KR20000076729A - Agrochemical formulations for water surface application - Google Patents

Abstract

The present invention

A) solid core material of calcined pumice having an apparent specific density of less than 1 and a particle diameter of about 500 to about 1,400 μm, and

B) a first coating layer comprising at least one water soluble polymer and

At least one pesticide active compound having low water solubility,

At least one dialkylsulfosuccinate salt,

At least one other surfactant,

At least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester, and

A second coating layer optionally comprising further additives, or

C) a first coating layer comprising at least one water soluble polymer and

At least one pesticide active compound having low water solubility,

-At least one pesticide active compound that is slightly soluble or well soluble in water,

At least one dialkylsulfosuccinate salt,

At least one other surfactant,

At least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester,

Wax or polyethylene,

Hydrophobic silica, and

Optionally consisting of a second coating layer comprising further additives,

Novel pesticide formulations for application to water, methods for their preparation and their use for the application of biologically active compounds to water of discussion.

Description

Agrochemical formulations for water surface application

The present invention relates to a novel pesticide formulation that is applied to the surface to float, move and solubility along the surface. The invention also relates to a process for the preparation of such formulations and to the use thereof for the application of pesticides to the water surface of the discussion. Finally, the present invention relates to a novel pesticide premixture composition.

Various forms of preparations for dispersing agricultural agents are already known. Thus, pesticides can be applied in the form of preparations such as granules, powders, hydrating powders, glidants, aqueous solutions, liquids, emulsions and the like. In addition, recently, tablets (so-called jumbos) and packs, ie, water-soluble bags containing a synthetic or active compound in solid form impregnated with the active compound, have been mixed with additives.

In addition, there is an increasing demand for further labor savings in the agricultural field, and the amount of pesticides to be applied in consideration of environmental aspects is minimized. have.

Under these circumstances, it has recently been developed to reduce the dosage of granules to an amount of 30 to 10 kg / dL, to spread the preparation using a machine, and to use a large throw-in formulation. By using a large throwing agent, the active ingredient was to be uniformly dispersed in the rice water. To this end, the preparation is introduced into the water from the rice paddy rather than in the rice paddy by workers entering the water. Specifically, 100 g or 50 g tablets, balls, and individual packages have been tested in which effective ingredients are readily dispersed in the water surface using water-soluble excipients and blowing agents. However, these formulations are applied in extremely localized areas as compared to conventional granules. Therefore, it takes a long time for the active ingredient of the preparation to be uniformly distributed in the sleeping surface, or in some cases, the active ingredient is not dispersed throughout the sleeping surface. As a result, its effect becomes nonuniform and phytotoxicity occurs.

Repeatedly, large throwing formulations are suitable to save labor costs for applying them. However, it has a disadvantage in that it is difficult to disperse the active ingredient of the preparation quickly and uniformly in the sleeping surface. Therefore, it is necessary to prepare a formulation that does not have this disadvantage.

In order to solve the above disadvantages, a pesticide preparation for sleep application has been proposed in JP-A 155 703/93. However, some of the known formulations do not spread sufficiently along the surface of the discussion and sink to the point of application. Moreover, when known formulations are used, the formulations are relatively large in size, which may be a problem in processing and distribution.

When using pesticide formulations for sleep application with good floating and mobility, it is important to control the solubility of the pesticide active ingredient in terms of phytotoxicity and biological effects. Some of the active pesticides are soluble in water, while others are poorly soluble in water, making water solubility difficult. In JP-A 92 007/96, for example, a premixture of pesticides in which an active ingredient is mixed with a substance which is insoluble or insoluble in water is used as a method for controlling the solubility of an active ingredient that is well soluble in water. The composition is proposed. Examples of this type of material include, for example, a combination of white carbon with microcrystalline wax higher than 50 ° C and lower than 130 ° C. However, the solubility of these agents is not sufficiently controlled and therefore improvements are desired.

As a result of intensive studies to solve the above-mentioned problems according to the present invention, a novel pesticide formulation for treating the discussion sleep was found. When the formulations are applied to the surface, these formulations float and move along the surface, thereby uniformly dispersing the biologically active substance throughout the surface of the paddy field.

1 shows a bag of a water-soluble film having a cutout.

It is a figure which shows the place where the arrangement of a petri dish and the preparation were dropped in Test Example 1 (diffusion test).

FIG. 3 is a diagram showing a point at which the preparation was dropped, a sample collection point, and a point where arrival of particles was observed in Test Example 2 (diffusion evaluation test in the discussion model).

Fig. 4 is a diagram showing a point at which a test agent (formulation) was dropped into paddy fields in Test Example 4 (herbicidal effect on paddy field and phytotoxicity on transplanted rice).

Therefore, the present invention

A) solid core material of calcined pumice having an apparent specific density of less than 1 and a particle diameter of about 500 to about 1,400 μm, and

B) a first coating layer comprising at least one water soluble polymer and

At least one pesticide active compound having low water solubility,

At least one dialkylsulfosuccinate salt,

At least one other surfactant,

At least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester and

A second coating layer optionally comprising further additives, or

C) a first coating layer comprising at least one water soluble polymer and

At least one pesticide active compound having low water solubility,

-At least one pesticide active compound that is slightly soluble or well soluble in water,

At least one dialkylsulfosuccinate salt,

At least one other surfactant,

At least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester,

Wax or polyethylene,

Hydrophobic silica and

Optionally consisting of a second coating layer comprising further additives

Provided are novel pesticide formulations in the form of solid particles.

The invention also

-At least one pesticide active compound that is slightly soluble or well soluble in water,

-Waxes,

Hydrophobic silica, and

Optionally including further additives

Provided are novel pesticide premix compositions.

The invention also

a) mixing at least one aqueous solution of water-soluble polymer with a solid core material of calcined pumice having an apparent secretion less than 1 and a particle diameter of about 500 to about 1,400 μm, and then drying the mixture,

b) the obtained pre-treated material is subjected to at least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester and then

At least one pesticide active compound having low water solubility,

At least one dialkylsulfosuccinate salt,

At least one other surfactant, and

Optionally coating in turn with a powder mixture comprising further additives,

c) pre-treated core-materials as described in (a) above with at least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester, and then

A powder mixture comprising the remaining ingredients described in (b) above and

-At least one pesticide active compound that is slightly soluble or well soluble in water,

Wax or polyethylene,

Hydrophobic silica, and

Characterized in that it is optionally coated in turn with a powder mixture containing further additives,

Provided are methods for preparing the above-mentioned pesticide formulations.

Finally, the present invention provides a method of applying a pesticide to a water of the argument, characterized in that the pesticide preparation according to the invention is added to the water of discussion.

In the present specification, the apparent secretivity is a value calculated by dividing the mass (g) of one particle with internal pores by the volume (ccm) of one particle with internal pores. This value is different from bulk specific density.

It is surprising that the pesticide preparations according to the invention are much more suitable for uniformly dispersing biologically active compounds in the water of water than the corresponding known preparations.

Pesticide formulations according to the invention have several advantages. Thus, when the formulation is applied to the water in question, the particles float and move in a random direction on the surface of the water. As a result, the particles develop very quickly and evenly throughout the water surface, and due to the movement of the particles, biologically active compounds are released from the particles and uniformly dispersed in the rice water. In the case of active compounds which are slightly soluble or well soluble in water, their solubility is inhibited, while in the case of active compounds having low water solubility, their solubility is promoted. Another advantage of the novel pesticide formulations of the invention is that they do not exhibit any adverse effects such as phytotoxicity. The preparations according to the invention also have a sustained effect if they contain active compounds which are slightly soluble or well soluble in water. Thus, the effectiveness of these formulations is maintained for a longer time than the effectiveness of this type of conventional formulation. It is also pointed out that the preparations according to the invention are very suitable for releasing each active compound at an optimum dissolution rate. That is, solubility is promoted or reduced depending on the solubility of the active ingredient. Finally, the premix composition according to the present invention can be used to prepare granules that exhibit sustained release in water.

The pesticide preparation according to the present invention, the preparation method thereof and the method of use thereof are described in detail below.

The core material used as a carrier in the agrochemical preparations according to the invention is in the form of particles having an apparent secretivity of less than 1, preferably 0.7 to 0.1 and a diameter of about 500 to about 1,400 μm, preferably of about 500 to about 1,000 μm. Is calcined pumice. A core material having such a diameter can be produced by removing particles larger than the upper limit of the above range and removing particles smaller than the lower limit using a standard sieve according to Japanese Industrial Standards (JIS).

As a specific example of calcined pumice, Shirasu Balloon may be mentioned.

The first coating layer comprises one or more water soluble polymers. Examples of such polymers may include polyvinyl alcohol, carboxymethyl-cellulose, polyvinylpyrrolidone, polyethylene glycol, methylcellulose, ethylcellulose, hydroxymethylcellulose, hydroxyethylcellulose and the like.

Polyvinyl alcohol and polyethylene glycol are particularly preferred. The water soluble polymers can be used individually or in combination of two or more components.

Dialkylsulfosuccinate salts and other surfactants in pesticide formulations according to the present invention change the interfacial tension between air and water, allowing the formulation to float and move on rice water, while simultaneously releasing the pesticide active ingredient into water. It is provided as a formulation.

As an example of such a dialkylsulfosuccinate salt, sodium dioctylsulfosuccinate may be mentioned.

The preparations according to the invention also contain at least one further surfactant (tension reducer) suitable for changing the interfacial tension between air and water. Preferred components of this type are materials that have the ability to reduce the surface tension of water by at least 30% when added to water at its critical micelle concentration (cmc). Examples of such materials include alkylsulfocarboxylate salts, lignosulfonate salts, alkylbenzenesulfonate salts, alkylnaphthalenesulfonate salts, formalin condensates of naphthalenesulfonate salts, fatty acid soaps, alkylsulfosuccinate di-salts, Alkylsulfoacetate salts, alkylsulfate salts, alkylphosphate salts, alkylsulfonate salts, alkylamino acid salts, alkylamine salts, acetylene-alcohols, acetylene-glycols, silicone type surfactants, secondary higher alcohol ethoxysulfates, fatty acid alkylolamides Sulfate ester salts, polyoxyethylene alkyl ethers, polyoxyethylene alkyl ether phosphate salts, glycerol fatty acid esters, sorbitan fatty acid esters, alkylammonium salts, alkylallylsulfonate salts, N-acylmethyl-taurine salts and the like can be mentioned. have.

Particularly preferred surfactants are sodium lignosulfonate, formalin condensates of sodium alkylnaphthalenesulfonates, sodium salts of fatty acid soaps, di-sodium salts of alkylsulfosuccinates, sodium alkylsulfoacetates, sodium alkylsulphates, sodium alkylsulfos Acetates, acetylene alcohols, acetylene glycols, silicone type surfactants and polyoxyethylene alkyl ethers. These compounds can be used individually or in mixture of 2 or more. Such materials are preferably those which form a solid powder at room temperature, generally at room temperature.

The mixing ratio of the dialkylsulfosuccinate salt and other surfactants in the formulations according to the invention may vary within certain ranges. Generally, 0.01 to 10 parts by weight, preferably 0.1 to 8 parts by weight of other surfactant is present per 1 part by weight of dialkylsulfosuccinate salt.

Pesticide formulations according to the invention also comprise at least one polyoxyethylene-sorbitan fatty acid ester or polyoxyethylene-sorbitol fatty acid ester. Preferred compounds of this group are polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan tristearate, polyoxyethylene sorbitan monooleate Polyoxyethylene-sorbitan fatty acid esters such as polyoxyethylene sorbitan trioleate, polyoxyethylene sorbitan monoisostearate, polyoxyethylene sorbitan dioleate and the like and also polyoxyethylene sorbitol hexastearate, polyoxy Polyoxyethylene-sorbitol fatty acid esters such as ethylene sorbitol tetrastearate, polyoxyethylene sorbitol tetraoleate, polyoxyethylene sorbitol monolaurate and polyoxyethylene sorbitol monooleate and the like.

Polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan tristearate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan trioleate, polyoxyethylene sorbitol hexastearate and polyoxyethylene sorbitol tetraoleate Eight is particularly preferred.

As a further additive, the pesticide preparation according to the invention comprises at least one oily surfactant. Preferred compounds of this group are polyoxyethylene polyoxypropylene alkyl ethers, polyoxyethylene polyoxypropylene alkylphenyl ethers, polyoxyethylene polyoxypropylene block polymers, polyoxyethylene polyoxypropylene block polymers benzyl (or styryl) phenyl ethers , Polyoxyethylene benzyl (or styryl) phenyl ether, polyoxyethylene allyl ether, polyoxyethylene allylphenyl ether, polyoxyethylene alkylamine ether, polyoxyethylene alkyl ether, polyoxyethylene alkyl ester, polyoxyethylene alkyl phenyl Ethers, polyoxyethylene alkyl phenyl ether-formaldehyde condensates, polyoxyethylene glycol fatty acid esters, polyoxyethylene castor oil, polyoxyethylene fetosterols, polyoxyethylene lanolin, sorbitan fatty acid esters, calcium alkylbenzenesulfonates, poly Oxyethylene lanolin alcohol ether, polyoxyethylene lanolin beeswax derivative, polyoxyethylene lanolin fatty acid ester, polyoxyethylene hardened castor oil, polyoxyethylene fatty acid amide, polyoxyethylene fatty acid ester, propylene glycol fatty acid ester, polyoxy Ethylene glycol fatty acid esters, polyglycerol fatty acid esters, polyoxyethylene polycyclic phenyl ethers, polyoxyethylene alkyl allyl ethers, polyoxyethylene alkyl ethers and the like.

Polyoxyethylene polyoxypropylene alkyl ether, polyoxyethylene polyoxypropylene block polymer, polyoxyethylene polyoxypropylene block polymer benzyl (or styryl) phenyl ether, polyoxyethylene benzyl (or styryl) phenyl ether, polyoxyethylene Cured castor oil, polyoxyethylene alkyl ethers, polyoxyethylene polycyclic phenyl ethers, calcium alkylbenzenesulfonates are particularly preferred. These compounds may be present individually or in mixtures of two or more, preferably polyoxyethylene-sorbitan (or sorbitol) fatty acid esters.

As further additives, the preparations according to the invention may also comprise paraffin wax, glycerol esters, animal fats or oils, butadiene, polyoxyethylene alkyl ethers, polyethylene glycols, propylene glycols, glycol ethers and the like.

Agrochemically active compounds having low water solubility herein are biologically active compounds such as herbicides, insecticides, fungicides and the like having a water solubility of less than 10 ppm at 20 ° C.

The following compounds may be mentioned as specific examples of agrochemically active compounds having low water solubility. However, the present invention is not limited to these:

Herbicidal Active Compounds:

2-benzothiazol-2-yloxy-N-methylacetanilide (common name: mefenacet),

1- (2-chlorophenyl) -4- (N-cyclohexyl-N-ethylcarbamoyl) -5 (4H) -tetrazolinone (common name: pentrazamide),

1- (α, α-dimethylbenzyl) -3- (paratolyl) urea (common name: dimron),

N-[(2-chlorophenyl) methyl] -N '-(1-methyl-1-phenylethyl) -urea (common name: cumyluron),

(RS) -2-bromo-N- (α, α-dimethylbenzyl) -3,3-dimethylbutylamide (common name: bromobutide),

α- (2-naphthoxy) propionanilide (common name: naproanilide),

(RS) -2- (2,4-dichloro-m-tolyloxy) propionanilide (common name: clomeprop),

2-chloro-N- (3-methoxy-2-tenyl) -2 ', 6'-dimethylacetanilide (common name: tenylchlor),

S-benzyl-1,2-dimethylpropyl (ethyl) thiocarbamate (common name: esprocarb),

O-3-t-butylphenyl-6-methoxy-2-pyridyl- (methyl) thiocarbamate (common name: pyributicab),

n-butyl (R) -2- [4- (4-cyano-2-fluorophenoxy) phenoxy] propionate (common name: cyhalopop-butyl),

1- (diethylcarbamoyl) -3- (2,4,6-trimethylphenylsulfonyl) -1,2,4-triazole (common name: carpenstrol),

4- (2,4-dichlorobenzoyl) -1,3-dimethyl-5-pyrazolyl-p-toluenesulfonate (common name: pyrazolate),

2- [4- (2,4-dichlorobenzoyl) -1,3-dimethylpyrazol-5-yloxy] acetophenone (common name: pyrazoxifen),

2- [4- (2,4-dichloro-m-toluoyl) -1,3-dimethylpyrazol-5-yloxy] -4-methylacetophenone (common name: benzophene),

Methyl 2-[(4,6-dimethoxy-2-pyrimidinyl) oxy] -6- [1- (methoxyimino) ethyl] benzoate (common name: pyriminobac-methyl),

O-ethyl-O- (3-methyl-6-nitrophenyl) secondary-butyl-phosphoroamidothioate (common name: butamifos),

N- (2,3-dichlorophenyl) -4- (ethoxymethoxy) benzamide (common name: etobenzanide)

5- (2,4-dichlorophenoxy) -2-nitrobenzoic acid (common name: biphenox) and the like.

Insecticidal Active Compounds:

Ethyl dimethyldithiophosphorylphenylacetate (common name: pentoate),

O, O-diethyl-O- (3-oxo-2-phenyl-2H-pyridazin-6-yl) phosphothioate (common name: pyridapention),

O, O-dimethyl-O-3,5,6-trichloro-2-pyridylphosphothioate (common name: chlorpyriphos-methyl),

2- (4-ethoxyphenyl) -2-methylpropyl 3-phenoxybenzyl ether (common name: etofenprox),

(±) -5-amino-1- (2,6-dichloro-α, α, α-trifluoro-p-tolyl) -4-trifluoromethylsulfinylpyrazole-3- (carbonitrile) ( Common name: fipronil),

2,3-dihydro-2,2-dimethyl-7-benzo [b] furanyl N-dibutylaminothio-N-methylcarbamate (common name: carbosulphan),

Ethyl N- [2,3-dihydro-2,2-dimethylbenzofuran-7-yloxycarbonyl (methyl) aminothio] -N-isopropyl-β-alanineate (common name: benfuracab) ,

Butyl 2,3-dihydro-2,2-dimethylbenzofuran-7-yl N, N'-dimethyl-N, N'-thiodicarbamate (common name: furathiocarb),

(RS) -α-cyano-3-phenoxybenzyl-2,2-dichloro-1- (4-ethoxyphenyl) cyclopropanecarboxylate (common name: cycloprotrin),

2-t-butylimino-3-isopropyl-5-phenyl-3,4,5,6-tetrahydro-2H-1,3,5-thiadiazin-4-one (common name: buprofezin ),

S, S'-2-dimethylaminotrimethylene di (benzenethiosulfonate) (general name: benzol tower) and the like.

Fungicidal Active Compounds:

1- (4-chlorobenzyl) -1-cyclopentyl-3-phenylurea (common name: phencycuron),

4,5,6,7-tetrachlorophthalide (common name: phthalide),

α, α, α-trifluoro-3'-isopropoxy-o-toluanilide (common name: flutolanyl),

6- (3,5-dichloro-4-methylphenyl) -3 (2H) -pyridazinone (common name: diclomezin),

(E) -methyl 2-[[6- (2-cyanophenoxy) -4-pyrimidinyl] oxy] -α- (methoxymethylene) benzeneacetate (common name: azoxystrobin),

N- [2,6-dibromo-4- (trifluoromethoxy) phenyl] -2-methyl-4- (trifluoromethyl) -5-thiazolocarboxamide (common name: tifluzamide ),

2,2-dichloro-N- [1- (4-chlorophenyl) ethyl] -1-ethyl-3-methylcyclopropanecarboxamide (common name: capropamide),

2-cyano-N- [1- (2,4-dichlorophenyl) ethyl] -3,3-dimethylbutanamide (common name: diclocimet),

S-methyl 1,2,3-benzothiadiazole-7-carbothioate (general name: acibenzola-S-methyl) and the like.

The preparations according to the invention may contain the aforementioned active ingredients individually or in combination of two or more.

The preparations according to the invention consisting of (A) and (B) may also contain customary extenders as further additives. Specific examples of preferred extenders may include sodium sulfate, potassium sulfate, potassium chloride, saccharides, polyethylene glycols, and the like. Sodium sulfate is particularly preferred. The volume of the resulting formulation can be made smaller than others by adding an extender that is well soluble in water to reduce the amount of calcined pumice which is the core material.

The concentration of the components in the pesticide preparation according to the invention consisting of (A) and (B) can vary within a relatively wide range. In general, the formulation is used per 100 parts by weight of the formulation.

About 0.05 to about 50 parts by weight, preferably about 1.0 to about 30 parts by weight, of agrochemically active compounds having low water solubility,

Dialkylsulfosuccinate salt and other surfactants in total from about 0.9 to about 25 parts by weight, preferably from about 2.0 to about 15 parts by weight,

About 1.0 to about 50 parts by weight, preferably about 7.0 to about 40 parts by weight of polyoxyethylene sorbitan (or sorbitol) fatty acid ester,

0 to about 50 parts by weight, preferably 0 to about 40 parts by weight, of other oily surfactants,

0 to about 40 parts by weight, preferably about 0 to about 25 parts by weight, of a water soluble extender,

About 0.1 to about 30 parts by weight, preferably about 0.1 to about 25 parts by weight, of the water-soluble polymer and

Calcined pumice containing from about 10 to about 80 parts by weight, preferably from about 30 to about 74 parts by weight.

However, the above mentioned ratios are only reference values and can be appropriately changed as necessary.

The pesticide preparation according to the invention consisting of (A) and (C) as well as the pesticide premix composition according to the invention contains wax or polyethylene.

Preferred waxes include candelilla wax, carnauba wax, rice wax, Japan wax, bead wax, ozokerite, ceresin; Petroleum waxes such as paraffin wax, microcrystalline wax, petrolatum; Hardened castor oil, 12-hydroxystearic acid amide, synthetic waxes such as polyhydric alcohol fatty acid esters, and the like.

Particularly preferred waxes are carnauba wax, microcrystalline wax, japan wax and paraffin wax. These waxes may be present individually or in combination of two or more.

Preferred polyethylenes are polyethylenes having a low molecular weight such as in the range of 1,000 to 15,000, preferably 1,300 to 7,000. Optionally, paraffin wax can be added to the polyethylene. It is also possible to replace some or all of the polyethylene with polypropylene.

The pesticide preparation according to the invention consisting of (A) and (C) as well as the pesticide premix composition according to the invention also contains hydrophobic silica in solid form. Silica having a low water adsorption capacity and low silanol group properties is preferable. These formulations may also contain talc and / or white carbon as additives.

If the pesticide preparation according to the invention consisting of (A) and (C) as well as the pesticide premix composition according to the invention comprises polyethylene, they may also contain liquid paraffin as an additive.

Liquid-paraffins are understood to be hydrocarbon oils which are highly purified by washing sulfuric oil fractions, for example spindle oil fractions, with a sulfuric acid wash. It is colorless and odorless, low volatility, mainly composed of alkylnaphthalene and is called "white oil".

Liquid paraffins are particularly suitable for formulations containing active compounds which are solid and / or heat labile because of a decrease in melting temperature.

The pesticide preparation according to the invention consisting of (A) and (C) as well as the pesticide premix composition according to the invention contains at least one pesticide active compound which is slightly soluble or well soluble in water. Such agrochemically active compounds herein are biologically active compounds such as herbicides, insecticides, fungicides and the like having a water solubility of at least 10 ppm, preferably at least 13 ppm at 20 ° C.

The following compounds may be mentioned as specific examples of agrochemically active compounds which are slightly dissolved or well dissolved in water. However, the present invention is not limited to these:

Herbicidal Active Compounds:

Methyl α- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -o-toluate (common name: bensulfuron-methyl),

Ethyl 5- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -1-methylpyrazole-4-carboxylate (common name: pyrazosulfuron-ethyl),

1- (2-chloroimidazo [1,2-a] pyridin-3-ylsulfonyl) -3- (4,6-dimethoxypyrimidin-2-yl) urea (common name: imazosulfuron),

Methyl 3- (4-methoxy-6-methyl-1,3,5-triazine-2-ylcarbamoylsulfamoyl) -2-tenoate (common name: thifensulfuron-methyl),

Methyl 2- [3- (4-methoxy-6-methyl-1,3,5-triazin-2-yl) ureidosulfonyl] benzoate (common name: metsulfuron-methyl),

1- (4,6-dimethoxypyrimidin-2-yl) -3- (3-trifluoromethyl-2-pyridylsulfonyl) urea (common name: plazasulfuron),

3-chloro-5- (4,6-dimethoxypyrimidin-2-ylcarbamoylsulfamoyl) -1-methylpyrazole-4-carboxylic acid (common name: halosulfuron),

1- (4,6-dimethoxy-1,3,5-triazin-2-yl) -3- [2- (2-methoxyethoxy) phenylsulfonyl] urea (common name: cynosulfuron) ,

1- (2-chlorophenylsulfonyl) -3- (4-methoxy-6-methyl-1,3,5-triazin-2-yl) urea (common name: chlorsulfuron),

1- (4,6-dimethoxypyrimidin-2-yl) -3- [1-methyl-4- (2-methyl-2H-tetrazol-5-yl) pyrazol-5-ylsulfonyl] urea (Common name: Azimsulfuron),

1 [[o- (cyclopropylcarbonyl) phenylsulfamoyl-3- (4,6-dimethoxy-2-pyrimidinyl) urea (common name: cyclosulfamlone),

2,4-dichlorophenoxy acetic acid (common name: 2,4-D),

2-methyl-4-chlorophenoxybutyric acid (common name: MCPB),

2-methylthio-4,6-bis (ethylamino) -s-triazine (common name: cymetrine),

2-methylthio-4-ethylamino-6- (1,2-dimethylpropylamino) -s-triazine (common name: dimethacrylate),

S- (4-chlorobenzyl) -N, N-diethylthiocarbamate (common name: thiobencarb),

S-1-methyl-1-phenylethylpiperidine-1-carbothioate (common name: dimepiperate),

S-ethylhexahydro-1H-azepine-1-carbothioate (common name: molinate),

2-chloro-2 ', 6'-diethyl-N- (butoxymethyl) acetanilide (common name: butachlor),

2-chloro-2 ', 6'-diethyl-N- (2-propoxyethyl) acetanilide (common name: pretilachlor),

S- (2-Methyl-1-piperidyl-carbonylmethyl) -O, O-di-n-propyldithiophosphate (common name: piperophosph),

O, O-diisopropyl-2- (benzenesulfonamido) ethyldithiophosphate (common name: bensulfide),

2,3-dihydro-3,3-dimethylbenzofuran-5-yl ethanesulfonate (common name: benfuresate),

3-isopropyl-2,1,3-benzothiadiazinone- (4) -2,2-dioxide (common name: bentazone),

2-amino-3-chloro-1,4-naphthoquinone (common name: ACN) and the like.

Insecticidal Active Compounds:

1- (6-chloro-3-pyridylmethyl) -N-nitroimidazolidine-2-ylideneamine (common name: imidacloprid),

(E) -N- (6-chloro-3-pyridylmethyl) -N-ethyl-N'-methyl-2-nitrovinylidenediamine (common name: nitenpyram),

3- (6-chloro-3-pyridylmethyl) -2-cyanoiminothiazolidine (common name: thiacloprid),

2-tert-butylphenyl-N-methylcarbamate (common name: BPMC),

2-isopropylphenyl-N-methylcarbamate (common name: isoprocarb),

1-naphthyl-N-methylcarbamate (common name: carbaryl),

O, O-dimethyl-O- (3-methyl-4-nitrophenyl) thiophosphate (common name: pention),

O, O-diethyl-S-2- (ethylthio) ethylphosphorodithioate (common name: disulfotone),

(2-isopropyl-4-methylpyrimidyl-6) -diethylthiophosphate (common name: diazinone),

O, O-dipropyl-O-4-methylthiophenylphosphate (common name: propaphos),

2-chloro-1- (2,4-dichlorophenyl) vinyldimethylphosphate (general name: dimethylvinforce).

Fungicidal Active Compounds:

1- (4-chlorophenoxy) -3,3-dimethyl-1- (1,2,4-thiazol-1-yl) -2-butanone (common name: triadimefon),

Diisopropyl 1,3-dithioran-2-ylidene-malonate (common name: isoprothiolane),

5-chloro-N- (1,3-dihydro-1,1,3-trimethyl-4-isobenzofuranyl) -1,3-dimethyl-1H-pyrazole-4-carboxamide (common name: Furamemet),

3-allyloxy-1,2-benzoisothiazole-1,1-dioxide (common name: probenazole),

1,2,5,6-tetrahydropyrrolo [3,2,1-ij] quinolin-4-one (common name: pyroquilon) and the like.

The formulations and premixture compositions may contain the active ingredients mentioned above individually or in combination of two or more.

The remaining components of the pesticide preparation according to the invention consisting of (A) and (C) are already described with reference to the preparation consisting of (A) and (B).

The pesticide premix composition according to the present invention has the property of inhibiting the dissolution of the pesticide active compound in the composition. The technique of such agrochemical premix compositions can be applied to a wide range of active compounds which are slightly soluble or well soluble in water, as well as active compounds which have low solubility in the active compounds.

Examples of agrochemically active compounds which have low water solubility and may be present in the agrochemical premix composition include fipronil, azoxystrobin, tifluzamide and the like.

Pesticide premix compositions containing polyethylene instead of waxes are already known. However, others containing waxes are not known until now.

The concentration of the components in the pesticide preparation according to the invention consisting of (A) and (C) can vary within a relatively wide range. In general, the formulation is used per 100 parts by weight of the formulation.

About 7 to about 12 parts by weight, preferably about 7.4 to about 11 parts by weight, of agrochemically active compounds having low water solubility,

About 0.9 to about 25 parts by weight, preferably about 2.0 to about 15 parts by weight, of dialkylsulfosuccinate salts and other surfactants,

About 0.5 to 4 parts by weight, preferably about 0.52 to about 3.5 parts by weight, of agrochemically active compounds that are slightly or soluble in water,

About 0.5 to about 12 parts by weight of wax, preferably about 1.0 to about 11 parts by weight or about 0.09 to about 12 parts by weight of polyethylene, preferably about 0.1 to 11 parts by weight,

About 1 to about 8 parts by weight, preferably about 1.5 to about 7 parts by weight of hydrophobic silica,

About 1 to about 50 parts by weight, preferably about 7 to about 40 parts by weight of polyoxyethylene sorbitan (or sorbitol) fatty acid ester,

0 to about 50 parts by weight of other surfactant, preferably 0 to about 40 parts by weight,

0 to about 10 parts by weight, preferably about 0 to about 9 parts by weight, of a water soluble extender,

About 0.1 to about 30 parts by weight, preferably about 0.1 to about 25 parts by weight, of the water-soluble polymer and

From about 15 to about 65 parts by weight of fired pumice, preferably from about 30 to about 60 parts by weight.

However, the above mentioned ratios are only reference values and can be appropriately changed as necessary.

In addition, if the pesticide preparations according to the invention consisting of (A) and (C) contain polyethylene instead of wax they may also contain about 5 to about 30 parts by weight, preferably 6 to 28 parts by weight of liquid paraffin. .

The concentration of components in the pesticide premix composition according to the invention can also vary within a relatively wide range. Generally, the premix composition is used per 100 parts by weight of the composition.

About 1 to about 40 parts by weight, preferably about 5 to about 35 parts by weight, of agrochemically active compounds that are slightly or soluble in water,

About 1 to about 50 parts by weight of wax, preferably about 2 to about 45 parts by weight,

About 30 to about 80 parts by weight, preferably about 35 to about 75 parts by weight of hydrophobic silica and

-0 to about 20 parts by weight of talc and / or 0 to about 20 parts by weight of white carbon.

If the wax is replaced with polyethylene in the pesticide premix composition, the pesticide premix composition contains about 1 to about 50 parts by weight, preferably about 2 to about 45 parts by weight of polyethylene.

Paraffin wax can be added to the polyethylene. It is also possible to replace some or all of the polyethylene with polypropylene.

When the wax is replaced with polyethylene in the pesticide premix composition, the pesticide premix composition also contains about 5 to about 40 parts by weight of ape paraffin, preferably about 10 to about 30 parts by weight.

The process for preparing the pesticide preparation according to the invention consisting of (A) and (B) is carried out in the first step (a) by treating the solid core material with an aqueous aqueous polymer solution and then drying the coated material.

The application amount of the water soluble polymer may vary within a certain range. Generally, the water soluble polymer is used in an amount such that the coated material contains from about 0.005 to about 2 parts by weight, preferably from about 0.02 to about 0.7 parts by weight of water soluble polymer per 1 part by weight of calcined pumice. The pre-treated core coolum is coated with a powder mixture of the components described in (B) in the second step (b).

Step (a) of the process is preferably carried out by adjusting the particle size by sorting the calcined pumice particles into a sieve similar to a standard body having pores of 500 to 1400 μm. Thereafter, calcined pumice having an adjusted particle diameter is mixed with the aqueous aqueous polymer solution. After the mixture is stirred briefly, the solid material is filtered off and dried. The method is generally carried out at room temperature. Screening of the particles may also be carried out after the particles have been coated with a water soluble polymer.

The second step of the process for producing the pesticide preparation according to the invention consisting of (A) and (B) is generally carried out in a coating apparatus such as a pan coater by applying the coated material obtained in step (a). It is carried out by treatment with polyethylene-sorbitan (or sorbitol) fatty acid esters. Then, while still operating the coating apparatus, a powder mixture of the remaining components mentioned in (B) is added.

The powder mixture for carrying out step (b) of the process preferably mixes the necessary ingredients and in a conventional manner, for example a pin mill, hammer mill, jet mill. It is manufactured by grinding in such a way.

At least one pesticide active compound having low water solubility,

At least one dialkylsulfosuccinate salt,

At least one other surfactant, and

The powder composition, optionally containing further additives, is added slowly to the pre-treated core material, preferably with the fan coater running, until the surface of the core material is coated almost uniformly with the powder composition.

Step (b) of the process according to the invention is preferably carried out at room temperature.

The process for preparing the pesticide preparation according to the invention consisting of (A) and (C) comprises treating the solid core material with an aqueous aqueous solution of water in the first step (a) and separating the obtained coated core material and then drying Is performed. The pre-coated material obtained is treated with polyoxyethylene-sorbitan (or sorbitol) fatty acid esters, followed by one or more powder compositions containing the remaining ingredients mentioned in (C).

Step (a) of the process and the treatment of the polyoxyethylene-sorbitan (or sorbitol) fatty acid esters are preferably carried out by the abovementioned method.

The powder mixture for carrying out step (c) of the process is preferably prepared by first preparing a premix composition and then adding it to a composition containing the remaining ingredients.

The pesticide premix composition preferably contains wax (or polyethylene) and hydrophobic silica, and optionally additional additives and Henschel mixers, Loedige mixers, which are slightly soluble or well soluble in water. , By mixing uniformly under elevated temperature (less than 130 ° C.) in an apparatus such as a bag mixer and the like, and continuously stirring until cooled to room temperature. Forced cooling or natural cooling by blowing or the like may be performed as a means for returning to room temperature, but is not limited thereto.

The powder premixture composition is then mixed with the powder mixture needed to carry out step (b) of the process of the invention. The blended mixture is then slowly added to the pretreated core material to operate the pan coater until the surface of the core material is coated almost uniformly with the powder composition.

In the case of using a liquid pesticide active compound to prepare a preparation according to the present invention, the pesticide active ingredient is adsorbed to a carrier such as white carbon, talc, diatomaceous earth, clay, etc., and then dialkylsulfosuccinate salt and other surfactants. May be mixed with to obtain a powder composition.

In order to increase the efficiency when applying the preparations according to the invention the preparations can be converted into solid preparations by packing them in water-soluble films in units of about 10 to about 200 g, preferably about 25 to about 60 g per package. . The water soluble film may have vent holes through which air can be passed as needed. These holes can also be made by making a bag and then cutting it. Cleavage can be carried out at 6-12 spots, preferably 7-10 spots per bag. The cutting can be done longitudinally, laterally or at an angle. However, it is particularly preferable to cut to the side. For example, it can be cut to a width of 0.1 to 0.5 mm and a length of 2 to 5 mm.

1 shows a bag of a water-soluble film having a cutout. In Figure 1 the numerical values have the following meanings:

1 = heat sealed bag part

2 = cutting

3 = enlarged cutting plane

As the packaging material, water-soluble polyvinyl alcohol, carboxymethyl cellulose, dextrin, starch, hydroxyethyl cellulose and the like can be mentioned as examples of the material constituting the water-soluble film.

In addition, the formulations according to the invention can be added to a particular mold in units of about 10 to about 200 g and can be converted to large moldings by heating and / or compressing. These forms can be spherical, disc shaped, cylindrical, cuboid and cubic, and the like. However, it is not limited only to the above-mentioned form.

In the case of molding, the following binders may be used, but are not limited to these: polyethylene glycol, saccharides, natural gums, polyvinyl alcohols, natural or synthetic rubbers, natural or modified celluloses and the like.

In practical use of the preparations according to the invention, they can be dropped into paddy fields directly from boxes, bottles, bags and the like with suitable outlets. When processed into a solid preparation packaged in a water-soluble film, sufficient effect can be obtained by dropping 2-40, preferably 5-20, per 10 paddy fields. In some cases, the dropping interval must be essentially uniform, but random in order to achieve the desired effect by dropping.

The pesticide premix composition according to the invention can also be applied for the preparation of various formulation forms. As the form of the preparation, mention may be made, for example, of powders, tablets, granules and seed coatings, with granules (particle diameters of 0.3 to 1.7 mm) generally being preferred. These formulations can be prepared by methods known per se. These can be prepared, for example, by mixing the pesticide premix composition with a solid diluent or carrier, if necessary, using a surfactant. Extrusion granulation, coating processing, rotary granulation, compression granulation, fluidized bed granulation and stirred granulation can be mentioned as a method for producing granules. Preferably, extrusion assembly and coating processing may be mentioned. As solid diluents for extrusion granulation, for example, soil natural minerals (e.g. kaolin, clay, talc, chalk, attapulgite, montmorillonite or diatomaceous earth, etc.), synthetic minerals (e.g., highly dispersed silicon dioxide, alumina, silicates). Etc.) may be mentioned. Solid carriers for coating assembly, for example crushed and fractionated natural rocks (e.g. silica, calcite, marble, pumice, calcite, dolomite, etc.), synthetic granules of inorganic and organic powders, organic materials (e.g. sawdust, coconut Mention may be made of micro-granules of skins, corn and tobacco stocks. In addition, nonionic and anionic surfactants such as polyoxyethylene fatty acid esters, polyoxyethylene fatty acid alcohol ethers (eg alkylaryl polyglycol ethers, alkylsulfonate salts, Alkyl sulfates, arylsulfonate salts, and the like)], lignin sulfonic acid, alkylbenzenesulfonic acid, dialkylsulfosuccinate salts, polyoxyalkylene alkylphenyl ether sulfonate salts, albumin hydrolysis products may be mixed. Glues can also be used in the formulation (granules). As a glue, mention may be made, for example, of carboxymethylcellulose, dextrins, modified dextrins, natural and synthetic polymers (eg, gum arabic, polyvinyl alcohol, polyvinyl acetate, etc.). Colorants can also be used. As colorants which can be used, mention may be made of inorganic pigments (for example iron oxide, titanium oxide and prussian blue) and organic dyes such as alizarin dyes, azo dyes or metal phthalocyanine dyes. The formulations may generally contain from 0.5 to 50% by weight, preferably from 1.0 to 45.0% by weight of the aforementioned pesticide premix composition.

Example

The present invention will be described in detail in the following Examples, but is not limited to these Examples in any way. As calcined pumice, Shirasu balun (trade name: manufactured by Neolite Industry) is selected by sieves similar to sieves having pores of 500 to 1,000 μm in accordance with Japanese Industrial Standards (JIS) to adjust the particle size. It is used after.

Formulation Example 1

Pentrazamide (70%) Bulk 11.60 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

4.00 parts by weight of sodium ligninsulfonate

A powder composition was prepared by thoroughly mixing the aforementioned components.

After precoating with polyvinyl alcohol (3.60 parts by weight), the selected sirasu balon (69.00 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (9.80 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble polyvinyl alcohol film and sealed with a heat sealer to obtain a solid pesticide formulation.

Formulation Example 2

Pentrazamide (70%) Bulk 11.60 parts by weight

4.50 parts by weight of sodium dioctylsulfosuccinate

8.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

The abovementioned ingredients were mixed and ground to prepare a powder composition.

After precoating with polyethylene glycol (6.40 parts by weight), the selected sirasu balon (57.50 parts) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (12.00 parts) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 3

Mefenacet (85%) Bulk 31.80 parts by weight

3.00 parts by weight of sodium dioctylsulfosuccinate

1.00 parts by weight of sodium lignin sulfonate

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (0.80 parts by weight), the selected sirasu balon (41.10 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan trioleate (22.30 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 4

Pentrazamide (70%) Bulk 11.60 parts by weight

5.00 parts by weight of sodium dioctylsulfosuccinate

2.00 parts by weight of sodium ligninsulfonate

3.00 parts by weight of sodium alkylnaphthalenesulfonate

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinylpyrrolidone (3.30 parts by weight), the selected sirasu balon (63.80 parts by weight) is introduced into the pan coater, and polyoxyethylene sorbitan monolaurate (7.90 parts by weight) and polyoxy A mixed solution of alkylene alkyl ether (3.40 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 5

Pentrazamide (70%) Bulk 11.60 parts by weight

2.50 parts by weight of sodium dioctylsulfosuccinate

0.50 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinyl alcohol (3.90 parts by weight), the selected sirasu balon (73.40 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (8.10 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 6

Mefenacet (85%) Bulk 31.80 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

1.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (0.90 parts by weight), the selected sirasu balon (45.00 parts) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (19.30 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

50 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat sealer to prepare a solid pesticide formulation.

Formulation Example 7

Preparation of Polyethylene Premix Composition of Bensulfuron-Methyl (25%)

Low molecular weight polyethylene (6.00 parts) was melted with liquid paraffin (24.00 parts) at about 100 ° C. Bensulsulfuron-methyl bulk (25 parts by weight) was added to the molten mass with mixing. After the mass became nearly homogeneous, hydrophobic silica (41.00 parts) and talc (4.00 parts) were added slowly. After the addition, the mass was mixed at about 100 ° C. for 30 minutes and cooled to room temperature while mixing. After cooling, the product was triturated with an air mill.

Formulation Example 8

Pentrazamide (70%) Bulk 11.60 parts by weight

2.50 parts by weight of sodium dioctylsulfosuccinate

0.50 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.80 parts by weight), the selected sirasu balon (73.50 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (8.10 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 9

Pentrazamide (70%) Bulk 11.60 parts by weight

5.00 parts by weight of sodium dioctylsulfosuccinate

8.00 parts by weight of sodium lignin sulfonate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinyl alcohol (1.10 parts by weight), the selected sirasu balon (52.10 parts) was introduced into the pan coater and polyoxyethylene sorbitan trioleate (16.70 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 10

Preparation of Carnauba Wax Premix Composition of Bensulfuron-Methyl (25%)

Carnauba wax (40.00 parts) was melted at about 100 ° C. To the molten mass was added bensulfuron-methyl bulk (25.00 parts) by mixing. After the mass became nearly homogeneous, hydrophobic silica (31.00 parts) and talc (4.00 parts) were added slowly. After the addition, the mass was mixed at about 100 ° C. for 30 minutes and cooled to room temperature while mixing. After cooling, the product was triturated with an air mill.

Formulation Example 11

Pentrazamide (70%) Bulk 11.60 parts by weight

2.60 parts by weight of sodium dioctylsulfosuccinate

0.60 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of carnauba wax premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.40 parts by weight), the selected sirasu balon (65.00 parts) was introduced into the pan coater, and polyoxyethylene sorbitan monooleate (7.90 parts by weight) and polyethylene glycol (3.40 parts). Parts by weight) of the mixed solution was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 12

Pentrazamide (70%) Bulk 21.50 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

2.00 parts by weight of polyether modified silicone

3.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of carnauba wax premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinylpyrrolidone (1.40 parts by weight), the selected sirasu balon (45.70 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (18.90 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 13

Pentrazamide (70%) Bulk 11.60 parts by weight

2.60 parts by weight of sodium dioctylsulfosuccinate

0.60 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of carnauba wax premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.40 parts by weight), the selected sirasu balon (65.00 parts) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (11.30 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 14

Pentrazamide (70%) Bulk 11.60 parts by weight

3.00 parts by weight of sodium dioctylsulfosuccinate

2.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyethylene glycol (6.70 parts by weight), the selected sirasu balon (60.20 parts by weight) is introduced into the pan coater, and polyoxyethylene styryl phenyl ether (11.00 parts by weight) and polyoxyalkylene alkyl ether (3.70 parts by weight) of the mixed solution was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 15

Pentrazamide (70%) Bulk 11.60 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

4.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with carboxymethyl cellulose (1.30 parts by weight), the selected Sirasu balon (62.80 parts) was introduced into the pan coater and polyoxyethylene cured castor oil (12.80 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 16

Pentrazamide (70%) Bulk 11.60 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

4.00 parts by weight of sodium ligninsulfonate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.20 parts by weight), the selected sirasu balon (59.60 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (12.80 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 17

Pentrazamide (70%) Bulk 11.60 parts by weight

1.00 parts by weight of sodium dioctylsulfosuccinate

6.00 parts by weight of sodium ligninsulfonate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (6.30 parts by weight), the selected sirasu balon (57.60 parts) was introduced into the pan coater and polyoxyethylene sorbitan trioleate (12.00 parts) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 18

Mefenacet (85%) Bulk 31.80 parts by weight

2.50 parts by weight of sodium dioctylsulfosuccinate

2.50 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (0.70 parts by weight), the selected sirasu balon (36.00 parts) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (21.00 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 19

Pentrazamide (70%) Bulk 11.60 parts by weight

2.50 parts by weight of sodium dioctylsulfosuccinate

1.50 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.40 parts by weight), the selected sirasu balon (63.80 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (11.70 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 20

Preparation of Microcrystalline Wax Premix Composition of Bensulfuron-Methyl (25%)

Microcrystalline wax (35.00 parts) was melted at about 100 ° C. To the molten mass was added bensulfuron-methyl bulk (25.00 parts) by mixing. After the mass became nearly homogeneous, hydrophobic silica (35.00 parts) and talc (5.00 parts) were added slowly. After the addition, the mass was mixed at about 100 ° C. for 30 minutes and cooled to room temperature while mixing. After cooling, the product was triturated with an air mill.

Formulation Example 21

Pentrazamide (70%) Bulk 11.60 parts by weight

2.60 parts by weight of sodium dioctylsulfosuccinate

0.60 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of microcrystalline wax premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (6.80 parts by weight), the selected sirasu balon (61.60 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (11.30 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 22

Pentrazamide (70%) Bulk 4.30 parts by weight

3.00 parts by weight of sodium dioctylsulfosuccinate

2.00 parts by weight of acetylenediol

4.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of microcrystalline wax premix composition of bensulfuron-methyl (15%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinyl alcohol (2.10 parts by weight), the selected sirasu balon (68.70 parts by weight) was introduced into the pan coater and polyoxyethylene polycyclic phenyl ether (10.40 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 23

Pentrazamide (70%) Bulk 11.60 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

2.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

4.00 parts by weight of ammonium sulfate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyethylene glycol (3.00 parts by weight), the selected sirasu balon (58.70 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (9.60 parts by weight) and polyoxyalkylene alkyl A mixed solution of ether (4.10 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 24

Pentrazamide (70%) Bulk 11.60 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

4.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinyl alcohol (3.20 parts by weight), the selected sirasu balon (60.90 parts by weight) is introduced into the pan coater and the polyoxyethylene polyoxypropylene block polymer (8.90 parts by weight) and propylene glycol (3.90 parts) Parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Formulation Example 25

Pentrazamide (70%) Bulk 11.60 parts by weight

2.50 parts by weight of sodium dioctylsulfosuccinate

4.00 parts by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinyl alcohol (3.40 parts by weight), selected sirasu balon (64.60 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitol tristearate (11.40 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Formulation Example 26

Pentrazamide (70%) Bulk 11.60 parts by weight

3.00 parts by weight of sodium dioctylsulfosuccinate

0.60 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After pre-coating with polyvinyl alcohol (4.00 parts by weight), the selected Shirasu balon (63.80 parts by weight) was introduced into the pan coater and polyoxyethylene alkyl ether (11.50 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Comparative Example 1

Pentrazamide (70%) Bulk 11.60 parts by weight

2.00 parts by weight of sodium dioctylsulfosuccinate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.50 parts by weight), the selected sirasu balon (67.30 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (10.60 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Comparative Example 2

Pentrazamide (70%) Bulk 11.60 parts by weight

0.5 parts by weight of sodium dioctylsulfosuccinate

5.50 parts by weight of a polyethylene premix composition of bensulfuron-methyl (25%)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

After precoating with polyvinyl alcohol (3.40 parts by weight), the selected sirasu balon (60.40 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (9.80 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

Comparative Example 3

Pentrazamide (70%) Bulk 11.60 parts by weight

Sodium dioctylsulfosuccinate 0.50 parts by weight

0.50 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

Premixture composition of bensulfuron-methyl (10%) ^* 13.80 parts by weight

^* These and after benseol puron-dancin premix composition of methyl (10%) was prepared by mixing the following components and the mixture is pulverized by air mill:

Bensulfuron-Methyl Bulk 10.00 parts by weight

White Carbon 10.00 parts by weight

Calcium Carbonate 80.00 parts by weight

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

Selected Sirasu balon (51.60 parts) was introduced into the pan coater and polyoxyethylene sorbitol tetraoleate (22.00 parts) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

Comparative Example 4

Pentrazamide (70%) Bulk 11.60 parts by weight

1.00 parts by weight of sodium dioctylsulfosuccinate

0.50 part by weight of sodium salt of naphthalenesulfonic acid-formalin condensate

Premixture composition of bensulfuron-methyl (10%) ^* 13.80 parts by weight

(As described in Comparative Example 3)

The above mentioned ingredients were thoroughly mixed and ground to prepare a powder composition.

Selected Sirasu balon (50.70 parts by weight) was introduced into the pan coater and polyoxyethylene sorbitan monooleate (22.00 parts by weight) was added dropwise. After sufficient dispersion of the liquid, the above mentioned powder composition was slowly added to the pan coater. Thereafter, the pan coater was operated until the powder composition was uniformly coated on the shirasu balun to obtain the desired pesticide formulation.

40 g of the pesticide formulation was introduced into a bag (10 × 10 cm) made of a 40 μm thick water-soluble PVA (polyvinyl alcohol) film and sealed with a heat adhesive to prepare a solid pesticide formulation.

The pesticide preparation according to the invention was packaged in a polyvinyl alcohol (PVA) film and the pack was dropped directly into paddy water. After dropping of the formulation, the PVA quickly dissolves, the contents diffuse on the rice water, the active ingredients are distributed evenly in the rice water, and do not remain as particles, floating in the rice water. In order to confirm that the active ingredient is separated from the particle core and the active ingredient is distributed evenly in the rice paddy, diffusion and separability tests were performed according to the following method.

Test Example 1

Spreading and Separation Evaluation Test

As shown in FIG. 2, 14 Petri dishes, each about 9 cm in diameter and 1.8 cm in depth, were placed in a vinyl sheet pool 5 m long and 10 m wide. Water was poured into the Petri dish and the entire pool so that the depth was about 5 cm. Thereafter, 40 g of the formulation according to Formulation Example 1, packaged in a PVA film bag (10 × 10 cm), was gently dropped onto the water surface of the pool. After 1 hour, suspended particles were taken into a stainless steel net with a 425 μm mesh. The particles were dried on filter paper, and the amount of pesticide active ingredient (pentrazamide) was measured by HPLC method.

At the same time, the Petri dish was pulled out. The water in each petri dish was collected in a measuring flask, then the petri dish was washed with acetonitrile and the wash was also collected in a meslitsk. The measuring flask was filled with a predetermined volume of water, and the amount of the pesticide active ingredient in each petri dish was measured by HPLC method.

In addition, the diffusion and separability of the formulations of Formulation Examples 11, 16, 19 and 24, and Comparative Formulation Examples 1 and 3 were tested in the same manner. For this purpose, the amount of pesticide active ingredient (pentrazamide) in the suspended particles and the Petri dish was measured as mentioned above.

The test results are shown in Table 1 below.

For the formulations of Formulation Examples 1, 11, 16, 19 and 24, the average weight of the active ingredients exceeds about 150 μg, whereas for the formulations of Comparative Formulations 1 and 3, the average weight of the active ingredients Μg and about 110 μg. This means that the preparations according to the invention are much more soluble than the comparative preparations.

In addition, the active ingredient content in the suspended particles is about 20% for the formulations of Comparative Examples 1 and 3, which means that the active ingredient remains to a significant extent in the suspended particles. In contrast, for Formulation Examples 1, 11, 16, 19 and 24, the active ingredient content in the suspended particles is about 2%, which means that the active ingredient is separated from the suspended particles and hardly remains in the suspended particles.

Test Example 2

(Diffusion Evaluation Test in Model Field)

As shown in FIG. 3, water was filled in a 10 m long and 10 m wide vinyl sheet pool to a depth of about 5 cm. 40 g of the formulation according to Formulation Example 8, packaged in a PVA film bag (10 × 10 cm), were dropped into the pool at the designated points. The diffusion state was then investigated by measuring the time required for the granules to reach the point shown in FIG. Thereafter, the amounts of water presented from the points shown in FIG. 3 were collected at regular time intervals and the concentrations of pesticide active ingredients (pentrazamide and bensulfuron-methyl) were measured.

Diffusion was tested in the same manner for the formulations of Formulation Examples 13, 21 and 24, and Comparative Formulation Examples 1 and 4. for teeth,

The time at which the particles of each formulation reach the specified point and

The concentration of the active ingredient at the designated point was measured as described above.

The test results are shown in Tables 2 to 4 below.

Formulation example Particle arrival time 8 2 minutes 41 seconds 13 2 minutes 23 seconds 21 2 minutes 19 seconds 24 2 minutes 36 seconds Comparative Example 1 4 minutes 58 seconds Comparative Example 4 3 minutes 47 seconds

As can be seen from Table 2, the arrival times of the particles of Formulation Examples 8, 13, 21 and 24 are all within 2 minutes 30 seconds, indicating that the granules rapidly drift and spread on the water surface. In contrast, the arrival time of the particles of Comparative Examples 1 and 4 exceeded 3 minutes 30 seconds in both cases, indicating that the diffusion of the granules is slower than that of the granules according to the invention.

As can be seen from Tables 3a, 3b and 4a, 4b, for Formulation Examples 8, 13, 21 and 24, the desired concentrations of active ingredients in water (pentrazamide and bansulfuron-methyl, respectively) were reached quickly after formulation release. It became. Moreover, the concentration difference of the active ingredients (pentrazamide and bansulfuron-methyl) at the collection point was not large, indicating that the active ingredients were uniformly distributed.

Test Example 3

(Dissolution test)

Soil was poured into the pot (16 × 25 × 10 cm) at a height of 5 cm, and water was poured so that the water depth was 3 cm. 20 mg of each formulation of Formulation Examples 8, 16 and 25 and Comparative Formulation Example 3 were weighed and placed in one pot. After the preparation was dropped and a predetermined time interval was taken, a small amount of water was taken and the concentrations of the dissolved active ingredients (pentrazamide and bensulfuron-methyl) were measured by HPLC method.

The test results are shown in Tables 5 and 6, respectively.

Pentrazamide concentration (ppm) change Formulation example Hours 0.17 0.29 One 2 3 8 0.566 0.519 0.450 0.322 0.320 16 0.551 0.562 0.409 0.350 0.328 25 0.622 0.599 0.513 0.327 0.259 Comparative Example 3 0.278 0.305 0.298 0.316 0.307

Bensulfuron-methyl concentration (ppm) change Formulation example Hours 0.17 0.29 One 2 3 8 0.0461 0.0446 0.0468 0.0549 0.0523 16 0.0346 0.0395 0.0492 0.0553 0.0500 25 0.0412 0.0449 0.0547 0.0527 0.0549 Comparative Example 3 0.0853 0.0875 0.0785 0.0739 0.0676

As can be seen from Table 5, in the case of Comparative Example 3, the concentration of pentrazamide was 0.3 ppm after 1 day, whereas in Formulation Examples 8, 16, and 25, the pentrazamide dissolved very rapidly immediately after the dropping of the formulation. The concentration reached a value of 0.5 ppm or more.

As can be seen from Table 6, Bensulsulfuron-methyl dissolves very rapidly immediately after the dropping of the formulation in Comparative Example 3, reaching a concentration higher than 0.08 ppm, whereas for Formulation Examples 8, 16 and 25, Bensulfuron -Methyl dissolved slowly after delivery and reached a value of about 0.05 ppm after one day, indicating that dissolution was inhibited.

Test Example 4

(Herbicidal Effects on Paddy Weeds and Phytotoxicity on Transplanted Rice)

Weeds (bark, beech, large hulls, coriander and broadleaf weeds) were prepared by overcoming naturally growing rice fields and divided into 100 m 2 (10 × 10 cm) areas. The parent (variety: Nihonbare, 2.5 leaf stage, plant length: 15 cm) was transplanted with 3 roots per hill and kept 4 cm deep. When the weeds grew to the 1.5-leaf step, 40 g of the formulation prepared according to Formulation Example 13 and packaged in a water-soluble PVA film bag was dropped. The dispersion state of the preparation was visually observed.

The drop site is a point located 50 cm × 50 cm from the corner of the compartment (see FIG. 5).

Herbicidal effects and phytotoxicity against transplanted rice were examined at 2 and 3 weeks after preparation release.

The evaluation criteria are as follows: complete killing is represented by 100 and no effect is represented by 0. At least 90 herbicidal effects were evaluated as viable and less than 10 phytotoxicities were evaluated as viable.

The test was also performed in the same manner for Formulation Example 19 and Comparative Formulation Examples 2 and 3.

These results are shown in Tables 7 to 9 below.

Formulation example Dispersion State after Formulation 13 No sedimentation was observed at the point of discharge, dispersed throughout the rice field within 30 minutes 19 No sedimentation was observed at the point of discharge, dispersed throughout the rice field within 30 minutes Comparative Example 2 White precipitation observed near the point of release Comparative Example 3 White precipitation observed near the point of release

From the test results mentioned above, it can be seen that the diffusivity of the preparations according to the invention in the field is good, and in each application it is not necessary to evenly dispense the preparations into the waters of the formulation, and the preparations are applied near the rice fields. Pesticide actives can also be dispersed throughout the paddy field. In addition, the preparations according to the invention are capable of controlling the dissolution of the pesticide active ingredient. That is, in the case of the pesticide active ingredient slightly dissolved or easily dissolved in water, it is possible to suppress the dissolution and to promote dissolution in the case of the pesticide active ingredient which is poorly dissolved in water having low water solubility.

Brief description of Figures 2-4.

It is a figure which shows the place where the arrangement of a petri dish and the preparation were dropped in Test Example 1 (diffusion test).

In this figure, the symbols have the following meanings:

O = Petri dish placement point and serial number

X = point of release of the formulation

FIG. 3 is a diagram showing a point at which the preparation was dropped, a sample collection point, and a point where arrival of particles was observed in Test Example 2 (diffusion evaluation test in the discussion model).

In this figure, the symbols have the following meanings:

X = point of release of the formulation

O = collection point

Δ = point at which particle arrival is observed

Fig. 4 is a diagram showing a point at which a test agent (formulation) was dropped into paddy fields in Test Example 4 (herbicidal effect on paddy field and phytotoxicity on transplanted rice).

In this figure, the symbols have the following meanings:

X = point of release of the formulation

Claims (13)

A) solid core material of calcined pumice having an apparent specific density of less than 1 and a particle diameter of about 500 to about 1,400 μm, and B) a first coating layer comprising at least one water soluble polymer and At least one pesticide active compound having low water solubility, At least one dialkylsulfosuccinate salt, At least one other surfactant, At least one polyoxyethylene sorbitan (or sorbitol) fatty acid ester, and A second coating layer optionally comprising further additives, or C) a first coating layer comprising at least one water soluble polymer and At least one pesticide active compound having low water solubility, -At least one pesticide active compound that is slightly soluble or well soluble in water, At least one dialkylsulfosuccinate salt, At least one other surfactant, At least one polyoxyethylene sorbitan (or sorbitol) fatty acid ester, Wax or polyethylene, Hydrophobic silica, and A second coating layer optionally comprising further additives Agrochemical formulations in the form of solid particles. -At least one pesticide active compound that is slightly soluble or well soluble in water, -Waxes, Hydrophobic silica, and A pesticide premixture composition, characterized in that it optionally contains further additives. 3. The pesticide premix composition according to claim 2, which is in the form of granules. The pesticide preparation according to claim 1, which contains at least one pesticide active compound having a water solubility of less than 10 ppm at 20 ° C. The method of claim 1, wherein the mefenacet, pentrazamide, dimron, cumyluron, bromobutide, naproanilide, clomeprop, tenylchlor, esprocarb, pyributicab, cyhalopopbutyl, carca Phentrol, pyrazolate, pyrazoxifen, benzophenad, pyriminobac-methyl, butamifos, etobenzanide, bifenox, pentoate, pyridapention, chlorpyriphosmethyl, etofenprox, pi Pronyl, carbosulfan, benfuracarb, furathiocarb, cycloprotrin, buprofezin, bensultap, pencicuron, phthalide, flutolanyl, diclomazine, azoxystrobin, tifluzamide, capro A pesticide formulation characterized in that it contains at least one pesticide active compound selected from the group consisting of pamide, diclocimet and acibenzola-S-methyl. The polyoxyethylene sorbitan (or sorbitol) fatty acid ester according to claim 1, wherein the polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan Tristearate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan trioleate, polyoxyethylene sorbitan monoisostearate, polyoxyethylene sorbitan dioleate, polyoxyethylene sorbitol hexastearate, poly Agrochemical preparations comprising at least one compound selected from the group consisting of oxyethylene sorbitol tetrastearate, polyoxyethylene sorbitol tetraoleate, polyoxyethylene sorbitol monolaurate and polyoxyethylene sorbitol monooleate. The method of claim 1, wherein bensulfuron-methyl, pyrazosulfuron-ethyl, imazosulfuron, thifensulfuron-methyl, metsulfuron-methyl, plazasulfuron, halosulfuron, cynosulfuron, chlorsulfuron, azime Sulfuron, cyclosulfamine, 2,4-D, MCPB, cymetrin, dimethamethrin, thiobencarb, dimepiperate, molinate, butachlor, pretilachlor, piperophosph, benzlide, ben Furacetate, ventazone, ACN, imidacloprid, nitenpyram, tiacloprid, BPMC, isoprocarb, carbaryl, pention, disulfotone, diazinone, propaphos, dimethylbinforce, triadimefon, isoprothiolane Pesticide formulation, characterized in that it contains at least one pesticide active compound selected from the group consisting of furamepyr, probenazole and pyroquilon. The pesticide preparation according to claim 1, which contains calcined pumice having a particle diameter of about 500 to about 1,000 μm. According to claim 1, per 100 parts by weight of the formulation From about 0.05 to about 50 parts by weight of agrochemically active compounds having low water solubility, From about 0.9 to about 25 parts by weight of dialkylsulfosuccinate salt and other surfactants, About 1.0 to about 50 parts by weight of a polyoxyethylene sorbitan (or sorbitol) fatty acid ester, About 0 to about 50 parts by weight of other oily surfactant, About 0 to about 40 parts by weight of a water soluble extender, About 0.1 to about 30 parts by weight of a water soluble polymer and A pesticide preparation characterized by containing from about 10 to about 80 parts by weight of calcined pumice. The pesticide preparation according to claim 1, which is packaged in a water-soluble film. The pesticide preparation according to claim 1, which is packaged in a water-soluble film having a cutout portion. a) mixing at least one aqueous solution of water-soluble polymer with a solid core material of calcined pumice having an apparent secretion less than 1 and a particle diameter of about 500 to about 1,400 μm, and then drying the mixture, b) the obtained pre-treated material is subjected to at least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester and then At least one pesticide active compound having low water solubility, At least one dialkylsulfosuccinate salt, At least one other surfactant, and Optionally coated with a powder mixture containing further additives, or c) a powder mixture containing the pre-treated core material described in (a) above with at least one polyoxyethylene-sorbitan (or sorbitol) fatty acid ester and then the remaining ingredients described in (b) above and -At least one pesticide active compound that is slightly soluble or well soluble in water, Wax or polyethylene, Hydrophobic silica, and A process for preparing the pesticide preparation according to claim 1, characterized in that it is coated with a powder mixture, optionally containing further additives. A method of applying a pesticide to an argument water, characterized by applying the pesticide preparation according to claim 1 to an argument sleep.