JPH09235203A - Agricultural chemical powdery composition having enhanced effect and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a powdery composition containing a finely crushed water- hardly soluble solid agrochemical active component such a manner that the agrochemical activity is maximally manifested. SOLUTION: The objective powdery agrochemical composition is obtained by uniformly blending 1 pt.wt. of an aqueous fine particle suspension obtained by wet crushing a water-hardly soluble solid agrochemical active component e.g. tertiary butyl (E)-α-(1,3-dimethyl-5-phenoxypyrazol4-ylmethyleneaminooxy)- ptoluate} with >=0.1 pt.wt. of water-absorptive carriers (one or more than two kinds selected from among white carbon, diatomaceous earth and cellulose powder) and mineral fine powder. Preferably, an average particle size of the agrochemical active component in the aqueous fine particle suspension is <=5μm. The solid agrochemical component is preferably mixed in a content of, e.g. 1-50 pts.wt. of water-dispersion or 0.05-10 pt.wt. of powder in 100 pts.wt. of the agrochemical powdery composition.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a pesticidal powdery composition containing a finely pulverized water-insoluble solid pesticidal active ingredient,
For example, regarding powders or wettable powders and a simple method for producing them, in detail, it is possible to maximize the pesticidal activity by wet pulverizing a solid pesticidal active ingredient that is poorly soluble in water in an aqueous medium. The present invention relates to a pesticide powder composition made possible and a method for producing the same.

[0002]

2. Description of the Related Art Conventionally, powders or wettable powders are widely used formulations because they can be manufactured at low cost. However, pulverization of the pesticidal active ingredient is performed by a dry pulverization method, and pulverization of the pesticidal active ingredient having an average particle size of 5 μm or less is substantially impossible. Therefore, in the case of a preparation containing a solid pesticide active ingredient which is poorly soluble in water, it is the current situation that the effect cannot be sufficiently expressed. On the other hand, in solid preparations such as granules and wettable powder granules, attempts have been made to improve the effect by incorporating finely pulverized pesticide active ingredients. For example, a slurry of wet pulverized active ingredients is kneaded. And a method for producing a herbicide composition for paddy field having improved dissolution (Japanese Patent Laid-Open No. 5-17303). A method for producing a hydrated granular pesticide using a powder prepared by freeze-drying a wet-milled slurry of an active ingredient (JP-A-3-163005). Method for producing granule wettable powder by spray-drying slurry of wet-milled active ingredient (JP-A-62-212303)
Japanese Patent Laid-Open No. Sho 63-35503) and the like are disclosed.

The above-mentioned technique is for finely pulverizing the active ingredient by wet pulverization to a particle size substantially unattainable by dry pulverization so as to maximize its effect. The water contained in the wet pulverized slurry is removed in the drying step in the process. However, there is no drying step in the manufacturing process of dosage forms such as powders and wettable powders, and these techniques cannot be adopted. Also,
Although the technique of (1) removes water by freeze-drying, it is difficult to apply it to the production method of powders, wettable powders, etc., which has the advantage of low production cost. On the other hand, as another method, various additives such as a surfactant, an oil component, and a polymer compound are added to try to enhance the efficacy of powders and wettable powders. In some. However, these methods require selection of the optimum addition amount for each pesticide active ingredient, and further, there is no suitable additive for every pesticide active ingredient.

[0004]

As described above, when a solid pesticidal active ingredient that is poorly soluble in water is manufactured into a dosage form such as a powder or wettable powder, it is possible to exert its effect to the maximum extent. The development of an efficient manufacturing method has been strongly desired.

[0005]

Means for Solving the Problems As a result of intensive studies to solve the above-mentioned problems, the inventors of the present invention have obtained an aqueous fine particle suspension obtained by wet-grinding a solid agricultural chemical active ingredient that is poorly soluble in water in an aqueous medium. The present invention has found a pesticide powder composition obtained by uniformly mixing a water-absorbent carrier and a fine powder of a mineral substance, and a method for producing the same. That is, the present invention is that the biological activity of the pesticidal active ingredient is remarkably enhanced, and is an economically superior pesticide powder composition and a method for producing them, the present pesticide powder composition, for example, powder or It is used as a wettable powder.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION Examples of the solid pesticide component which is sparingly soluble in water according to the present invention include (1). Tertiary butyl (E) -α- (1,3-
Dimethyl-5-phenoxypyrazol-4-ylmethyleneaminoxy) -p-toluate (hereinafter referred to as compound a). (2). 2-tert-butylimino-3-isopropyl-5-phenyl-1,3,5-thiadiazin-4-
ON (hereinafter referred to as compound b). (3). N-tert-butyl-N '-(4-ethylbenzoyl) -3,5-dimethylbenzohydrazine (hereinafter referred to as compound c). (4). α, α, α-trifluoro-3′-isopropoxy-o-toluanilide (hereinafter referred to as compound d). (5). 5-amino-3-cyano-1- (2,6-dichloro-4-trifluoromethylphenyl) -4-trifluoromethylsulfinylpyrazole (hereinafter referred to as compound e
). (6). Methyl 2- (2- (4- (2-cyanophenoxy) pyrimidin-6-yloxy) phenyl) -2-
Methoxypropenoate (hereinafter referred to as compound f). (7). 4,5,6,7-Tetrachlorophthalide (hereinafter referred to as compound g). (8). Tetrachloroisophthalonitrile (hereinafter referred to as compound h). These solid agricultural chemical components can be added to 100 parts by weight of the agricultural chemical powder composition at a ratio of 1 to 50 parts by weight for a wettable powder and 0.05 to 10 parts by weight for a powder.

The water absorbing carrier may be an inorganic or organic powder substance having a high water absorbing ability, and examples thereof include white carbon, diatomaceous earth and cellulose powder. These may be used alone or as a mixture, and the addition amount of the water-absorbing carrier may be an amount such that the powder state is formed by absorbing the water in the aqueous fine particle suspension of the agrochemical active ingredient. The amount is preferably 0.1 part by weight or more, and particularly preferably 0.3 to 1.0 part by weight, relative to 1 part by weight of the fine particle suspension. As the fine mineral powder, in addition to commonly used clay, calcium carbonate, diatomaceous earth and the like, a fine powder of a carrier for agricultural chemicals can be used. As the formulation additive, an agricultural chemical formulation aid such as a surfactant, a stabilizer, a physical property improver or the like which is generally used for powders or wettable powders can be used.

An aqueous fine particle suspension prepared by wet pulverization of a solid pesticidal active ingredient which is poorly soluble in water can be prepared by the same production method as that for an ordinary pesticide aqueous suspension preparation, and a wetting agent, dispersant, stabilizer, Thickeners and other additives can be added as well. The pesticidal active ingredient in the aqueous fine particle suspension may be added in a proportion of 10 to 80 parts by weight. The method for producing a pesticidal powdered composition of the present invention may be a method in which each component is uniformly distributed in the composition, for example, an aqueous fine particle suspension obtained by wet pulverizing an agrochemical active ingredient into a water-absorbent carrier powder. A powder obtained by uniformly impregnating and mixing and pulverizing is used as a raw material to mix and homogenize mineral fine powder and other components with a conventional production method and a mixture of other components of the composition with an aqueous fine particle suspension of the agrochemical active ingredient. It can be manufactured by a manufacturing method in which it is added to a mixture of a water-absorbing carrier, mineral fine powder and other components and mixed and homogenized. The average particle size of the pesticidal active ingredient in the aqueous fine particle suspension can be adjusted to, for example, 5 μm or 0.5 by adjusting the grinding time.
The desired average particle size can be set to μm, 0.3 μm, or the like.

[0009]

EXAMPLES Examples of the agricultural chemical powder composition of the present invention are shown below, but the present invention is not limited thereto. still,
In Examples and Comparative Examples, “part” means “part by weight”. Embodiment 1 FIG. [Production of Premix of Compound c] Dioctyl sulfosuccinic acid sodium salt 0.70 parts, polyoxyethylene polystyryl phenyl ether 1.00 parts, ethylene glycol 6.25 parts, 1,2-benzisothiazoline-3
-ON 0.15 part, dimethylpolysiloxane 0.50
Parts and 19.4 parts of water were mixed and homogenized with a TK homomixer (made by Tokushu Kika Kogyo). Compound c (99
%) 21.0 parts and rosin glycerin ester 1.00 parts were added and further mixed, and wet-milled with Dynomill KDL (manufactured by Shinmaru Enter-Frises) to an average particle size of 3 μm. To this pulverized product was added 33.3 parts of hydrous silicic acid and mixed by a universal mixer (manufactured by Shinagawa Seisakusho), and then pulverized by a sample mill (manufactured by Hosokawa Micron) to give compound c of 25.2.
% Was obtained.

[Production of Dust of Compound c] 3.14 parts of premix of compound c, 0.15 of diisopropylphosphoric acid
Parts, 0.20 parts of polybutene, 1.00 parts of hydrous silicic acid, 30.3 parts of calcium carbonate and 65.51 parts of clay for DL (driftless) dusting agent were mixed with a universal mixer and then pulverized with a sample mill. D containing 0.75% of compound c
L powder was obtained.

Embodiment 2 FIG. 3.14 parts of premix of compound c of Example 1, 1.85 parts of compound b powder (85%),
Compound d powder (85%) 1.85 parts, diisopropylphosphoric acid 0.30 parts, polybutene 0.20 parts, hydrous silicic acid 2.00 parts, calcium carbonate 30.0 parts and DL powder clay 60.66 parts After mixing with a universal mixer, the mixture was ground with a sample mill to obtain a DL powder containing 0.75% of compound c, 1.5% of compound b and 1.5% of compound d.

Embodiment 3 FIG. [Production of Premix of Compound c] 1.40 parts of dioctylsulfosuccinic acid sodium salt, 1.00 parts of polyoxyethylene polystyryl phenyl ether, 6.25 parts of ethylene glycol, 1,2-benzisothiazoline-3
-ON 0.15 part, dimethylpolysiloxane 0.50
And 18.7 parts of water were mixed and homogenized with a TK homomixer. 21.0 parts of compound c (99%) and 1.00 parts of rosin glycerin ester were added thereto, and further mixed, and wet pulverized with Dynomill KDL to an average particle size of 0.5 μm. To this pulverized product was added 33.3 parts of hydrous silicic acid and mixed by a universal mixer (manufactured by Shinagawa Seisakusho), and then pulverized by a sample mill (manufactured by Hosokawa Micron) to give compound c 2
A premix containing 5.2% was obtained.

[Production of Powder of Compound c] 3.14 parts of premix of compound c, 0.15 of diisopropylphosphoric acid
Parts, polybutene 0.20 parts, hydrous silicic acid 1.00 parts, calcium carbonate 30.3 parts and DL powder clay 65.5
After 1 part was mixed with a universal mixer, it was ground with a sample mill to obtain a DL powder containing 0.75% of compound c.

Embodiment 4 FIG. 3.14 parts of premix of compound c of Example 3, 1.85 parts of compound b powder (85%),
Compound d powder (85%) 1.85 parts, diisopropylphosphoric acid 0.30 parts, polybutene 0.20 parts, hydrous silicic acid 2.00 parts, calcium carbonate 30.0 parts and DL powder clay 60.66 parts After mixing with a universal mixer, the mixture was ground with a sample mill to obtain a DL powder containing 0.75% of compound c, 1.5% of compound b and 1.5% of compound d.

Embodiment 5 FIG. [Production of Premix of Compound a] 4.00 parts of a mixture of dioctyl sulfosuccinic acid sodium salt, polyoxyethylene nonyl phenyl ether and polyoxyethylene polystyryl phenyl ether (Sorpol 3105, manufactured by Toho Kagaku), propylene glycol 10.0 parts , Dimethylpolysiloxane 0.10 part, and water 15.3 parts were mixed and homogenized with a TK homomixer, and compound a was added thereto.
(99%) 20.6 parts were added and further mixed, and wet pulverized with a Dynomill KDL to an average particle size of 3 μm. 33.3 parts of hydrous silicic acid was added to this crushed product and mixed by a universal mixer (manufactured by Shinagawa Kogyo Co., Ltd.), and then crushed by a sample mill (manufactured by Hosokawa Micron) and premix containing 24.5% of compound a. Got

[Production of Wettable Powder of Compound a] 20.5 parts of premix of compound a, 3.00 parts of polyoxyethylene nonylphenyl ether sulfate, 2.00 parts of naphthalene sulfonate formalin condensate, hydrous silicic acid 2.
After mixing 00 parts and 72.5 parts of the wettable powder clay with a universal mixer, the mixture was pulverized with a sample mill to give compound a of 5.0.
% Wettable powder was obtained.

Comparative Example 1. 1.32 parts of compound c powder (60%) prepared by dry pulverization to an average particle size of 12 μm, 0.15 part of diisopropylphosphoric acid, 0.20 part of polybutene, 30.0 parts of calcium carbonate and 68.33 clay for DL powder
The parts were mixed by a universal mixer and then pulverized by a sample mill to obtain a DL powder containing 0.75% of compound c.

Comparative Example 2. 1.32 parts of compound c powder (60%) prepared by dry pulverization to an average particle size of 12 μm, compound b
Powder (85%) 1.85 parts, Compound d powder (85%)
1.85 parts, diisopropyl phosphoric acid 0.30 parts, polybutene 0.20 parts, hydrous silicic acid 1.00 parts, calcium carbonate 30.0 parts, and DL powder clay 63.48 parts are mixed in a universal mixer. After that, it was pulverized with a sample mill to obtain a DL powder containing 0.75% of compound c, 1.5% of compound b and 1.5% of compound d.

Test Example 1 Twenty third-instar larvae of Cobbnomaiga were released in pot-planted rice and allowed to stand in a greenhouse and rolled for 4 days. DLs obtained in Examples and Test Examples were added to this pot.
The powder was treated with a bell jar duster in a prescribed amount, air-dried for 6 hours in a humidifier in a greenhouse, immediately subjected to artificial rain treatment, and then allowed to stand in a greenhouse. Five days after the treatment, the number of deaths, abnormalities, and surviving insects was investigated (two consecutive times). The results are shown in Table 1.

[0020]

[Table 1]

Test Example 2.1 A predetermined amount of DL powder obtained in Examples and Comparative Examples was applied to a paddy field divided into 70 m ² of ward using a power sprayer (pipe duster) at three different times. Sprayed. After 14 days from the treatment, the number of damaged strains of Cobbnomaiga and the number of damaged leaves of 100 strains per ward were counted for the top three leaves, and the control value was calculated. The results are shown in Table 2.

[0022]

[Table 2]

Test Example 3. D obtained in Examples and Comparative Examples
The physical properties and component stability of L powder were investigated. The results are shown in Table 3.

[0024]

[Table 3]

As shown in Table 1, Table 2 and Table 3,
The pesticide powder composition of the present invention had a better biological effect than the control formulation composition, and the physical properties of the pesticide powder composition were good, for example, within DL powder formulations.

Claims (9)

[Claims] 1. A pesticide powder composition comprising an aqueous fine particle suspension obtained by wet pulverizing a solid pesticidal active ingredient which is poorly soluble in water in an aqueous medium, a water-absorbing carrier and a fine powder of a mineral substance. 2. The pesticide powder composition according to claim 1, wherein the pesticidal active ingredient in the aqueous fine particle suspension has an average particle size of 5 μm or less. 3. The pesticide powder composition according to claim 1, wherein the water-absorbent carrier is one kind or two or more kinds selected from white carbon, diatomaceous earth or cellulose powder. 4. The pesticide powder composition according to claim 1, wherein the water-absorbent carrier is blended in an amount of 0.1 part by weight or more based on 1 part by weight of the aqueous fine particle suspension. 5. The pesticide powder composition according to claim 1, which is a powder or wettable powder. 6. A pesticide powdery composition, characterized in that a solid pesticidal active ingredient which is sparingly soluble in water is wet-ground in an aqueous medium to uniformly mix an aqueous fine particle suspension, a water-absorbing carrier and a fine powder of a mineral substance. Manufacturing method. 7. The method for producing a pesticidal powdery composition according to claim 6, wherein the pesticidal active ingredient in the aqueous fine particle suspension has an average particle size of 5 μm or less. 8. The method for producing an agricultural chemical powder composition according to claim 6, wherein the water-absorbent carrier is one or more selected from white carbon, diatomaceous earth, and cellulose powder. 9. The method for producing an agricultural chemical powder composition according to claim 6, wherein the water-absorbent carrier is added in an amount of 0.1 part by weight or more based on 1 part by weight of the aqueous fine particle suspension.