JPS6011402A - Stabilized wettable powder for controlling plant blight - Google Patents

Abstract

PURPOSE:To obtain a wettable powder exhibiting excellent stabilizing effect to trifolin, storable stably for a long period, and having excellent dispersibility in water and flowability, by combining a surface active compound and trifolin which is a piperazine-type fungicide. CONSTITUTION:The objective agent is produced by compounding (A) trifolin {N,N'-[(1-formamido-2,2,2-trichloro)ethyl]piperazine} which is a piperazine-type fungicide having relatively low toxicity and exhibiting excellent preventive and curing effect against a wide variety of plant blights such as powdery mildew, rust, scab, etc. of vegetables, fruits, etc. homogeneously with (B) an alkyl-naphthalenesulfonic acid alkali metal salt and (C) a calcined silica, and if necessary, (D) a mineral powder, alumina, etc. The amounts of the components (B) and (C) are 0.1-4pts.wt. and 3-30pts.wt. per 1pt.wt. of trifolin, respectively. The composition is applied by diluting to the trifolin concentration of 50-200ppm. The diluted liquid has excellent dispersibility in water, and does not cause the clogging of the nozzle during the application process.

Description

[Detailed description of the invention] The present invention relates to a stabilized plant disease control irrigation agent.

N,l-bis((1-formamido-2,2,2-)lichloro)ethyl]pibeodine (hereinafter abbreviated as triforin) >It-L A piperazine-based fungicide with relatively low toxicity, effective against a wide range of plant diseases. , especially vegetables that have been actively cultivated in recent years (e.g. Japanese cabbage, eggplant, etc.) 1. Fruits! (e.g. ginger, eggplant, etc.)
It exhibits excellent preventive and therapeutic effects on powdery mildew, rust, akaya blight, scab, and anthracnose, which are important diseases of peach, etc.) and flower petals (e.g., roses, chrysanthemums, etc.).

However, various formulations of triforine lack stability, and even if their hydrating powders are prepared using known methods, triforine decomposes during storage, reducing the pesticidal effect, and furthermore, they have poor water dispersibility and fluidity, which is a major drawback. When preparing a spray solution by diluting it with water, the spray nozzle orifice sometimes closed, resulting in a spray dome.

In view of these circumstances, the present inventors have conducted various studies and found that a combination of a surfactant-containing alkali metal salt of alkylnaphthalene sulfonate and calcined silica has a specific stabilizing effect on triforine, and at the same time, it has been found that The present invention was completed based on the finding that the properties and fluidity of the product were improved.

That is, the present invention relates to a stabilized plant disease control irrigation agent (hereinafter sometimes abbreviated as triforine hydrating agent) characterized by containing triforine, an alkylnaphthalene sulfonic acid alkali metal salt, and calcined silica. .

The alkylnaphthalene sulfonic acid alkali metal salt used in the triforine aqueous solution of the present invention is an alkali metal salt of a compound in which the naphthalene nucleus is substituted with one or more amine groups and one or more sulfonic acid groups. Examples of the alkyl group here include methyl, ethyl fi/, n-propyμ
, isopropyl/lz, n-butyl, isobutyμ, t-butyl, n-benchiμ, isobenchiμ, hexyl/l/, heptyl, octyl, and other direct or branched alkyl groups having 1 to 8 carbon atoms are used. and those substituted with one or two of the same or different alkyl groups mentioned above are often used.

In addition, when an alkyl group having 6 or more carbon atoms is substituted, it is a monosubstituted product or a lower alkyl group having 1 to 4 carbon atoms.
It is preferable that it is a di-substituted product with 1/group.

The number of sulfones substituted with the naphthalene nucleus may be one, but it may be desirable to have two or three Re. As the alkali metal, for example, lithium, sodium, potassium, etc. are frequently used. Normal commercial products of such alkylnafculene acid alkali metal salts contain several tens of percent of solvents such as ethylene glycol-V, but there is no need for the production of the triforine aqueous agent of the present invention. I can't help it. However, it is best to remove impurities such as mirabilite beforehand.

The pyrogenic silica used in the triforine irrigation agent of the present invention means heat-treated silica (or anhydrous 7; yadic acid). The temperature in this heat treatment is usually in the range of about 100°C to 1500°C under normal pressure, preferably 300°C.
℃ to about 1400℃, most preferably 800℃ to 1
(approximately 300°C) 5. The heat treatment can also be carried out under reduced pressure, and the heating temperature at that time may be lower than the heating temperature under normal pressure. As a raw material for this calcined silica, commercially available silica (for example, Fine C μ■; product number RX
-70, X-70, P-8, manufactured by Tokuyama Soda) are used as appropriate. This raw material silica can be in any form, such as crystalline, amorphous, glassy, colloidal, etc., and it is preferable to form it into a powder of about 300 mesh or more before heat treatment.

This calcined silica is pulverized as needed to give a particle size of about 300 mesh or more, and then the present invention (
It is used as a raw material for Riforin irrigation agent.

When using the triforine irrigation agent of the present invention (1), the amount of alkali gold naphthalene fonic acid TjA salt relative to triforine is about 0.1 to 4 times, preferably about 0.
．． The amount of pyrogenic silica is preferably about 3 to 30 times, preferably about 5 to 255 times by weight.

In addition to the alkali gold n salt of alkylnaphthalene sulfonate and the a-component silica, alumina may be added as a stabilizer to the triforine irrigation agent of the present invention. The alumina used is commonly used non-activated alumina with weak or no adsorption properties (e.g. alumina: product '#A L-41+ AL-42, AI, -4).
3, AL-25 and AL-31, Sumitomo Aluminum Smelting (4'lff'J), or activated alumina with adsorptive properties can be used, but inactive alumina is preferable. When used, the alumina may be pulverized to a particle size of about 300 mesh or more, and then used as a raw material, either as is or after being heat-treated in the same manner as the silica.

The amount of alumina added to the triforine hydrating agent of the present invention is about 0.1 to 20 times the weight of triforine, preferably about 0.2 to 100 times by weight. When producing the triforine water preparation of the present invention, it is preferable to add mineral powder as described below about 0.5 to 7 times, preferably about 1 to 5 times by weight, the weight of triforin.

In addition, the triforine water conservancy of the present invention may be used as needed in soap odes, polyoxyalkylaryl esters/L/types (e.g., Nonar μ■, manufactured by Toho Chemical Co., Ltd.), alkyl/L' sulfates (
Examples, EmerμlO■, Emerμ4dsec, Kao Atlas [
flll), ax phosphonates (e.g., Neogen q◇
, Neogen T @, 1st Kogyo Shuyakuku 1 Nine Neo Verex ■, Kao Atlas Kusou), polyethylene glycol ether/l/ode (e.g., Nonipou/L'85■, Nonipou/I/10 button ■, Noniball) 160■, manufactured by Sanyo Chemical Industries)
, polyhydric alcohol esthetics/l's (e.g., Tween 20
Nonionic and anionic surfactants such as [F], Tween 8-9 (manufactured by Kao Atlas W) can also be used in combination.

Examples of the mineral powder used in the triforine irrigation agent of the present invention include diatomaceous earths such as kunilite (trade name, manufactured by Kunimine Kako Co., Ltd.) and radiolite, and kaolin, such as Siegphyte (trade name, manufactured by Sieglite Chemical Co., Ltd.). For example, Vitasy A/ (trade name, manufactured by Tabon Chemical), Toxy/
Finely powdered silicic acid such as I/ (trade name, manufactured by Tokuyama Soda Co., Ltd.), Nitsupsi / I/ (trade name 9 manufactured by Nippon Silica Co., Ltd.), Carb V Tsukunu (trade name, Salt Kidney (FlIVj Lou Hui)), such as Zeophyte (product name) For example, zeolites such as zeolite (made by Sun Zeolite), clays such as kaolin, bentonite, clay, and glues such as talc powder and waxite are used, and these can be one or two types. A mixture of two or more species can be used. Further, the particle size of the mineral powder is generally 200 mesh or more, preferably 300 mesh or more.

The plant disease control irrigation agent of the present invention includes the above-mentioned triforine, alkylnaphthalene sulfonic acid alkali metal salt, calcined silica,
By uniformly mixing 'ellJ quality powder, alumina, surfactant, etc., a91! ! will be built.

Such a hydrating powder for controlling plant diseases of the present invention is stable even when stored for a long period of time, and triforine does not decompose. The plant disease control water use agent of the present invention usually has a triforine concentration of 50
It can be used after being diluted to about 200 PPf and is stable for a long time even after dilution.The diluted solution has good dispersibility in water and well drainage, and the spray nozzle opening is closed during spraying. Not at all.

When the triforine hydrating agent of the present invention is used as a fungicidal composition for I% rows, the amount used is 10% of the triforine in the composition.
7-/L/, i=about 25f to 15(l), preferably about 409 to 8(l).

The triforine irrigation agent of the present invention is suitable for vegetables (e.g.
various plant diseases (e.g. powdery mildew,
It is possible to treat various diseases by spraying them at the time when they occur (Rust disease, Red star disease, Scotch disease, PJ rust disease, etc.). Plant diseases can be prevented.

Triforine, which is a raw material used in the triforine irrigation agent of the present invention, can be produced according to a known method. The alkali metal salt of alkylnaphthalene sulfonic acid, which is still a raw material, can be prepared by a method known per se, for example, [Synthesis and Concentration of Surfactants] 88-
90 pages, 1957 (published by Maki Shoten), USP 2020
35B and USP 2143493.

The present invention will be described in detail below with reference to Examples and Experimental Examples.

In addition, parts and percentages in the examples refer to nail damage percentages and heavy bite percentages.

Example 1 After uniformly mixing 9.4 parts of triforine, 6 parts of sodium dibutylnaphthalene sulfonate, and 18 parts of N-methylpyrrolidone, 18 parts of fine silica powder, which was calcined at 930°C, 10 parts of amimina, and diatoms were added. An irrigation agent obtained by adding 35 parts of soil, mixing it uniformly with a doomplender, and then processing it with a hammer-type crusher.

Example Nitori, 9.4 parts of Holin, 3 parts of sodium dipropylnaphthalene sulfonate, and 10 parts of N-methylpyrrolidone were mixed uniformly, and then calcined at 1100 tE to produce 15 parts of fine silica powder, 15 parts of alumina, and diatoms. An irrigation agent obtained in the same manner as in Example 1, adding 30 parts of soil and 20 parts of clay.

Example 3゜Triforine 7.5 parts - Djibouti~Naphthalene/I/71
= 5 parts of potassium salt, 15 parts of pyrrolidone, crook;
20 parts of fine silica powder, 30 parts of diatomaceous earth and 20 parts of puffed puff pastry were added, and the following procedure was carried out in the same manner as in Example Z (
-) hydrating agents.

Example (After uniformly mixing 10 parts of triforine, 15 parts of sodium dibutylnaphthalene/l'banate, and 5 parts of N-methylpyrrolidone, 20 parts of fine silica powder, 5 parts of alumina, which had been calcined at 850°C. 30 parts of Keihoko clay and 15 parts of clay
An irrigation agent obtained in the same manner as in Example t below.

Example Left 15 parts of triforine, 5 parts of sodium probylbutylnaphthalene sulfonate, and 10 parts of N-methylpyrrolidone were uniformly mixed, and 850 tons! An irrigation agent obtained in the same manner as in Example 1 by adding io parts of fine silica powder calcined with io, 20 parts of alumina, ±20 parts of diatoms, and 10 parts of clay.

Accidental example/, (Stability test of triforin water use agent) Example/
After putting the triforine irrigation agent according to the present invention shown in ~E into a sample bottle and storing it in a 40 ° C incubator and room temperature, the triforine content was measured by high performance liquid chromatography (filler: bolus polystyrene gel/L/), Measure oral changes. The results are shown in Table 1.

Table 1 Medium control triforine hydrating agent 75 parts of triforine, 15 parts of isopropyl μamine dodecyμ benzenesulfonate, and 10 parts of N-methylpyrrolidone were mixed uniformly, 50 parts of unfired silica fine powder and 10 parts of clay were added, and the mixture was mixed in a drum blender. Irrigation agent obtained by uniformly mixing the water with a machine and then processing it with a hammer-type crusher.

51! ! Experimental Example 2 (Water dispersibility test of triforine water use agent)
Each of the triforine irrigation agent according to the present invention and the control triforine irrigation agent shown in Examples/~S' was mixed with 3° hard water 50
Pour the water into a 500 liter beaker containing 0.0 L, and use a glass rod (L! diameter 0.5 cm, length 25 cm) to add 1 liter per second.
Stir 10 times to the right and 10 times to the left.

This suspension is passed through a 48-mesh sieve, and the resulting sieve residue is dried under reduced pressure (65 to IIg'5V) for 10 minutes, and then the weight fi (g) of the sieve residue is measured. It is entwined with the formula.

The results are shown in Table 2.

Controls similar to those used in Example 1/)! Jyl=! J
Hydration 6”In

Claims (1)

[Claims] Stabilization characterized by containing N,N'-bis[(1-formamido-2,2゜2-trichloro)ethyl]pibeodine, an alkali metal salt of alkylnaphthalenesulfonic acid, and pyrogenic silica. Hydrating agent for plant disease control.