JP2003095803A - Aqueous suspension germicide composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an aqueous suspension germicide composition having good suspensibility of a solid component after diluting the formulation with water, good handling property and effectiveness and not causing phytotoxicity. SOLUTION: This aqueous suspension germicide composition comprises (a) 1-50 wt.% sterilization active component which has <=500 ppm water solubility and is solid at ordinary temperature and (b) 1-10 wt.% polyoxyalkylene polystyrylphenyl ether phosphoric acid ester salt. In the germicide composition, a volume fraction of >=10 μm average particle diameter in the solid component is <=25%.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to an aqueous suspension fungicide composition.

[0002]

2. Description of the Related Art Hitherto, as a means for controlling various pathogenic fungi against plants, a method has been used in which a preparation containing a bactericidal active ingredient is diluted to a predetermined concentration and then sprayed on a field with a sprayer. Further, in this means, an aqueous suspension preparation in which an active ingredient is finely pulverized in the presence of a dispersant and suspended in water, a so-called flowable preparation, is widely used.

By the way, when studying the formulation of such a flowable preparation, the particle size of the active ingredient and the selection of the surfactant influence the efficacy and the physical properties of the preparation, which is particularly important.
In addition, a flowable formulation is generally diluted with a predetermined amount of water before use, but most pesticide raw materials have a specific gravity of 1 or more, and the dispersion stability (suspendability) of the diluted solution of the formulation is high. ) Is an important requirement when used in real situations.

[0004]

An object of the present invention is to provide an excellent aqueous suspension bactericide which has good suspension of solid components after preparation water dilution, good handleability, is also effective in efficacy and does not cause phytotoxicity. To provide a composition.

[0005]

Under such circumstances, as a result of extensive studies, a specific dispersant was added to an aqueous suspension bactericidal composition containing a solid bactericidal active ingredient having a water solubility of 500 ppm or less at room temperature. A composition in which the content range of the bactericidal active ingredient and the dispersant is specified and the particle size range of the solid component is specified has extremely stable properties, and thus the conventional problems described above can be solved. This led to the present invention. That is, according to the present invention, (a) the water solubility is 500 p
1 to 50% by weight of a bactericidal active ingredient (hereinafter referred to as the present active ingredient) which is solid at room temperature of pm or less and (b) polyoxyalkylene polystyrylphenyl ether phosphate ester salt (hereinafter referred to as the present dispersant). ) 1 to 10% by weight of an aqueous suspension bactericidal composition, wherein the volume fraction of solid particles having an average particle size of 10 μm or more is 25% or less (hereinafter referred to as “the present invention”). The composition will be referred to as a composition).

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION As the polyoxyalkylene polystyrylphenol phosphate ester salt contained in the present composition, polyoxyethylene tristyrylphenol phosphate ester salt is preferable, and among them, its potassium salt and triethanolamine salt. Is particularly preferable in terms of physical properties of the preparation. Its content in the composition is 1 to 10% by weight, preferably 2 to 7% by weight.

This active ingredient has a water solubility of 500 pp at room temperature.
As long as it is a solid bactericidal active ingredient of m or less and does not contain any other water-insoluble solid ingredient, the solid ingredient in the present composition substantially consists of the present active ingredient. Examples of the active ingredient include benzimidazole compounds such as benomyl, carbendazim, thiabendazole, and thiophanatemethyl; phenylcarbamate compounds such as dietofencarb; dicarboximide compounds such as procymidone, iprodione, vinclozolin; diniconazole, epoxyconazole, tebuconazole. , Azole compounds such as difenoconazole, cyproconazole, flusilazole, triadimefone; acylalanine compounds such as metalaxyl; carboxamide compounds such as flametopyr, mepronil, furtranil, trifluzamide; amide compounds such as diclosimet; tolclofos-methyl, Organic phosphorus compounds such as pyrazophos; Anilinopyrimidine compounds such as pyrimesanil, mepanipyrim, cyprodinil Compound; fludioxonil, cyanopyrrole compounds such as fenpiclonil; antibiotics such as polyoxins; azoxystrobin, kresoxim-methyl, S
Methoxy acrylate compounds such as SF-126; chlorothalonil, manzeb, captan, folpet, oxine copper, basic copper chloride, probenazole, fusalide, dimethomorph, famoxadone, oxolinic acid, fluazinam, ferrimzone and the like can be mentioned. Among them, procymidone and diclocymet are particularly preferable in order to exert the performance of this agent.

If necessary, other active ingredients and auxiliary agents such as a thickener, an antifreezing agent, an antiseptic, an antifoaming agent, a spreading agent, a stabilizer, etc., as long as the physical properties of the composition are not impaired. May be contained.

Examples of thickeners include natural polysaccharides such as xanthan gum and locust bean gum, mineral substances such as magnesium aluminum silicate and bentonite, and semisynthetic polysaccharides such as sodium carboxymethyl cellulose.
Examples thereof include synthetic water-soluble polymers such as polyacrylic acid salts, and two or more kinds of these may be mixed and used. Although its content varies depending on the type of thickener, it is usually 0.01 to 10% by weight with respect to the present composition.

Examples of the antifreezing agent include propylene glycol, ethylene glycol, diethylene glycol and the like, and the content thereof varies depending on the kind, but is usually 0.1 to 20% by weight relative to the present composition. Examples of the preservatives include isothiazolone-based preservatives such as 5-chloro-2-methyl-4-isothiazolin-3-one, and examples of the defoaming agent include silicone-based defoaming agents.

In addition, when applied in actual situations, preparations containing other active ingredients, for example, bactericidal preparations, insecticidal preparations, herbicidal preparations, fertilizer preparations, etc. are mixed and applied within a range not impairing the characteristics of the composition. May be.

The present composition can be produced, for example, by the following method. In this composition, the average particle size in the solid component is 10 μm.
It is necessary to manufacture such that the proportion of m or more is 25% or less, and various crushing equipment can be used for that purpose. In the case of dry crushing, a ball mill, a centrifugal crusher, a jet mill, a mortar or the like can be used. Further, in the case of wet pulverization, a bead mill, high speed disperser or the like can be used. By adjusting the crushing time while measuring the particle size of the crushed particles with, for example, a Coulter counter or the like, the ratio of the target solid components having an average particle size of 10 μm or more can be 25% or less.

In the case of dry pulverization, the present active ingredient is finely pulverized by the above pulverizing equipment, and then gradually added to water in which the present dispersant is dissolved with stirring, and if necessary, a thickener,
The present composition can be prepared by adding and mixing an antifreezing agent, an antiseptic, an antifoaming agent, a spreading agent, an auxiliary agent such as a stabilizer, and water for adjusting the concentration.

In the case of wet pulverization, the active ingredient is put into water in which the present dispersant is dissolved under stirring and finely pulverized by the above pulverizing equipment, and if necessary, a thickener, an antifreezing agent and an antiseptic agent. , Defoaming agents, spreading agents, stabilizers and other auxiliary agents,
The present composition can be prepared by adding and mixing water for concentration adjustment. In order to reduce the solid component having a particle size of 10 μm or more, it is desirable to perform coarse pulverization or sieving to remove large particles before fine pulverization.

The present composition can be applied by a method in which a usual aqueous suspension fungicide composition is applied, and as a crop to be treated,
Rice, wheat, barley, corn, cotton, soybean, peas,
Peanuts, beets, potatoes, cabbage, cucumbers, tomatoes, grapes, peaches, oysters, apples, mandarin oranges, pears, strawberries, tobacco, and carnations, roses, and other flowers. In the treatment, the composition can be appropriately diluted with water according to the required concentration of the active ingredient, and can be applied by spraying with a power spray or a hand sprayer.

[0016]

Examples Example 1 (1) Procymidone 2012.11 g (containing 2000 g as an active ingredient), a silicon-based defoamer (trade name: Antifoam C, manufactured by Dow Corning Asia) 8 g, polyoxyethylene tristyrylphenyl ether phosphorus Acid triethanolamine salt (trade name: Soprofol FL, manufactured by Rhodia Nikka) 160 g, propylene glycol 20
0g and 953.22g of deionized water were mixed and pulverized with a Dynomill (rotation number: 4500 rpm, glass beads used: 3GX, bead filling rate: 80%, retention time: 3
Min), and a crushed slurry containing 60% of procymidone was prepared.

(2) Separately, aluminum magnesium silicate (trade name: Bee Gum Gran, manufactured by Sansei) 2
4g, Zansan gum (trade name: Kerzan S, Sansan) 1
2 g and 1,2-benzisothiazolin-3-one (trade name: Proxel GXL, manufactured by Avicia) 12 g were mixed and dissolved and dispersed in 1551.96 g of deionized water to prepare a thickener solution.

(3) Ground slurry 10 prepared in (1)
320 g of the thickening agent prepared in (2) was added to 00 g, and 72.11 g of deionized water was further added and mixed to obtain the present composition 1 containing 43.1% by weight of procymidone.

Example 2 The crushing time in the Dynomill was changed (rotation speed: 450).
0 rpm, glass beads used: 3GX, bead filling rate:
This composition 2 was prepared in the same manner as in Example 1 except that 80% and the residence time were 2 minutes).

Formulation Example 3 (1) Diclosimet drug substance 83.5 g (containing 78.3 g as an active ingredient), silicone antifoaming agent (trade name: Antifoam CE, manufactured by Dow Corning Asia) 2 g, polyoxyethylene tristyryl Phenyl ether phosphate potassium salt (trade name: Soprofol FLK, manufactured by Rhodia Nichika) 62.5 g, propylene glycol (manufactured by Showa Denko) 50 g, and deionized water 142.5 g are mixed, and Dynomill (Shinmaru Enterprises) Made KD-L
With a volume average particle size of 10 μm or more to 25% or less (rotation number: 4500 rpm, glass beads used: 4GX, bead filling rate: 80%, residence time:
3 minutes), a crushed slurry containing 23% of diclocymet was prepared.

(2) Separately, aluminum magnesium silicate (trade name: Bee Gum Gran, manufactured by Sansei)
4.8 g, xanthan gum (trade name: Kerzan S, manufactured by Sansei) 2.4 g, 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazoline-
A thickener liquid was prepared by mixing, dissolving and dispersing 3 g of a 3-one mixture (trade name: Biohop L, manufactured by Abyssia) in 312.7 g of deionized water.

The thickening agent solution prepared in (2) was added to the crushed slurry prepared in (1), and deionized water was further added and mixed to obtain Composition 3 of the present invention containing 7.8% by weight of diclocymet. Obtained. The particle size of the solid component is measured by a Coulter counter (Coulter Multisizer TA-II
(Type) As a result of measurement, the volume fraction of particles having a volume average particle diameter of 10 μm or more was 20.5%.

Comparative Example 1 Dynomill grinding conditions were changed (rotation speed: 450).
0 rpm, glass beads used: 3GX, bead filling rate:
Comparative Example Composition 1 was prepared in the same manner as in Example 1 except that 80%, residence time: 1.5 minutes).

COMPARATIVE EXAMPLE 2 Dynomill grinding conditions were changed (rotation speed: 300).
0 rpm, glass beads used: 3GX, bead filling rate:
Comparative Example Composition 2 was prepared in the same manner as in Example 1 except that 80%, residence time: 3 minutes).

Test Example 1 For each of the present compositions 1 and 2 and the comparative compositions 1 and 2, the suspension rate was measured by the following method. The results are shown in Table 1. Further, for each of the above compositions, the particle size was measured using a Coulter Counter TA-II type,
The volume fraction (%) of particles having a volume average particle diameter of 10 μm or more was determined. The results are shown in Table 1.

(Suspension Rate Measuring Method) 0.5 g of the test sample was weighed in a 250 ml graduated cylinder with a stopper, which had been preheated to 30 ° C., and standard hard water having a hardness of 342 ppm at 30 ° C. was added to 250 ml to make a stopper. One cylinder
Invert 30 times a minute, shake and stir in a constant temperature water bath at 30 ° C. After 30 minutes, gently remove the upper 225 ml, analyze the content of procymidone in the rest by gas chromatography, and calculate the suspension rate according to the following formula.

Suspension rate = 250/225 × 100 × (C-
Q) / C C: Total procymidone amount in 250 ml Q: Procymidone amount in bottom 25 ml

[0028]

[Table 1]

[0029]

Test Example 2 This composition 1 was diluted with tap water so that the amount of the active ingredient was 500 ppm, and the diluted solution was spray-treated with cucumber until the leaves were sufficiently wet. 1 day after the treatment, Botrytis cinerea was inoculated, and the preventive effect was evaluated 5 days after the inoculation,
Good results were shown without any phytotoxicity.

Test Example 3 The present composition 3 was diluted with tap water so that the amount of the active ingredient was 500 ppm, and the diluted solution was sprayed on rice until the leaves were sufficiently wet. One day after the treatment, the rice blast fungus was inoculated, and the preventive effect was evaluated 7 days after the inoculation.

[0032]

EFFECTS OF THE INVENTION According to the present invention, it is possible to provide an excellent aqueous suspension bactericidal composition which can maintain good uniformity of the active ingredient when diluted with water, has an excellent bactericidal effect, and does not cause chemical damage. As it can be provided, its practical value is extremely high.

Claims (5)

[Claims] 1. An aqueous suspension containing (a) 1 to 50% by weight of a bactericidal active ingredient which is solid at room temperature and has a water solubility of 500 ppm or less, and (b) 1 to 10% by weight of polyoxyalkylene polystyrylphenyl ether phosphate ester salt. An aqueous suspension bactericidal composition, which is a turbid bactericidal composition, wherein the volume fraction of the solid component having an average particle size of 10 μm or more is 25% or less. 2. The aquatic suspension fungicide composition according to claim 1, wherein the polyoxyalkylene polystyryl phenyl ether phosphate ester salt is a polyoxyethylene tristyryl phenyl ether phosphate ester salt. 3. The aqueous suspension germicide composition according to claim 2, wherein the polyoxyethylene tristyrylphenyl ether phosphate salt is a potassium salt or a triethanolamine salt. 4. The bactericidal active ingredient is procymidone.
The aqueous suspension bactericidal composition according to any one of 1 to 3. 5. The aquatic suspension fungicide composition according to claim 1, wherein the fungicidal active ingredient is diclocymet.