JP2002226302A - Silica carrier for agricultural formulation and agricultural formulation - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a solid formulation having excellent preservation stability of a fine powder and a granular wettable powder having excellent disintegrating properties due to high water dispersibility and slight occurrence of aggregation because the silica carrier has the characteristic values. SOLUTION: The silica carrier for the agricultural formulation is characterized in that the carrier is an amorphous silica having the definite pore peak of >=100 mm3/nm.g maximum dVp/dRp (wherein, Rp denotes the pore radius; Vp denotes the pore volume) and 1-20 nm pore peak radius.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a silica carrier for agricultural chemicals and an agricultural chemical.

[0002]

2. Description of the Related Art
In the field of agrochemical formulations, precipitated silica, a type of amorphous silica, has been widely used as a carrier. Its use is
It is used for various purposes, such as a grinding aid, a flow improver for a solid agent, and an adsorbent such as a solvent or a pesticide liquid raw material. As a dosage form, it is mainly used in a solid preparation, but it may also be used in a liquid preparation such as a case where a solid drug substance is pulverized dry and then converted into a liquid preparation. However, precipitated silica has no clear particle morphology and is bulky, so that the morphology of the particles is easily changed by external stimuli such as force and temperature, and the precipitated silica may be aggregated or solidified. As a result, for example, powdery preparations such as powders and wettable powders have the problems that the liquid components carried during storage are oozing out and solidification occurs due to excessive adhesion between precipitated silicas. Was. Furthermore, in the case of granular or tablet-like preparations such as granules, water dispersible granules, and surface application agents, if the content of precipitated silica is large, the granules cannot be molded due to clogging in the granulator or cannot be molded. Even so, the disintegration in water was very bad. Above all, in the case of a preparation intended to be dispersed in water, such as a water dispersible granule or a surface application agent, disintegration and dispersibility in water are important physical properties, and have good physical properties using precipitated silica. Formulation was difficult to make. The disadvantages of precipitated silica have increased, especially when the pesticidal drug substance is liquid, semi-solid or viscous.

In this case, it has been proposed to use such a calcined product of wet silica as a carrier (Patent No. 2).
966496) is still poor in dispersibility, and few of them have excellent physical properties as a carrier for agricultural chemicals to date,
Development of silica having good storage stability and water dispersibility of pesticides has been desired.

The present invention has been made to meet the above-mentioned demands, and has as its object to provide a silica carrier for agricultural chemicals and an agricultural chemical having extremely high storage stability and water dispersibility of agricultural chemicals.

[0005]

Means for Solving the Problems and Embodiments of the Invention The present inventors have conducted intensive studies in order to achieve the above object and found that dVp / dRp (where Rp is the pore radius and Vp is the pore volume. Has a clear pore peak of 100 mm ³ / nm · g or more, and has a pore peak radius of 1 to 20 nm.
The use of amorphous silica as a silica carrier for pesticide preparations provides an agrochemical preparation with improved consolidation after storage, excellent water dispersibility, and excellent uniform diffusion of active ingredients. It has been found that the present invention can be performed, and the present invention has been accomplished.

Hereinafter, the present invention will be described in more detail.
The silica carrier for agrochemical formulations of the present invention has a maximum dVp / dRp
Is an amorphous silica having a clear pore peak of 100 mm ³ / nm · g or more and a pore peak radius of 1 to 20 nm. Here, Rp indicates the pore radius and Vp indicates the pore volume.

In the present invention, the specific surface area, pore volume, pore distribution, and pore peak radius are values calculated by the nitrogen adsorption method, and more specifically, values calculated by the following method.

[Specific surface area] Using a fully automatic specific surface area / pore distribution measuring device (BELSORP28) manufactured by Bell Japan Co., Ltd., the adsorption isotherm of nitrogen gas was measured for a sample degassed under vacuum at 160 ° C. for 90 minutes. And calculated by the BET method (references: S. Brunauer, PH Emmett,
E. FIG. Teller, J.M. Amer. Chem. So
c. , 60 , 309 (1938)).

[Pore volume] A sample degassed under vacuum at 160 ° C. for 90 minutes was subjected to pore analysis by a Drillmore-Hill analysis method in accordance with JIS-K1150 from the nitrogen desorption isotherm measured by the aforementioned BELSORP28. Calculate the volume. The range of the pore radius for calculating the pore volume is 1 to 100 nm.

[Pore Distribution] The pore distribution of a sample degassed under vacuum at 160 ° C. for 90 minutes is determined from the nitrogen desorption isotherm measured by the aforementioned BELSORP28. The calculation of the pore distribution is performed by the method of Drillmore-Hill [D. Dolimore, G .;
R. Heal, J.M. Appl. Chem. , 14 . 10
9 (1964)].

[Pore Peak and Pore Peak Radius] From the pore distribution curve, the point where the maximum value of dVp / dRp is shown is defined as the pore peak, and the radius at the peak is defined as the pore peak radius.

In the silica of the present invention, the maximum dVp / d
Those having an Rp of less than 100 mm ³ / nm · g have the same structure and physical properties as ordinary precipitated silica, have high adhesion between silica particles, and have low water dispersibility. ³ / nm · g or more, preferably 1
00 to 500 mm ³ / nm · g, more preferably 100
２００200 mm ³ / nm · g, more preferably 120-1
It is 80 mm ³ / nm · g. The pore peak radius is 1 to 20 nm, preferably 8 to 15 nm, and more preferably 10 to 14 nm. As described above, the measurement range in this method is a pore peak of 1 nm or more, and a peak of 1 nm or less cannot be measured. If it exceeds 20 nm, the maximum dVp / dRp
Is very difficult to obtain silica of 100 mm ³ / nm · g or more. Further, if the pore peak radius is less than 8 nm, the oil absorption decreases, and the absorptivity of the pesticidal liquid raw material decreases. Those having a peak radius of 8 nm or more are preferred.

Further, the average particle size of the silica of the present invention may be pulverized in the preparation step and is not particularly limited, but is usually 1 μm or more, preferably 1 to 30 μm. Particles having a particle size of less than 1 μm are too fine and difficult to produce with ordinary pulverizing and classifying equipment. However, as described above, the average particle size does not matter if the agricultural chemical formulation equipment has a sufficient capacity.

When the silica used in the present invention is used for the purpose of absorbing a liquid or semi-solid material or a solvent as described above, it is preferable that the oil-absorbing ability is high.
Those having a P oil absorption of 150 mL / 100 g or more are preferred. The upper limit is not particularly limited, but is usually 500 mL /
It is 100 g, and even if it exceeds this, there is no particular problem.

The silica of the present invention has a specific surface area (nitrogen adsorption method) of 200 to 500 m ² / g, particularly 2 by the BET method.
It is preferably from 00 to 250 m ² / g.

The silica of the present invention can be obtained by a known method according to a method for producing a so-called wet silica, in which an aqueous solution of an alkali metal silicate such as sodium silicate is reacted with a mineral acid such as sulfuric acid or hydrochloric acid. .

The feature is that the concentration of silicic acid in the alkali metal silicate aqueous solution is 20 w / v% or less, preferably 10 w / v% or less.

As the silicate, sodium silicate No. 3 is often used from an economic viewpoint, but other silicates can also be produced. The mineral acid is not particularly limited, such as carbonic acid and phosphoric acid, but sulfuric acid and hydrochloric acid are often used from an economic viewpoint. The concentration of the mineral acid is preferably 6 to 16N.

As a specific production method, for example, the above-mentioned alkali metal silicate aqueous solution is heated and sulfuric acid of a predetermined concentration is added. The temperature of the aqueous alkali metal silicate solution when adding sulfuric acid is
The temperature is preferably 0 ° C or higher, and more preferably 50 to 100 ° C. If necessary, sulfuric acid may be added in several portions. The amount of sulfuric acid added is such that the final neutralization ratio is 70% or more, preferably 80 to 95%. If necessary, after the addition of sulfuric acid,
Heat it up. If crystals do not easily precipitate, a salt such as sodium sulfate may be mixed.

The pH at the end of the reaction is determined by the desired final pH.
However, it is preferable to lower the value to 5.5 or less.

The obtained silica slurry is filtered,
Wash and redisperse in water. At this time, the pH may be adjusted to the target value again. The target value can be freely adjusted from a weak acid to a weak base in accordance with the stability of the pesticidal active ingredient. Then, it is filtered, washed and dried to obtain coarse silica. Further, silica having a predetermined particle size is obtained by pulverization and classification.

When the above-mentioned silica is used as a pesticide carrier, the pesticide raw material and the present silica can be mixed and applied to all known and used dosage forms, and there is no particular limitation. Moreover, it can be used without any problem in the field where conventional precipitated silica is used. For example, fine powder preparations such as powders and wettable powders, granular preparations such as granules, powders and granules, wettable powders and solid preparations such as tablets, or homogeneous solutions such as liquids, oils, emulsifiers, and microemulsions And liquid preparations such as emulsified or suspended preparations such as liquid preparations, suspensions in water, suspensions in oil, emulsions in water, emulsions in oils, and microcapsules. Each preparation can be produced by a known composition and a known production method.

The types and constituents of commonly used pesticide preparations are summarized in Table 1 below. However, the present invention is not limited to these. Also, it is essential depending on the kind of pesticide active ingredient, the purpose of use of the preparation and the method of application. The components and the quasi-components used as needed may not always coincide with the values in the table, but are usually used within the following composition ranges. In addition, all% show weight%.

[0024]

[Table 1]

Further, in addition to these, from the application surface, there may be mentioned, for example, air-dispersing agents (liquid preparations, solid preparations), water-applied preparations (granular preparations, tablets, liquid preparations, etc.), seed treatment agents, box treatment agents and the like. However, these are names given from the application side and are basically classified into the dosage forms listed above, and the content of the active ingredient in the preparation can be adjusted according to the purpose, and among the surface application agents, the water surface In the case of an agent, an extender having a specific gravity of 1 or less is contained depending on the form of the liquid agent / solid agent. In addition, acid blue and rhodamine B are used as seed treatment agents so that the adhesion of the agent is easy to understand.
And the like.

Regardless of the type of preparation, colorants such as acid blue and rhodamine B, antioxidants and light absorbers, HALS, a mixture of mono- and diisopropyl phosphate, alkali metal borate and alkali Stabilizers such as pH adjusters such as earth metal borate, mineral oil,
Oils such as isoparaffin oil, silicone oil and vegetable oil,
It is also possible to add a spreading agent obtained by adding various surfactants thereto, and an efficacy enhancer comprising various surfactants such as a silicone-based surfactant and a quaternary ammonium-based surfactant.

The use of the silica in various dosage forms is not particularly limited, and is usually used for the following purposes. However, the component name is often treated simply as a solid carrier.

For example, in the case of a solid preparation, the pesticidal drug substance is solid or used as an auxiliary of other solid components, for example, as a grinding aid, a fluidity improver, a dust explosion reducer, etc.
When the pesticidal drug substance is liquid or semi-solid, or when the formulation contains a solvent or the like, it is used, for example, as an adsorbent for the drug substance or solvent. In the case of a liquid preparation, for example, as a viscosity modifier, or as a fluidity improver for a solid component to be mixed, or when the solid component is mixed after being pulverized, for example, a grinding aid or a fluidity improver It is used as an agent and a dust explosion reducing agent.

The following are examples of the above-mentioned components, but are not limited thereto.

As the pesticidal active ingredient, its physical properties may be any of solid, liquid and semi-solid, and its application is, for example, insecticide, acaricide, fungicide, herbicide,
Examples include plant growth regulators and insect growth regulators, but are not limited thereto. For example, the following compounds can be mentioned, and one or a mixture of two or more isomers such as geometric isomers and optical isomers can also be mentioned.

O, O-dimethyl O- (3-methyl-4-
Nitrophenyl) phosphorothioate, O, O-dimethyl O- (3-methyl-4- (methylthio) phenyl) phosphorothioate, O, O-diethyl O-2-isopropyl-6-methylpyrimidin-4-yl phosphorothioate, O, O -Diethyl O-3,5,6-trichloro-
2-pyridyl phosphorothioate, O, S-dimethylacetyl phosphoramidothioate, S-2,3-dihydro-5-methoxy-2-oxo-1,3,4-thiadiazol-3-ylmethyl O, O-dimethyl phosphoro Dithioate, O, O-diethyl S-2-ethylthioethyl phosphorodithioate, 2,2-dichlorovinyldimethyl phosphate, O-ethyl O-4- (methylthio) phenyl S-propyl phosphorodithioate, O- 4-cyanophenyl O, O-dimethyl phosphorothioate, 2-
Methoxy-4H-1,3,2-benzodioxaphosphorin-2-sulfide, O, O-dimethyl S- (N-methylcarbamoylmethyl) dithiophosphate, ethyl 2
-Dimethoxyphosphinothioylthio (phenyl) acetate, diethyl (dimethoxyphosphinothioylthio) succinate, dimethyl 2,2,2-trichloro-
1-hydroxyethylphosphonate, S-3,4-dihydro-4-oxo-1,2,3-benzotriazine-3
-Ylmethyl O, O-dimethyl phosphorodithioate,
Dimethyl-{(E) -1-methyl-2- (methylcarbamoyl) vinyl} phosphate, O, O, O ', O'-
Organic phosphorus compounds such as tetraethyl-S, S'-methylenebis (phosphorodithioate) and O-2,6-dichloro-4-methylphenyl O, O-dimethylphosphorothioate;

2-sec-butylphenylmethylcarbamate, ethyl N- {2,3-dihydro-2,2-dimethylbenzofuran-7-yloxycarbonyl (methyl) aminothio} -N-isopropyl-β-alaninate, Isopropoxyphenyl-N-methylcarbamate, 2,3-dihydro-2,2-dimethyl-7-benzo [b] furanyl N-dibutylaminothio-N-methylcarbamate, 1-naphthyl-N-methylcarbamate, S- Methyl-N- (methylcarbamoyloxy) thioacetimidate, 2- (ethylthiomethyl) phenylmethylcarbamate, 2-methyl-2- (methylthio) propionaldehyde O-methylcarbamoyloxime, N, N-dimethyl-2- Methylcarbamoyloxyimino-2- (methyl E) acetamide, S-4-
Carbamate compounds such as phenoxybutyl-N, N-dimethylthiocarbamate;

2- (4-ethoxyphenyl) -2-methyl-1- (3-phenoxybenzyl) oxypropane,
(RS) -α-cyano-3-phenoxybenzyl (R
S) -2- (4-chlorophenyl) -3-methylbutyrate, (S) -α-cyano-3-phenoxybenzyl (S) -2- (4-chlorophenyl) -3-methylbutyrate, (RS) -Α-cyano-3-phenoxybenzyl 2,2,3,3-tetramethylcyclopropanecarboxylate, (RS) -α-cyano-3-phenoxybenzyl (1RS) -cis, trans-3- (2,2 −
Dichlorovinyl) -2,2-dimethylcyclopropanecarboxylate, 3-phenoxybenzyl (1RS)-
Cis, trans-3- (2,2-dichlorovinyl)-
2,2-dimethylcyclopropane carboxylate,
(RS) -α-cyano-3-phenoxybenzyl (1
RS, 3Z) -cis-3- (2-chloro-3,3,3-
(Trifluoroprop-1-enyl) -2,2-dimethylcyclopropanecarboxylate, (S) -α-cyano-3-phenoxybenzyl (1R) -cis-3-
(2,2-dibromovinyl) -2,2-dimethylcyclopropanecarboxylate, (RS) -α-cyano-3
-Phenoxybenzyl (RS) -2,2-dichloro-
1- (4-ethoxyphenyl) cyclopropanecarboxylate, α-cyano-3-phenoxybenzyl N-
(2-chloro-α, α, α-trifluoro-p-tolyl) -D-valinate, 2-methyl-3-phenylbenzyl (1RS, 3Z) -cis-3- (2-chloro-
3,3,3-trifluoro-1-propenyl) -2,2
-Dimethylcyclopropanecarboxylate, 2- (4
-Bromodifluoromethoxyphenyl) -2-methyl-
1- (3-phenoxybenzyl) methylpropane,
(S) -α-cyano-3-phenoxybenzyl (1
R) -cis-3- (1,2,2,2-tetrabromoethyl) -2,2-dimethylcyclopropanecarboxylate, (4-ethoxyphenyl)-{3- (4-fluoro-3-phenoxyphenyl) ) Propyl｝ dimethylsilane, 3-phenoxybenzyl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (RS) -α-
Cyano-3-phenoxybenzyl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, 5-benzyl-3-furylmethyl (1R) -cis, Transformer
2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (S) -α-cyano-3-phenoxybenzyl (1R, 3Z) -cis- (2,2-dimethyl-3) -｛3-oxo-3- (1,
1,1,3,3,3-hexafluoropropyloxy)
Propenyl @ cyclopropanecarboxylate, (R
S) -α-Cyano-4-fluoro-3-phenoxybenzyl 3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropanecarboxylate, 2,3,5,6
-Tetrafluoro-4-methylbenzyl (1RS, 3
Z) -cis-3- (2-chloro-3,3,3-trifluoro-1-propenyl) -2,2-dimethylcyclopropanecarboxylate, 2,3,5,6-tetrafluorobenzyl (1R) -Trans-3- (2,2-dichlorovinyl) -2,2-dimethylcyclopropanecarboxylate, 3,4,5,6-tetrahydrophthalimidomethyl (1RS) -cis, trans-2,2-dimethyl-3 -(2-methyl-1-propenyl) cyclopropanecarboxylate, (RS) -2-methyl-4-oxo-3- (2-propenyl) -2-cyclopentene-
1-yl (1RS) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (S) -2-methyl-4-oxo-3- ( 2-propynyl) -2-cyclopentene-1
-Yl (1R) -cis, trans-2,2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, (RS) -1-ethynyl-2-methyl-2-pentenyl ( 1R) -cis, trans-2,
2-dimethyl-3- (2-methyl-1-propenyl) cyclopropanecarboxylate, 2,5-dioxo-3
-(2-propynyl) imidazolidin-1-ylmethyl (1R) -cis, trans-2,2-dimethyl-3-
(2-methyl-1-propenyl) cyclopropanecarboxylate, 5- (2-propynyl) furfuryl (1
R) -cis, trans-2,2-dimethyl-3- (2-
Methyl-1-propenyl) cyclopropanecarboxylate, 5- (2-propynyl) furfuryl 2,2,3
Pyrethroid compounds such as 3-tetramethylcyclopropanecarboxylate, N-phosphonomethylglycine and its pharmaceutically acceptable salts, phosphorylates such as 4-hydroxymethylphosphinoyl-L-homoalanyl-L-alanine Tidoaminoacid compounds,

3-Isopropyl-1H-2,1,3-benzothiadiazin-4 (3H) -one 2,2-dioxide, 2-tert-butylimino-3-isopropyl-5-phenyl-1,3 , Thiadiazine derivatives such as, 5-thiadiazin-4-one, nitroimidazolidine derivatives, S, S '-(2-dimethylaminotrimethylene) bis (thiocarbamate), N, N-dimethyl-1,2,2
Nereistoxin derivatives such as 3-trithian-5-ylamine, S, S'-2-dimethylaminotrimethylene di (benzenethiosulfonate), N-cyano-N'-
N-cyanoamidine derivatives such as methyl-N '-(6-chloro-3-pyridylmethyl) acetamidine;
8,9,10,10-hexachloro-1,5,5a,
6,9,9a-hexahydro-6,9-methano-2,
4,3-benzodioxathiepine oxide, 1,2,2
3,4,5,6-hexachlorocyclohexane, 1,1
Chlorinated hydrocarbon compounds such as -bis (4-chlorophenyl) -2,2,2-trichloroethanol, 1- {3,5
-Dichloro-4- (3-chloro-5-trifluoromethylpyridin-2-yloxy) phenyl} -3- (2,
6-difluorobenzoyl) urea, 1- (3,5-dichloro-2,4-difluorophenyl) -3- (2,6
Benzoylphenylurea-based compounds such as -difluorobenzoyl) urea and 1- {4- (2-chloro-4-trifluoromethylphenoxy) -2-fluorophenyl} -3- (2,6-difluorobenzoyl) urea;
N, N '-{(methylimino) dimethylidine} -di-
Formamidine derivatives such as 2,4-xylidine, N '-(4-chloro-2-methylphenyl) -N, N-dimethylmethinimidamide, N- (2,6-diisopropyl-4
Thiourea derivatives such as -phenoxyphenyl) -N'-t-butylcarbodiimide, N-phenylpyrazole compounds,

5-methoxy-3- (2-methoxyphenyl) -1,3,4-oxadiazole-2- (3H)-
On, isopropyl 4,4'-dibromobenzylate,
4-chlorophenyl 2,4,5-trichlorophenylsulfone, S, S-6-methylquinoxaline-2,3-
Diyldithiocarbonate, 2- (4-tert-butylphenoxy) cyclohexylprop-2-ylsulfite, bis {tris (2-methyl-2-phenylpropyl) tin} oxide, (4RS, 5RS) -5
(4-chlorophenyl) -N-chlorohexyl-4-methyl-2-oxo-1,3-thiazolidine-3-carboxamide, 3,6-bis (2-chlorophenyl) -1,
2,4,5-tetrazine, 2-tert-butyl-5-
(4-tert-butylbenzylthio) -4-chloropyridazin-3 (2H) -one, tert-butyl
(E) -4-[(1,3-Dimethyl-5-phenoxypyrazol-4-yl) methyleneaminooxymethyl] benzoate, N-4-tert-butylbenzyl) -4
-Chloro-3-ethyl-1-methyl-5-pyrazolecarboxamide, tetranactin, dinactin, trinactin, 5-chloro-N- [2- {4- (2-ethoxyethyl) -2,3-dimethylphenoxy} ethyl] -6
Ethylpyrimidin-4-amine], milbemectin, abamectin, ivermectin, azadirachtin [AZA
D], 5-methyl [1,2,4] triazolo [3,4-
b] benzothiazole, methyl 1- (butylcarbamoyl) benzimidazole-2-carbamate, 6-
(3,5-dichloro-4-methylphenyl) -3 (2
H) -Pyridazinone, 1- (4-chlorophenoxy)-
3,3-dimethyl-1- (1H-1,2,4-triazol-1-yl) butanone, (E) -4-chloro-2-
(Trifluoromethyl) -N- [1- (imidazole-
1-yl) -2-propoxyethylidene] aniline, 1
-[N-propyl-N- [2- (2,4,6-trichlorophenoxy) ethyl] carbamoyl] imidazole,
(E) -1- (4-chlorophenyl) -4,4-dimethyl-2- (1H-1,2,4-triazol-1-yl) -1-penten-3-ol, 1- (4-chlorophenyl ) -4,4-Dimethyl-2- (1H-1,2,4
-Triazol-1-yl) pentan-3-ol,
(E) -1- (2,4-dichlorophenyl) -4,4-
Dimethyl-2- (1H-1,2,4-triazole-1
-Yl) -1-penten-3-ol, 1- (2,4-
Dichlorophenyl) -4,4-dimethyl-2- (1H-
1,2,4-triazol-1-yl) pentane-3-
All, 4- [3- (4-tert-butylphenyl)
-2-methylpropyl] -2,6-dimethylmorpholine, 2- (2,4-dichlorophenyl) -1- (1H-
1,2,4-triazol-1-yl) hexane-2-
All, O, O-diethyl O-2-quinoxalinyl phosphorothioate, O- (6-ethoxy-2-ethyl-
4-pyrimidinyl) O, O-dimethyl phosphorothioate, 2-diethylamino-5,6-dimethylpyrimidin-4-yl dimethylcarbamate, 4- (2,4
-Dichlorobenzoyl) -1,3-dimethyl-5-pyrazolyl p-toluenesulfonate, 4-amino-6-
(1,1-dimethylethyl) -3-methylthio-1,
2,4-triazin-5 (4H) -one, 2-chloro-
N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl) aminocarbonyl] benzenesulfonamide, 2-methoxycarbonyl-N-[(4,6-
Dimethoxypyrimidin-2-yl) aminocarbonyl]
Benzenesulfonamide, 2-methoxycarbonyl-N
-[(4,6-dimethylpyrimidin-2-yl) aminocarbonyl] benzenesulfonamide, 2-methoxycarbonyl-N-[(4-methoxy-6-methyl-1,
3,5-triazin-2-yl) aminocarbonyl] benzenesulfonamide, 2-ethoxycarbonyl-N-
[(4-chloro-6-methoxypyrimidin-2-yl)
Aminocarbonyl] benzenesulfonamide, 2- (2
-Chloroethoxy) -N-[(4-methoxy-6-methyl-1,3,5-triazin-2-yl) aminocarbonyl] benzenesulfonamide, 2-methoxycarbonyl-N-[(4,6-dimethoxy Pyrimidin-2-yl) aminocarbonyl] phenylmethanesulfonamide, 2-methoxycarbonyl-N-[(4-methoxy-
6-methyl-1,3,5-triazin-2-yl) aminocarbonyl] thiophen-3-sulfonamide, 4-
Ethoxycarbonyl-N-[(4,6-dimethoxypyrimidin-2-yl) aminocarbonyl] -1-methylpyrazole-5-sulfonamide, 2- [4,5-dihydro-4-methyl-4- (1- Methylethyl) -5-oxo-1H-imidazol-2-yl] -3-quinolinecarboxylic acid, 5-ethyl-5,8-dihydro-8-oxo [1,3] dioxolo [4,5-g] quinoline -7-carboxylic acid, 2- [4,5-dihydro-4-methyl-4-
(1-Methylethyl) -5-oxo-1H-imidazol-2-yl] -5-ethyl-3-pyridinecarboxylic acid, methyl 6- (4-isopropyl-4-methyl-5)
-Oxoimidazolin-2-yl) -m-toluate,
Methyl 2- (4-isopropyl-4-methyl-5-oxoimidazolin-2-yl) -p-toluate, 2-
(4-Isopropyl-4-methyl-5-oxoimidazolin-2-yl) nicotinic acid, N- (4-chlorophenyl) methyl-N-cyclopentyl-N'-phenylurea, (RS) -2-cyano-N- [(R) -1 (2,4
-Dichlorophenyl) ethyl] -3,3-dimethylbutylamide, N- (1,3-dihydro-1,1,3-trimethylisobenzofuran-4-yl) -5-chloro-
1,3-dimethylpyrazole-4-carboxamide,
N- [2,6-dibromo-4- (trifluoromethoxy) phenyl] -2-methyl-4- (trifluoromethyl) -5-thiazol-carboxamide, 2,2-dichloro-N- [1- (4-chlorophenyl) ethyl] -3
-Methylcyclopropanecarboxamide, methyl (E) -2-6- (2-cyanophenoxy) pyrimidin-4-yloxy-phenyl-3-methoxyacrylate, 5-methyl-1,2,4-triazolo [ 3,4
-B] benzothiazole, 3-allyloxy-1,2-
Benzoisothiazole-1,1-dioxide, diisopropyl = 1,3-dithiolan-2-ylidene-malonate, O, O-dipropyl O-4-methylthiophenyl phosphate and the like.

The content of the pesticidal active ingredient varies depending on the dilution ratio of the preparation and the form of application, and also varies depending on the form of the preparation, and is not particularly limited, but is usually as described above.

Examples of the surfactant include a nonionic surfactant, an anionic surfactant, a cationic surfactant, an amphoteric surfactant, and a mixture thereof. Usually, nonionic and / or anionic surfactants are used. Specific examples of the nonionic surfactant include, for example, polyoxyethylene carboxylate, polyoxyethylene polyoxypropylene alkylaryl ether, polyoxyethylene polyoxypropylene block copolymer, polyvinyl alcohol, maleic anhydride and diisobutylene. Copolymer, polyvinylpyrrolidone, polyoxyethylene polystyrene block copolymer, polyoxyethylene alkylaryl ether, polyoxyethylene alkyl ether, polyoxyethylene polyoxypropylene tristyryl phenyl ether, polyoxyethylene styryl phenyl ether, polyoxy Ethylene tristyryl phenyl ether, polyoxyethylene fatty acid ester, fatty acid ester, polyhydric alcohol fatty acid ester, polyoxy Ethylene polyhydric alcohol fatty acid ester, may be mentioned polyoxyethylene alkylamines, specifically as the anionic surfactants, such as dialkyl sulfo carboxylic acid esters, alkyl aryl sulfonate,
Alkyl sulfonate, sulfosuccinate, higher fatty acid alkali salt, polycarboxylate, polyoxyethylene alkyl ether phosphate, polyoxyethylene alkyl aryl ether phosphate, polyoxyethylene tristyryl phenyl ether phosphate, Alkyl naphthalene sulfonate, formalin condensate of alkyl naphthalene sulfonate, metal salt of naphthalene sulfonic acid polycondensate, alkenyl sulfonate,
Examples thereof include dialkyl succil sulfonate and lignin sulfonate. Surfactant alone or 2
A mixture of more than one species can be used. The content in the pesticidal composition is not particularly limited by the formulation dilution ratio and spray form, and is also not particularly limited by various formulation forms.
As described above.

Examples of the solvent include aromatic solvents, polar solvents, animal and vegetable oils and the like. Solvents include paraffinic solvents, aromatic solvents, polar solvents, animal and vegetable oils,
Various waxes and the like can be mentioned. As the paraffin solvent, normal paraffin, isoparaffin,
Cycloparaffin, liquid paraffin and the like can be mentioned. Examples of the aromatic solvent include xylene, alkylbenzene, alkylnaphthalene, phenylxylylethane, diphenylxylylethane, and the like, and examples of the polar solvent include cyclohexanone, heptanone, octanone, nonanone, N-methyl 2-pyrrolidone, Ketones such as acetophenone, hexyl acetate, benzyl acetate, phenylethyl acetate, benzyl benzoate, methyl benzoate, isobutyl oleate, benzyl salicylate, butyl cyclohexyl acetate, methyl benzyl acetate, methyl oleate, methyl laurate, and 2 to 4 ethylene groups Mono- or di-alkylene dicarboxylic acids such as dibasic acid esters, diisodecyl phthalate, dioctyl phthalate, diisodecyl adipate, diisobutyl adipate and isobutyl adipate Esters such as Le, ethylene glycol, propylene glycol, benzyl alcohol, phenylethyl alcohol, butyl cyclohexanol,
Alcohols such as phenyloxyethanol can be mentioned, and animal and vegetable oils include rapeseed oil, soybean oil, linseed oil and the like. Furthermore, higher fatty acids and esters of higher fatty acids can be mentioned.

The solvents can be used alone or as a mixture of two or more. Irrespective of the dosage form, those having a high flash point are usually good, preferably at least 60 ° C, more preferably at least 100 ° C. The combination and content of the solvent varies depending on the dosage form and the purpose of the content, but depending on the purpose such as handleability during production, prevention of crystal precipitation during storage at low temperature, enhancement of efficacy, handleability during spraying of the formulation such as viscosity control, etc. It can be determined as appropriate.

The content of the solvent in the preparation varies depending on the dilution ratio of the preparation and the form of application, and also varies depending on the form of the preparation, but is not particularly limited, but is usually as described above.

As the thickener, there are those used in oil and those used in water. As those used in oil, for example, BENTONE SD-1 (trade name of RHEOX Corporation), BENTONE SD-2 (trade name of RHEOX Corporation), BENTONE SD-3 (RHEOX Corporation)
X Corporation), BENTONE 34 (RHE
OX Corporation), BENTONE 38 (R
HEOX Co., Ltd.), THIXATROL
ST (trade name of RHEOX Corporation), THIXATR
OL SR / 100 (trade name of RHEOX Corporation),
THIXATROL289 (trade name of RHEOX Corporation), THIXCIN R (trade name of RHEOX Corporation), THIXATROL 53X (company RHEO)
Organic clays such as X), organic bentonite, and organic montmorillonite.

Examples of those used in water include water-soluble polymers such as polyoxyalkylene, polyvinyl alcohol, sodium polycarboxylate carboxymethylcellulose, hydroxyethylcellulose, methylcellulose and derivatives thereof, xanthan gum, welan gum, guar gum, tragacanth gum, sodium alginate and the like. Biogum, magnesium aluminum silicate and the like. The content in these preparations varies depending on the dilution ratio of the preparation and the form of application, and also varies depending on the form of the preparation, and is not particularly limited, but is usually as described above.

As the defoaming agent, for example, TSF 451
(Toshiba Silicone Co., Ltd.), TSA720 (Toshiba Silicone Co., Ltd.), YSA02 (Toshiba Silicone Co., Ltd.), antifoam C
(Trade name of Dow Corning), Antifoam CE
(Trade name of Dow Corning), TSA730 (trade name of Toshiba Silicone Co.), TSA731 (trade name of Toshiba Silicone Co., Ltd.), TSA732 (trade name of Toshiba Silicone Co., Ltd.), YMA6509 (trade name of Toshiba Silicone Co., Ltd.)
And water-dispersible silicone-based defoamers, and fluoro-based compounds such as perfluoroalkylphosphoric acid.

The content of the antifoaming agent in the preparation varies depending on the dilution ratio of the preparation and the form of application, and also varies depending on the form of the preparation, and is not particularly limited, but is usually as described above.

Examples of the antifreeze include glycols such as propylene glycol, polypropylene glycol, ethylene glycol and diethylene glycol. The content of the antifreezing agent in the preparation varies depending on the dilution ratio of the preparation and the form of application, and also varies depending on the form of the preparation, and is not particularly limited, but is usually as described above.

Examples of the solid carrier include mineral substances and inorganic fine powders used in ordinary agricultural chemical solid preparations. Specific examples include clay, diatomaceous earth, talc, calcium carbonate, ammonium sulfate, bentonite, and zeolite. Acid clay, activated clay, attapulgite, ammonium sulfate, sodium sulfate, potassium chloride, urea, synthetic hydrous silicon oxide, carboxymethyl cellulose, and the like. Also, starch, dextrin, lactose,
Sugars such as sucrose, wood flour, walnut shells, corn cobs,
Organic fine powder such as powdered cellulose is exemplified.

In particular, when a liquid component such as a liquid base or a solvent is contained, an oil-absorbing solid carrier such as synthetic hydrous silicon oxide, attapulgite, bentonite, or zeolite, especially wet silica is used as the oil-absorbing agent. Is preferred.
The content of the solid carrier in the preparation varies depending on the dilution ratio of the preparation and the form of application, and also varies depending on the form of the preparation, and is not particularly limited, but is usually as described above.

Examples of the auxiliary agent include a fluidity and dispersibility improver, or an active ingredient stabilizer. Specific examples include metal salts of higher fatty acids, tall oil fatty acids, calcium stearate, alkyl phosphate derivatives, alkali metal borates and alkaline earth metal borates. The content of the auxiliary in the preparation is usually 70% by weight or less, preferably 30% by weight or less, more preferably 10% by weight or less.

When the composition is an oil, it can be obtained, for example, by mixing the pesticide raw material and a solvent or, if necessary, further adding a solvent, a surfactant, a viscosity modifier and the like. As the solvent and the surfactant, those described above can be used. As the viscosity modifier, for example, a high-viscosity solvent such as animal or vegetable oils or liquid paraffin, or a thickener usable in oil is used. The content of each component in the preparation varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.

When the present composition is a liquid preparation, for example, a pesticide drug substance having a water solubility higher than the dilution ratio and water or a water-soluble solvent, and if necessary, a surfactant or a stabilizing agent as a solubilizing agent. , A coloring agent, an antifoaming agent, etc., and can be produced in the same manner as for the oil agent. As the solvent and the surfactant, those described above can be used. In particular, in the case of a liquid preparation, a water-soluble coloring agent is often mixed so that it can be identified even after dilution with water.
The content of each component in the preparation varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.

When the present composition is an emulsion, it can be obtained, for example, by dissolving the present compound in a mixture comprising a solvent, a surfactant and the like. As the surfactant and the solvent, one or a mixture of two or more of those exemplified above can be mentioned, and the content thereof is not particularly limited in various ways depending on the formulation dilution ratio and spraying form, but usually, As described above.

When the present composition is an oil-in-suspension type formulation, for example, a mixture obtained by adding an auxiliary agent such as a surfactant, a thickener and a solvent, if necessary, to a pesticidal active ingredient is mixed with glass beads, zirconia. And the like, and obtained by pulverizing and dispersing using a wet pulverization technique using a medium such as In addition, a mixture of a pesticide bulk material and a surfactant, if necessary, an oil-absorbing agent, a grinding aid, a thickener, a defoaming agent, a solvent, etc., is preliminarily pulverized by a dry pulverization method such as a hammer mill or an air mill. It can also be obtained by uniformly dispersing the compound. The thickener can be prepared, for example, by adding a thickener or a solvent dispersion thereof during wet pulverization dispersion or after pulverization dispersion, and mixing while heating as necessary.

As the solvent, the solvents exemplified above can be mentioned. Usually, the solubility of the pesticidal drug substance is preferably 1% or less. For example, a solvent such as paraffin oil or vegetable oil is often selected. Usually, these solvents often have high viscosity, and aromatic or ester-based solvents may be mixed for the purpose of adjusting the viscosity or lowering the consolidation point. The solvent can be appropriately selected from the above solvents. The content of the solvent in the preparation varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.

Examples of the thickener include the thickeners used in the above-mentioned oils. The content of the thickener is not particularly limited in various ways depending on the dilution ratio of the preparation and the form of spraying. , As described above.

Examples of the surfactant include the surfactants exemplified above, and the content thereof is not particularly limited in various ways depending on the dilution ratio of the preparation and the form of spraying. is there. Examples of the defoaming agent include those exemplified above, and among them, oil type and solid type are preferred. The content in the formulation is not particularly limited in various ways depending on the formulation dilution ratio and spraying form,
Usually, as described above.

When the present composition is a water-suspended preparation, for example, a surfactant, a thickener, water, an antifoaming agent, and an antifreezing agent are added to a water-insoluble solid pesticide as needed. The mixture is obtained by pulverizing and dispersing the mixture using a wet pulverization technique using a medium such as glass beads or zirconia. In addition, the mixture of the pesticide active ingredient and the surfactant, if necessary, a grinding aid such as wet silica, a thickener, a defoaming agent, an antifreezing agent, etc., is previously prepared by a dry grinding method such as a hammer mill or an air mill. It can also be obtained by uniformly dispersing the pulverized compound. The thickener can be prepared, for example, by adding a thickener or an aqueous dispersion thereof at the time of wet pulverization dispersion or after pulverization dispersion, and mixing while heating as necessary.

In some cases, a solvent may be supported on an oil-absorbing agent such as wet silica or the like and mixed. Examples of the solvent include the solvents exemplified above. Examples of the thickener include the thickeners used in water exemplified above. Examples of the surfactant include the surfactants exemplified above. Examples of the defoaming agent include those exemplified above, and among them, an aqueous dispersion type is preferable. Examples of the antifreeze include the above-mentioned glycols. The content is various and not particularly defined depending on the dilution ratio of the preparation and the form of application, but is usually as described above.

When the present composition is an aqueous emulsion preparation, for example, a solution obtained by dissolving a pesticidal solid drug substance in a hydrophobic solvent, or a solution of a pesticide liquid drug substance and / or a hydrophobic solvent,
And a surfactant are dispersed in water, and if necessary, an antifreezing agent, a thickener, an antifoaming agent and the like are added. Alternatively, it can be obtained by dispersing a water-soluble pesticidal active ingredient, a hydrophobic solvent and a surfactant in water with a stirrer such as a homogenizer, and adding an antifreezing agent or a thickener as necessary. Examples of the surfactant include the surfactants exemplified above. Among them, water-soluble polymers such as polyvinyl alcohol and polyoxyethylene polyoxypropylene block polymer are preferred.

Examples of the solvent include the above-mentioned aromatic solvents and insoluble polar solvents.
0% by weight or less, preferably 50% by weight or less, more preferably 30% by weight or less. Examples of the antifreeze include the above-mentioned glycols.

Examples of the thickener include those used in the aforementioned water, and examples of the antifoaming agent include the aforementioned water-dispersed type antifoaming agents.

The contents of these are various and not particularly limited depending on the dilution ratio of the preparation and the form of spraying.
As described above.

When the present composition is a suspoemulsion preparation, for example, as a suspended solid component,
Examples include water-insoluble solid components such as grinding aids, surfactants and potency enhancers, and as emulsified liquid ingredients, pesticide liquid raw materials, hydrophobic solvents and potency enhancers, hydrophobic specific gravity regulators And the like. As a method for producing the preparation,
A mixture of the water-insoluble solid component, the surfactant, and water,
An emulsion prepared by preparing a suspension that has been pulverized and dispersed using a method of wet pulverization using media such as glass beads and zirconia, and adding a liquid component and a surfactant, and dispersing the suspension with a stirrer such as a homogenizer. Is prepared by mixing the suspension and the emulsion, and if necessary, adding and mixing a thickener, an antifreezing agent, an antifoaming agent and the like. In addition, a liquid component and a surfactant are added, and an emulsion is prepared by dispersing with a stirrer such as a homogenizer, and a solid component previously ground by a dry grinding method such as a hammer mill or an air mill, and a thickener as necessary. , An antifreezing agent, an antifoaming agent and the like can be added to the emulsion and uniformly dispersed. These components are the same as those exemplified for the aqueous live suspension preparation and the emulsion preparation in water, and the content thereof is not particularly limited in various ways depending on the dilution ratio of the preparation and the spraying form, but is usually as described above. It is.

When the present composition is a microemulsion preparation, it can be produced, for example, by uniformly mixing a pesticide raw material, a solvent, and a surfactant, adding water with stirring, and subjecting the mixture to a phase inversion method. This aqueous solution can be obtained by adding and mixing a thickener, an antifreezing agent, an antifoaming agent and the like as necessary. These components are the same as those exemplified for the aqueous suspension preparation and the emulsion preparation in water. Furthermore, since it is a transparent aqueous solution as in the case of a liquid preparation, a water-soluble coloring agent is often used for identification. The content of each of these components varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.

When the present composition is a microcapsule preparation,
It can be produced by the same method as that for producing a water-in-water emulsion preparation or a water-in-suspension preparation, except that it is encapsulated after preparing a suspension or emulsified state. Some examples of the encapsulation method include an interfacial polymerization method, an emulsion polymerization method, a suspension polymerization method, an in-situ method, a curing-in-liquid coating method, a phase separation method, and a drying method in liquid. Generally, an interfacial polymerization method is often employed for production reasons. In this case, as a polymerizable monomer, a hydrophobic compound containing an isocyanate group and water, urea, an amino group such as glycols, or a hydroxyl group are used. The contained water-soluble compound is used. Examples of the solvent, thickener, antifreezing agent, and antifoaming agent used in the present preparation can be the same as those of the above-mentioned aqueous emulsion preparation, and the content thereof is usually as described above.

When the present composition is a powder, for example, the aforementioned solid carrier is mixed with the pesticidal drug substance, and if necessary, the above-mentioned solvent, stabilizer, colorant, surfactant, fluidity improver, drift An auxiliary agent such as an inhibitor and an efficacy enhancer is added, and the mixture is pulverized by a hammer mill, a Nara-type pulverizer, an air mill (such as a jet O miser) or the like. These components can be the same as those described above, and the content thereof is not particularly limited in various ways depending on the dilution ratio of the preparation and the form of application, but is usually as described above.

As the anti-drift agent, a highly viscous solvent such as machine oil or a liquid surfactant is generally used.

When the present composition is a water solvent, for example, a pesticide drug substance having a water solubility higher than the dilution ratio and a water-soluble solid carrier such as saccharides, inorganic salts and organic acid salts, and if necessary, a solvent such as a solvent or It can be manufactured by mixing a surfactant, a stabilizer, a colorant, a fluidity improver, an efficacy enhancer, an antifoaming agent, and the like, and pulverizing and mixing in the same manner as for a powder. The solvent used as a dissolution aid is preferably a water-soluble solvent. However, when it is dissolved in water in combination with a surfactant, the solvent itself may be a hydrophobic solvent.

The content of each of these components is not particularly limited in various ways depending on the dilution ratio of the preparation and the form of application, but is usually as described above.

When the composition is a wettable powder, for example, a solid carrier is mixed with the pesticidal active ingredient and a surfactant, and if necessary, the above-mentioned solvent, stabilizer, coloring agent, surfactant, Auxiliary agents such as a property improving agent, an efficacy enhancer, and an antifoaming agent are added, and the mixture is pulverized by a hammer mill, a Nara-type pulverizer, or an air mill (such as a jet O miser), and then mixed to produce a product.

When the pesticidal drug substance is liquid or contains a solvent, it preferably contains an oil-absorbing solid carrier such as wet silica. The content of each component in the preparation varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.

When the present composition is a granular preparation of granules or wettable granules, it can be produced, for example, by a method of granulation or a method of impregnating granules. Specific examples of the method by granulation include a fluidized bed granulation method, a spray drying granulation method, an extrusion granulation method, a tumbling granulation method, and a compression granulation method.

For example, the fluidized-bed granulation method is used to prepare a powder consisting of a pulverized agricultural chemical solid and / or an agricultural chemical liquid which has been solidified by an oil-absorbing agent and a solid carrier, or By spraying an aqueous solution or dispersion containing a binding agent, if necessary, onto a powder added with a surfactant, a solvent, a lubricant, an antifoaming agent, etc., to agglomerate the powder particles, and to remove water after granulation. It is a method of manufacturing by drying. Incidentally, as a method of adding the liquid composition, for example, in addition to the method of adding at the time of preparing the powder,
It is also possible to obtain a granular material by granulation and drying according to the above-mentioned method, or to spray-mix a solvent to the granular material.

The spray-drying granulation method includes, for example, a pulverized agricultural chemical solid and / or an agricultural chemical liquid which has been solidified by an oil absorbing agent, if necessary, a solid carrier, a solvent, a surfactant,
An aqueous solution or dispersion containing a binder, a lubricant, an antifoaming agent,
This is a method of granulating by spraying in hot air and simultaneously drying moisture. In addition, as a method of adding the liquid composition,
For example, in addition to the above-described method of adding the powder at the time of preparing the powder before spray drying, it is also possible to produce a granular material containing no liquid composition by the method and then spray the granular composition with the liquid composition.

In the extrusion granulation, a powder consisting of a pulverized agricultural chemical solid and / or an agrochemical liquid raw material solidified by an oil absorbing agent and a solid carrier or, if necessary, a solvent and an interface. Activator, lubricant, powder to which the antifoaming agent is added, after adding water or an aqueous solution containing a binder, and kneading, extruding the kneaded material with a screen, crushing to an appropriate length, After drying the water with a drier, granulate. In this method, the liquid composition may be manufactured by mixing with water or an aqueous solution containing a binder instead of mixing with the powder. Further, the liquid composition can be spray-mixed to a granulated product obtained by granulating without adding the liquid composition.

As the solid carrier, for example, in the case of the spray-drying granulation method, it is not always necessary. However, in general, the solid carriers exemplified in the above powders are used, and one or more of them can be used. The content in the preparation varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.

Examples of the surfactant include the surfactants exemplified above, and one or more of them may be used. In granules and wettable powders, the content in the preparation varies depending on the dilution ratio of the preparation and the form of application, but is not particularly limited, but is usually as described above.
However, when producing a wettable powder by a spray-drying granulation method, the content in the preparation is usually 0.1 to 95% by weight.

Examples of the binder include carboxymethylcellulose, methylcellulose, polyvinyl alcohol, polyvinylpyrrolidone, dextrin, soluble starch, and ligninsulfonate. In some cases, such as when bentonite is used as the solid carrier, it is unnecessary, but it is usually as described above.

Examples of the solvent and the defoaming agent include the solvents exemplified above.

Examples of the lubricant include a wax-like substance, a highly viscous oil equivalent to a lubricating oil, and an oil-absorbing agent such as silica. As the waxy substance, capric acid, lauric acid, stearic acid,
Fatty acids usually having 10 or more carbon atoms such as oleic acid, calcium stearate, magnesium stearate, sodium stearate, zinc stearate, aluminum stearate, metal salts of fatty acids such as barium stearate,
Powdered paraffin, various waxes, and liquid substances include fatty acids having usually 6 to 9 carbon atoms such as caproic acid, caprylic acid, and pelargonic acid; higher alcohols such as oleyl alcohol and stearyl alcohol; liquid paraffin; naphthenes; and silicone oils. And liquid substances such as derivatives thereof.

In the case of dry granulation, a powder consisting of a pulverized agricultural chemical solid and / or an agricultural chemical liquid which has been solidified by an oil absorbing agent and a solid carrier or, if necessary, a solvent and Powder obtained by adding a surfactant, a lubricant, a binder, and an antifoaming agent is compression-molded by a roller compactor or the like, and then crushed and sieved. In this case, sugars such as lactose are often used as the solid carrier.

In the case of a water dispersible granule, a disintegrant may be further contained as necessary. Examples of the disintegrant include carboxymethylcellulose calcium, a crosslinked product of polyvinylpyrrolidone, a substance which swells in water such as xanthan gum, or, in the case of dry granulated products, a mixture of a solid acid such as maleic anhydride and a carbonate such as sodium hydrogen carbonate. Which react in water to generate and release carbon dioxide.
The content in these preparations varies depending on the preparation dilution ratio and spraying form, and is not particularly limited, but is usually as described above.

The method of impregnating the granules is as follows.
Pulverized pumice, pulverized bentonite, pulverized vermiculite, pulverized pearlite, various kinds of calcined particles, etc. on porous granular carriers, for example, solutions or suspensions prepared from pesticide raw materials and solvents, and if necessary, further surface activity It can be produced by supporting a solution prepared by adding an agent or a coating agent. Further, in the case of granules and wettable powders, a granular preparation can also be prepared by supporting a solution or suspension prepared from an agricultural chemical base and a solvent on a granular carrier granulated by various granulation methods. . The granular carrier is usually contained in the preparation in an amount of 30 to 95% by weight. The content of the solvent is about 50% by weight.

In the case of producing a tablet, a powder consisting of a ground pesticide solid and / or a liquid pesticide solidified by an oil absorbing agent and a solid carrier, or if necessary, a surfactant, Mixing agent, solvent, binder, disintegrant, etc.
It is formed into a predetermined size and shape with a tableting machine. Examples of the solid carrier include those described above, and saccharides such as lactose are often used. The other components are almost the same as the above-mentioned granules, and the content in the preparation is not particularly limited in various ways depending on the preparation dilution ratio and the spray form, but usually,
As described above.

The present composition formulated in various forms is used for controlling pests, controlling plant growth, and the like. Applicable land can be applied not only to agricultural land such as rice fields, but also to orchards, pastures, lawns, forestry or waterways, canals or other non-agricultural land. When spraying the composition,
Weather conditions, formulation, treatment time, treatment method, soil conditions,
Although it may vary depending on the target crop and the target weed, the application method may be any form that is sprayed with ordinary pesticides. For example, there can be mentioned a method of spraying directly on a field or a non-agricultural land, a seedling box, or the like, or a method of diluting with water and then applying it to a crop or soil with a sprayer or the like. The dilution ratio in water depends on the type and content of the pesticidal active ingredient in this drug, the type of target pest, and the application scene, but is usually 10 to 10.
About 10,000 times, preferably about 50 to 8000 times,
More preferably, it is about 500 to 4000 times.

Examples of the sprayer method include ground spraying such as a shoulder sprayer and a boom sprayer, and air spraying such as a radio-controlled helicopter, a helicopter and a Cessna.

As the packaging form of the present preparation, a container that can be used for ordinary agricultural chemical preparations can be used. For example, in the case of a liquid agent, a plastic bottle, a tin can, an iron can, a chemi-drum, a single can, a lorry and the like coated in a single layer or multiple layers can be mentioned, and in the case of a solid agent, an aluminum bag, a paper bag, a paper pack, a water-soluble Films and the like. In order to avoid moisture absorption during storage, an aluminum bag, a paper bag whose interior is coated with aluminum, a plastic bag, or the like is preferable. In addition, by filling those packed in a water-soluble pack into these bags, prevention of moisture absorption during storage, improvement in safety, improvement in usability during dilution, and the like can be expected.

The preparation may further contain, if necessary, other herbicides, insecticides, acaricides, nematicides, fungicides, plant growth regulators, insect growth regulators, fertilizers, soil conditioners, synergists. Agent,
It may contain an adjuvant or the like.

[0088]

According to the present invention, since the silica carrier has the above characteristic values, it is highly dispersible in water and hardly aggregates. It is possible to provide a water dispersible granule having excellent properties.

[0089]

EXAMPLES The present invention will be described below in detail with reference to examples and comparative examples, but the present invention is not limited to the following examples.

Example 1 100 L of an aqueous solution of sodium silicate No. 3 having a silicic acid concentration of 5 w / v% was heated to 95 ° C., and 2.5 L of 12N sulfuric acid was added with stirring.
Next, the mixture was stirred for 30 minutes, and 2.2 L of 12 N sulfuric acid was added. Heat for an additional 30 minutes. After adjusting the pH to 4.0, the slurry was filtered, washed and redispersed in water. pH
Was adjusted to 4.0, the slurry was filtered, washed, dried, pulverized, and classified to obtain silica having a predetermined particle size.

Example 2 100 L of an aqueous solution of sodium silicate No. 3 having a silicic acid concentration of 5 w / v% was heated to 95 ° C., and 2.5 L of 12 N sulfuric acid was added with stirring.
Next, the mixture was stirred for 30 minutes, and 2.2 L of 12 N sulfuric acid was added. Heat for an additional 30 minutes. After adjusting the pH to 7.0, the slurry was filtered, washed and redispersed in water. pH
Was adjusted to 8.5, the slurry was filtered, washed, dried, pulverized, and classified to obtain silica having a predetermined particle size.

Comparative Example 1 100 L of an aqueous solution of sodium silicate No. 3 having a silicic acid concentration of 7 w / v% was heated to 90 ° C., and 2.7 L of sulfuric acid having a 12N concentration was added with stirring.
Next, the mixture was stirred for 30 minutes, and 3.9 L of 12 N sulfuric acid was added. Heat for an additional 30 minutes. Filter this slurry,
Washed and redispersed in water. The slurry was filtered, washed, dried, pulverized, and classified to obtain silica having a predetermined particle size.

Comparative Example 2 The silica obtained in Comparative Example 1 was heat-treated at 900 ° C. for 1 hour to obtain a calcined product of wet silica. Table 1 shows the physical properties of the silica obtained above. In addition, the physical property measuring method is as follows. FIG. 1 shows a pore distribution curve.

[Average Particle Size] The particle size distribution was measured with a Coulter Counter MS-II type particle size analyzer manufactured by Beckman Coulter KK using an aperture of 100 μm or 30 μm, and the median diameter (50% particle size) was measured. The average particle diameter was used.

[Pore distribution] A nitrogen adsorption isotherm at a liquid nitrogen temperature was determined using a fully automatic gas adsorption apparatus BELSORP28 manufactured by Japan Bell Co., Ltd., and the obtained desorption isotherm was obtained in accordance with JIS-K1150. The pore distribution (Rp vs. dVp / dRp) was determined by applying the Drillmore-Heel analysis method to The sample was pretreated at 160 ° C. for 90 minutes.

[Pore Peak Radius] This is the pore radius indicating the maximum value of dVp / dRp obtained from the pore distribution diagram of each sample shown in FIG.

[Oil Absorption] Using an automatic oil absorption measurement device manufactured by Frontex Co., Ltd., the oil absorption per 100 g of silica with respect to dibutyl phthalate (DBP) oil was taken as the oil absorption.

[0098]

[Table 2]

Next, a wettable powder with the formulation shown in Table 3 was prepared using the above silica.

[0100]

[Table 3]

After the silica and the liquid raw material were previously mixed in a mortar, they were pulverized and mixed. Thereafter, a surfactant and clay were added and mixed. Water was added so as to have an appropriate water content, and this was granulated by extrusion granulation with a net diameter of 0.8 mm, and the length of the grains was adjusted, followed by drying at 60 ° C. for 45 minutes.
The mixture was sieved with sieves having a net diameter of 1180 μm and 800 μm to remove coarse and fine particles.

The obtained water dispersible granules were measured for disintegration in water, self-diffusion and dispersibility by the following methods. Table 4 shows the results.

[0103] 1.0 g of the prepared granules was added to a Nessler tube containing 50 mL of water-disintegrable 3rd degree hard water, and the mixture was turned upside down. The number of inversions required before the particles disappeared was defined as the disintegration in water.

Self-diffusion property In the measurement of disintegration in water, one or two granules were placed in hard water three times, and the disintegration of the grains when they reached the bottom of the tube was visually judged.

Dispersibility After the measurement of disintegration in water, the completely dispersed liquid is allowed to stand for 10 minutes. The settled volume was defined as dispersibility.

[0106]

[Table 4]

From the above results, the silica according to the present invention was used in comparison with Comparative Example 1 using the conventional precipitated silica and Comparative Example 2 using the calcined product of wet silica which is considered to have good dispersibility. It can be seen that Examples 1 and 2 had very good disintegration and dispersibility in water. Therefore, it can be seen that by using the silica of the present invention, which is a gel type silica, as a carrier for an agricultural chemical liquid bulk material, a disintegrable wettable powder with good disintegration that cannot be obtained with conventional precipitated silica and calcined silica can be obtained. Was.

[Brief description of the drawings]

FIG. 1 is a pore distribution curve of silica of Examples and Comparative Examples.

 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Shugo Nishi 1125 Kariya, Ako-shi, Hyogo Prefecture Shionogi Pharmaceutical Co., Ltd. BC07 BC18 BC19 BC20 DA02 DA15 DG16 DH03

Claims (4)

[Claims] 1. An amorphous silica having a maximum dVp / dR
p (where Rp is the pore radius and Vp is the pore volume) has a distinct pore peak of 100 mm ³ / nm · g or more, and the pore peak radius is 1 to 20 nm. Silica carrier for agricultural chemicals. 2. A pesticide preparation containing the silica carrier according to claim 1. 3. A pesticidal solid preparation containing the silica carrier according to claim 1. A water dispersible agricultural chemical granule containing the silica carrier according to claim 1.