochemical solid preparations of the present invention may be prepared as a thick preliminary mixture with other auxiliaries in advance, if necessary, and then mixed with other ingredients, and then granulated, dried and formulated. It can manufacture. The granulator to be used may be, for example, an extrusion granulator such as a lateral pressure or a basket type, a mixing granulator, an electric granulator, a fluidized bed granulator or a spray granulator, and is preferably an extrusion granulator. If the components contain foamed shirasu or foamed pearlite, pressurizing them strongly may cause the balloon to crush and buoyancy may deteriorate, and even if it contains cork, pressurizing them strongly will lower the buoyancy. It is preferable to use a granulator that is not applied.

In the case of producing the granules by the coating method, the agrochemical solid preparations of the present invention are prepared by placing the floating particle nuclei prepared in advance in a stirring mixer, adding a liquid binder as necessary to wet the surface of the granules, and then It can be prepared by adding a rich premix and stirring again to coat the pesticide active ingredient on the surface of the particle nucleus. The stirring mixer to be used is preferably a low speed mixing machine with less pulverization of particles, and may be, for example, an outer mixer, a ribbon blender, a rotary blender or a V-type mixer, and is preferably a outer mixer or a ribbon blender. In addition, in the rich preliminary mixture, for example, a sleep expanding agent, a sleeping flocculant, other sleeping expanding agents, disintegrating and dispersing agents, a wetting agent, an extender, a granularity improving agent, a solvent, an emulsifying agent or a stabilizer can be blended.

In the case of producing the granules by the absorption method, the agrochemical solid preparations of the present invention generally contain a liquid or liquefied pesticide active ingredient or a thick preliminary mixture of the above-mentioned floating particle nucleus into a stirring mixer. It can be prepared by addition and absorption. In the said preliminary mixture, a sleep expanding agent, a solvent, an emulsifier, or a stabilizer can be mix | blended as needed, for example.

In the case of producing the surface-floating granules by the coating method or the absorption method, the presence of the sleep expanding agent in the outermost layer can more effectively exert its effect. Therefore, it is preferable to add the lasting agent after coating or absorbing the active ingredient of pesticide or other auxiliary agent. As described above, in the granulation method, the coating method and the absorption method, necessary steps in the processes such as granulation, coating and absorption may be carried out at once or may be carried out in two or more stages as necessary. It may be granulated to obtain a floating particle nucleus, and the remaining pesticide active ingredient may be coated thereon, or the surface expanding agent may be coated or absorbed on the surface of the floating granules prepared by the granulation method, and the coating method and the absorption method may be applied to the same formulation. You may apply.

The particle nucleus used in the coating method or the absorption method may be a particle nucleus prepared by excluding a part of the particle nucleus or a raw material prepared by the same method as the granulation agent of the granulation method, and a cork or foamed shirasu prepared in a suitable particle size in advance. The surface floating agent such as calcined vermiculite, expanded pearlite, expanded pumice and expanded synthetic resin may be used as the particle nucleus as it is.

The particle size of the sleep-floating pesticide granules of the present invention is usually 0.1 to 5 mm, preferably 0.3 to 3 mm, and more preferably 0.5 to 2 mm. If the particle size is too large, drying of the particles becomes difficult when produced by the granulation method, and the granules are susceptible to the influence of wind on the water surface, which is not preferable.                 

In the case of the granules granulated from a powder raw material, the sleep-floating pesticide granules of the present invention may be any of disintegratable granules and non-disintegrating granules when introduced into water.

The shape of the particles of the sleep-floating pesticide granules of the present invention is not particularly limited and may be, for example, columnar, spherical or indefinite.

The apparent specific gravity of the sleep-sustaining agrochemical granules of the present invention is usually 0.15 to 0.50, preferably 0.20 to 0.45, and more preferably 0.25 to 0.40 in view of ease of handling, productivity, and floating solubility of the particles in the surface.

Since the sleep-sustaining pesticide solid preparation of the present invention contains a high concentration of the pesticide active ingredient, it must be dispersed, dissolved or diffused in water promptly after it has been expanded to the surface. If the granules containing the high concentration of pesticide active ingredients are precipitated due to insufficient dispersion, dissolution and diffusion, local presence of the active ingredients of pesticides may occur at the settling point, which may cause weakness or ineffectiveness. In addition, if the pesticide active ingredient is not freed from the granules and floats on the water surface for a long time, the problem of being gathered in one place by the wind is concerned.

Although the sleep-floating pesticide solid preparation of the present invention can be uniformly processed in paddy fields in the same way as ordinary granules, it is very good to spread on the surface of the water. Treatment (input treatment), ② shake the rice paddy along the rice paddy (edge treatment), or ③ treat the surface-floating pesticide solid preparation or pack at the water inlet when watering the rice paddy, and with irrigation water. Diffusion into paddy fields (water inlet treatment), etc., and even in paddy fields with some obstacles in the water or rice paddy where rice is grown, the active ingredients of pesticides can be uniformly diffused into paddy fields without sufficient damage. Can increase the biological effect.

The water-soluble film of the pack for processing into the rice paddies is a film having a property of dissolving or dispersing in water. The raw material of the water-soluble film used may be, for example, polyvinyl alcohol or derivatives thereof, pullulan film or polyethylene oxide or derivatives thereof, and preferably polyvinyl alcohol or derivatives thereof.

When the sleep-floating pesticide solid preparation of the present invention is divided into packs of water-soluble films that do not have electrostatic properties, the water-soluble film may inhibit the expansion of the sleep-floating pesticide solid preparation. In this case, the sleep expansion agent dissolves in water and loses power before the surface-sustaining pesticide solid preparation is sufficiently diffused. Malleable In such a case, the pesticide active ingredient is present locally in a narrow range near the dropping point, and there is a fear that a desirable result cannot be obtained. Thus, the water soluble film is preferably an expandable water soluble paper.

The expansion acceptor is itself a film or sheet having a property of easily dispersing or dissolving in water to make the surface-floating agrochemical solid agent extend to the surface of the water. The electrolytic receptacle used may be, for example, a film or sheet consisting of polyvinyl alcohol or a derivative thereof (hereinafter abbreviated as PVA film).

A PVA film is a polyvinyl alcohol having a degree of polymerization of 500 to 2000 and a saponification degree of 80 to 98% in the form of a film or a sheet with a small amount of plasticizer and stabilizer, and a small amount of carboxylic acid or sulfonic acid in the polymer. Films or sheets containing copolymers.

The water-soluble film needs to have high mechanical strength and cold resistance and is water-soluble. If the polymerization degree of polyvinyl alcohol serving as a raw material is too high or the degree of saponification is too high, it is difficult to dissolve in cold water, which is not preferable. Although the thickness of a water-soluble film also depends on film strength and dissolution time, it is 20-80 micrometers normally, Preferably it is 30-50 micrometers.

Although the edge part of a water-soluble film may be sealed with a paste, there exists a problem in workability, and the part which paste | laminated by the paste may not melt | dissolve well, and it is preferable that it can heat-sealed at this point.

The weight of the pack for input treatment to the paddy field is usually 10 to 200 g per pack, preferably 20 to 100 g, and more preferably 25 to 60 g. With this weight, it is possible for a child, a female or an elderly person to easily put a pack at a target point within 15 m. If the pack is heavier than this, it is painful to put it in, and it is not easy to process a large area, and at a weight below this, the pack is affected by the wind, making it difficult to reach the target point.

Since the sleep-floating pesticide solid preparation of the present invention is widely expanded in the water surface, and the active ingredient of the pesticide is widely spread, it is not necessary to inject it into the paddy field at an ordinary size, and it is 2 to 3 m away from the rice field. It is enough to put it on the surface.

Too many packs to be put into the paddy field may require labor to be put into the paddy field, resulting in labor savings and economic disadvantages. Too few packs may lead to insufficient expansion of the surface-floating pesticide solid preparation. It is 1-30 pieces of rice paddies 10a, Preferably it is 2-20 pieces.

The pack for processing in the paddy field is enveloped in paper, resin, an aluminum foil or aluminum or silica deposited on it, an envelope, a box or a bottle made of metal, wood, or the like.

The sleep-floating pesticide solid preparation of the present invention can be packaged in the same manner as the outer case of the pack, even in the case of the sleep-floating pesticide solid preparation which is subjected to edge treatment or water inlet treatment.

The sleep-floating pesticide solid preparation of the present invention is stable with respect to moisture absorption in terms of physical properties. Therefore, although it is not necessary to be careful about moisture absorption compared with the preparation containing a foaming agent, since a water-soluble film will be destroyed when water is added, it is preferable to use the exterior which performed appropriate waterproofing.

1 is a pesticide active ingredient concentration measurement position of Test Example 2.

2 is a pesticide active ingredient concentration measurement position of Test Example 3.

3 is a method of treating pesticide of Test Example 4.

Best Mode for Carrying Out the Invention

Although an Example, a comparative example, and a test example are given to the following and this invention is demonstrated more concretely, this invention is not limited to these. The following parts mean parts by weight.

(Examples 1-18)

Sleep-suspendable granules

24 parts of pyroquilon original, 3 parts of talc (Japanese pharmacy room) and 1 part of Carplex # 80 (manufactured by Shionogi Seiyaku Co., Ltd., amorphous synthetic silica) were mixed and ground with a sample mill (Fuji Powder Co., Ltd., hammer mill). A pyroquilon premix was obtained. In addition, each of the sleep extenders and Carflex # 80 shown in Table 1 were mixed at a ratio of 1: 1, and ground with a sample mill to obtain a 50% sleep extender premix, respectively.

While putting 35 parts of Hirucon S-1 (manufactured by Hiruishiga Chemical Co., Ltd., calcined vermiculite 3 to 0.5 mm) into a ribbon blender, while adding 33 parts of super oil C (manufactured by Nippon Seki Oil Co., Ltd., crude liquid paraffin) Mix and wet the surface of the particles, add 28 parts of the pyroquilon premix, mix and coat the surface of the particles, and then add 4 parts of the 50% sleep filler premix and mix to coat the surface of the particles. The sleep-floating expandable granules containing were obtained.

In Table 1 below, Et is an ethyl group, 2-Et-C ₆ H ₁₃ is a 2-ethylhexyl group, iso-C ₉ H ₁₉ is an isononyl group, and EO is a formula -CH ₂ -CH ₂ -O- PO is a group represented by the formula -CH ₂ -CH (CH ₃ ) -O-,-(EO) _3- (PO) _5- (EO) ₂ -is 3 mol of ethylene oxide, propylene oxide 5 Moles and 2 moles of ethylene oxide represent groups added in this order, the "-" symbol in the derivative column indicates that the sleep expanding agent is a compound (I), and the "ethyl ether" symbol in the derivative column indicates that the sleep expanding agent is a compound (I ), And the "ammonium phosphate ester ammonium salt" symbol in the derivative column indicates that the sleep expanding agent is an ammonium salt of the phosphate ester of compound (I).

Sleep enhancer R ¹ O- (AO) _m- (BO) _n -H (I) Example number Sleep expansion agent R ₁ -(AO) _m- (BO) _n- derivative One C ₆ H ₁₃ -(EO) _2- - 2 2-Et-C ₆ H ₁₃ -(EO) _2- - 3 2-Et-C ₆ H ₁₃ -(EO) _2- 2-ethylhexyl ether 4 2-Et-C ₆ H ₁₃ -(EO) _5- - 5 2-Et-C ₆ H ₁₃ (EO) _3- Ethyl ether 6 2-Et-C ₆ H ₁₃ -(EO) _3- (PO) _5- (EO) _2- - 7 2-Et-C ₆ H ₁₃ -(EO) _15- (PO) _3- - 8 iso-C ₉ H ₁₉ -(EO) _2- (PO) _7.2- (EO) _5.3- - 9 2-Et-C ₆ H ₁₃ -(EO) _2- Ammonium Phosphate 10 2-Et-C ₆ H ₁₃ -(EO) _2- Phosphate Sodium Phosphate 11 2-Et-C ₆ H ₁₃ -(EO) _2- Phosphate ester triethanol amine salt 12 2-Et-C ₆ H ₁₃ -(EO) _2- Phosphate Ester 13 2-Et-C ₆ H ₁₃ -(EO) _2- Calcium Phosphate 14 2-Et-C ₆ H ₁₃ -(EO) _2- Ammonium Sulfate 15 2-Et-C ₆ H ₁₃ -(EO) _2- Potassium Sulfate 16 C ₄ H ₉ -(EO) _2- (PO) _1- Phosphate ester isopropylamine salt 17 C ₆ H ₁₃ -(EO) _2- (PO) _1- Phosphate ester triethanol amine salt 18 iso-C ₉ H ₁₉ -(EO) _2- (PO) _7.2- (EO) _5.3- Phosphate Sodium Phosphate

The sleep extenders described in Examples 1, 2, 9, 10, and 12 were commercially available products (manufactured by Nippon Nukazai Co., Ltd.). Other sleep expanding agents can be produced according to the method described, for example, as a new surfactant (Hori Gucci Hiroshi, Sankyo Publishing Co., Ltd., published 50 years).

( Example 19)

Sleep Floatable Granules and Pack

42 parts of foamed shirasu (0.3-1.0 mm) were put into a Nauter mixer (manufactured by Hosogawa Micron Co., Ltd.) and mixed while adding 25 parts of super oil C to wet the surface of the particles, followed by the preparation of pyroquilon described in Examples 1-18. 28 parts of the mixture was added and mixed to coat the particle surface, and then 5 parts of the 50% sleep filler pre-mixture described in Example 8 was added and mixed to coat the particle surface, whereby sleep flotation containing 24% pyroquilon A granule was obtained.

50 g of each of the obtained sleep-floating expandable granules is divided into Hiceron C200 (a PVA film having a thickness of 40 µm, manufactured by Nippon Kosei Film Co., Ltd.), to obtain a pack for non-feeding.

(Example 20)

Sleep Floatable Powder Formulation and Non-feeding Pack

47.5 parts of foamed shirasu (0.03-0.15 mm) and 22.5 parts of polyvinyl chloride powder were placed in a redige mixer (manufactured by Matsuzakaboeki Co., Ltd.), and 25 parts of pretilachlor original material and 5 parts of sleep extender described in Example 17 were prepared. It mixed, adding the mixed solution, and obtained the sleep-floating expandable powder formulation containing 25% of pretillachlor.

The obtained sleeping floatable powder formulation was divided into 30 g each of hysrone C200, and the pack for non-injection was obtained.                 

(Example 21)

Sleep Floatable Granules and Pack

63 parts of pyrazolate elements and 0.85 parts of nuchol 291PG (sodium salt of diethylhexylsulfosuccinate, manufactured by Nippon Nukazai Co., Ltd.) were suspended in 36.15 parts of water, and the suspension was dinomil (bead mill, Shinmaru enterprise). Pulverized product was used to obtain a pulverized product containing 63% of pyrazolate. To 57.14 parts of the obtained pulverized product, 2.5 parts of toxanone GR31A (manufactured by Sanyosei Co., Ltd., acrylic acid dispersant) was added and mixed to obtain a pyrazolate slurry. 14 parts of cork (0.2 to 0.5 mm), 7 parts of bentonite (manufactured by Hotaku Kogyo Co., Ltd., Hotakajirushi), 7 parts of serogen 7A (sodium salt of carboxymethylcellulose, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) and wood mill 14.52 parts of (Neolite Kosan Co., Ltd.) were mixed in a kneader, and 59.64 parts of the pyrazolate slurries were added and kneaded by adding a small amount of water, followed by a dome gran (manufactured by Fuji Powder Co., Ltd., extrusion granulator) for a screen of 1.5 mm. Passed through and extruded to assemble. The obtained wet particle | grain was dried at 100 degreeC using the fluidized bed drier, and it isolate | separated into the sieve of 4.76-1.20 mm, and obtained the pyrazolate rich granule. 80 parts of the obtained thick granules were put in a nut mixer, and a mixed solution of 15 parts of butachlor and 5 parts of the sleep expanding agent described in Example 18 was added, mixed and absorbed to thereby obtain 36% of pyrazolate and 15% of butachlor. The sleep-floating expandable granules containing were obtained.

The obtained sleep-floating expandable granules were divided into 50 g each of hysrone C200 to obtain a pack for non-feeding.

(Comparative Examples 1-4)

Sleep Floating Granules

Each sleep-floating granule was obtained by the same method as Example 1 except having used the sleep extender shown in Table 2 below instead of the sleep extender described in Example 1.

Comparative example number Sleep expansion agent One Safinol 104 (acetylene surfactant, manufactured by Nisshin Chemical Co., Ltd.) 2 Seal Guard 309 (Silicon Surfactant, manufactured by Tore Dow Corning Corporation) 3 Unidine DS101 (fluorine-based surfactant, manufactured by Daikin Kogyo Co., Ltd.) 4 Nucol 291PG (sodium salt of diethylhexylsulfosuccinate, manufactured by Nippon Nukaza Co., Ltd.)

(Comparative Example 5)

Sleep Floating Powder Formulation and Non-feeding Pack

In the same manner as in Example 20, except for using Nucall 291PG instead of the sleep expanding agent described in Example 20, a sleep-floating powder formulation and a pack for non-feeding were obtained.

(Test Example 1)

Possibilities of Pesticide Active Ingredients in Contaminated Water Surfaces

Water was placed in a resin container having a width of 25.5 cm and a length of 32 cm to adjust the water depth to 2 cm. After the water had calmed down, 0.25 g of wood mill was evenly sprayed on the water surface to cover the water surface with the wood mill. 0.1 g of the sleep-floating expandable granules of Examples 1 to 18 and the sleep-floating granules of Comparative Examples 1 to 4 were respectively charged in the center of the water surface. 1 minute after the injection of granules, the state of sleep was photographed and the ratio of the number of cracks into which the granules entered and the area where the wood mill was pushed out of the surface by the injection of granules and the ratio to the area of the container ( 5% units) was measured to determine the integrity of the water surface. The results are shown in Table 3.

Possibilities of Pesticide Active Ingredients in Contaminated Water Surfaces Test granules Confirmability Surface Crack (Number) % Of water surface with wood mill pushed away Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Example 11 Example 12 Example 13 Example 14 Example 15 Example 16 Example 17 Example 18 4 4 4 4 4 5 5 6 6 5 4 7 4 5 5 6 4 5 50 55 55 50 55 70 55 75 70 65 60 75 65 60 60 70 60 75 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 2 3 1 2 25 30 10 15

The sleep-suspending granules of the present invention exhibited excellent electrostatic properties even under conditions contaminated with sleep compared to the sleep-suspending granules of Comparative Examples.

(Test Example 2)

Uniformity of Pesticide Active Ingredients in Contaminated Water Surfaces

In a room with no wind, edges 90 cm wide, 7 m long and 10 cm deep were made of foamed plastic and installed horizontally. A black vinyl sheet was attached to the inner surface of the edge and water was added to adjust the depth to 5 cm. 20 g of wood mill was spread evenly on the water surface through a sieve having an opening diameter of 0.5 mm. After the sleep was calm, 3.15 g of the sleep-suspendable granules of Example 19 and 3.15 g of the sleep-suspendable granules of Comparative Example 2 were each treated at a position of 10 cm from the end of the edge. After 5 minutes of treatment, the distance from the input point to the tip of which the surface of the wood mill was pushed out by the introduction of particles was measured, and after 3 hours, 7 hours and 24 hours of treatment, as shown in FIG. At the points a and c 50 cm away from both ends on the centerline, the concentration of the active pesticide active ingredient in water at a depth of 2.5 cm was measured to investigate the uniformity of the active pesticide active ingredient. The results are shown in Table 4.

Uniformity of Pesticide Active Ingredients in Contaminated Water Surfaces Test granules Distance from granulation input point to tip where wood mill is pushed out (m) Pesticide active ingredient concentration measurement location Pyroquilon concentration in water (ppm)                                          3 hours after treatment 7 hours 24 hours Example 19 5.8 a b c 3.62 3.07 0.05 3.02 2.81 0.65 2.80 2.53 1.58  Comparative Example 2 2.9 a b c 8.49 0.04 0 6.35 1.31 0 5.85 1.83 0.04

Compared with the sleep-suspending granules of the comparative example, the sleep-suspending granules of the present invention had a faster diffusion of the active ingredient of the pesticides under the condition of contaminated sleep, and a better uniformity of the active ingredients of the pesticides in water.

(Test Example 3)

Uniformity and Herbicidal Effects of Pesticide Active Ingredients in Paddy Rice Fields

Rice fields were planted in 10 m × 10 m fields. After 7 days, the water surface was covered with a wood mill by adjusting it to a depth of 5 cm and uniformly treating 100 g of wood mill per compartment with Mizether Duster (Small spreader, manufactured by Arimitsu Kogyo Co., Ltd.). The pack for non-feeding of Example 20 and the comparative example 5 was thrown into the center of each compartment, and the state which the granules spread on the water surface was observed. In addition, the area where the wood mill was pushed out was measured at the point where diffusion reached the maximum after 10 minutes of treatment. After 24 hours of treatment, as shown in Fig. 2, water from the bottom of the rice paddy was collected from the dropping point 3 and the points 1, 2, 4 and 5 separated by 1 m from each corner, and analyzed by determining the concentration of the pesticide active ingredient in water. The results are shown in Table 6.

Uniformity of Pesticide Active Ingredients in Rice Fields Contaminated with Water Trial Pack Wood Mill Pushed Out and Area (m ² ) Pesticide active ingredient concentration measurement location Concentration of pretilachlor after 24 hours (ppm) Example 20 7 starfish shapes, 20 1 (wind blowing side) 2 3 (center) 4 5 (wind blowing side) 1.03 1.45 2.80 1.28 1.85  Comparative Example 5 2 on board, 3 1 (wind blowing side) 2 3 (center) 4 5 (wind blowing side) 0.32 0.94 6.23 0.72 1.03

Further, after 40 days of non-feeding pack treatment, the herbicidal effect on Echinochloa crusgalli, which had been sown before seeding at water collection points 1 to 5, was examined. The occurrence of dynabier was not seen. On the other hand, in the processing tool of the comparative example 5, some residues were confirmed at the point of 1 and 4 which touched the wind blowing side at the time of a process.

As described above, the paddle pack of Example 20 of the present invention has a good spreading of the pesticide active ingredient in the paddy field in the paddy field contaminated with water, and is uniformly spread all over the paddy field after 1 day of treatment. Although the effect was also favorable, in the pack for non-injection of the comparative example 5, even after 1 day of processing, it did not become uniform and herbicide effect was also inferior to Example 20.

(Test Example 4)

Herbicide Effect Test in Paddy Rice Fields

It was planted in rice paddies with a width of 30a. After confirming that algae occurred in about one third of the rice paddy area 10 days after planting, as shown in Fig. 3, 1500 g of the surface-floating expandable granules of Example 21 were treated with water inlet treatment methods (the granules were irrigated with irrigation water). Processing method of pesticide flowing into the rice paddies from the water inlet) and edge processing method (processing method of pesticide which shakes 750 g of granule at about 50 cm from the rice paddy while walking the long rice paddy on both sides) and Example 21 A 50 g × 30 pack for paddy feeding was used using a charging treatment method (a pesticide treatment method in which 15 packs were put at a point of about 7 m from the paddy field while walking on both sides of the long paddy field). After 40 days of application, herbicidal effects were examined for the 3 m position and the central 3 rows from two long rice fields. In either test zone, almost no residue was observed, and a very high herbicidal effect was obtained.

The pesticide solid preparation of the present invention has good water surface stability even in rice fields with algae, vinegar, and the like, and has good uniformity of the active ingredient of the pesticides in the rice fields. Therefore, it is a pesticide solid preparation which a farmer can use safely in the pesticide treatment after rice grows, or the paddy field with the above-mentioned obstacle, and the effect of the pesticide active ingredient is fully exhibited. In addition, the pack for non-loading of the present invention can be used under the above disadvantageous conditions, and contributes greatly to the labor force saving of the paddy agriculture.

Claims (16)

A compound represented by the general formula (I), the phosphoric esters, the sulfate esters and their salts of the ester and the compound of the C ₁ ~C _{10 1} or two or more sleep check premise is selected from the group consisting of alkyl ether; Pesticide active ingredient; And sleep-sustaining agrochemical solids containing a sleep-sustaining agent selected from foamed shirasu, foamed pearlite, foamed pumice, calcined vermiculite, cork, wood mill, foamed synthetic resin, synthetic resin powder or plastic hollow body: [Formula 1] R ¹ O- (AO) _m- (BO) _n -H [Wherein, R ¹ represents a C ₄ to C ₁₀ alkyl group, A represents a group represented by the formula -CH ₂ -CH _2- , B represents a group represented by the formula -CH ₂ -CH (CH ₃ )-, m represents 0-30, n represents 0-30, provided m and n are not 0 at the same time, when n is 0, m is 2 or more, and when m and n are not all 0 m AO The order in which the groups and the n BO groups combine is arbitrary. delete The sleep-floating pesticide solid preparation according to claim 1, wherein R ¹ is a C ₆ -C ₁₀ alkyl group. The sleep-floating pesticide solid preparation according to claim 1, wherein m is 0 to 10 and n is 0 to 10. The sleeping part according to claim 1, wherein R ¹ is an ethylhexyl or isononyl group, m is 0 to 10, n is 0 to 10, a phosphate ester or an ammonium salt, sodium salt or potassium salt of the phosphate ester. Oily pesticide solids. The sleep-floating pesticide solid preparation according to claim 1, wherein R ¹ is an ethylhexyl or isononyl group, m is 2 to 8, n is 0 to 8, a phosphate ester or a sodium salt of the phosphate ester. delete delete The sleep-floating pesticide solid preparation according to any one of claims 1 and 3 to 6, wherein the sleep-floating pesticide solid preparation is a granule having a particle diameter of 0.1 to 5 mm. A pack for non-injection, wherein the sleeping-floating agrochemical solid preparation according to any one of claims 1 and 3 to 6 is contained in a water-soluble film. The pack according to claim 10, wherein the water-soluble film is a film or sheet made of polyvinyl alcohol or a derivative thereof. The pack of claim 10, wherein the pack has a weight of 10 to 200 g per pack. A method for controlling harmful organisms generated in rice paddies, wherein the pack for paddy fields according to claim 10 is treated in 1 to 30 paddies per 10 a. A method for extinguishing harmful organisms occurring in paddy fields, wherein the sleep-floating pesticide solid preparation according to any one of claims 1 and 3 to 6 is shaken and processed along the paddy field. The water-borne floating pesticide solid preparation according to any one of claims 1 and 3 to 6, which is treated in the water inlet when water is applied to the rice paddy, is produced in the rice paddy, which is diffused into the rice paddy with irrigation water. How to get rid of harmful organisms. A method for controlling harmful organisms generated in rice paddies, wherein the pack for paddy fields according to claim 10 is treated at the water inlet when the paddy is watered, and diffused into the paddy field with irrigation water.

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