A wettable powder for pesticide sterilization, its preparation method and application

Abstract

The present invention discloses a wettable powder for pesticide bactericidal action, its preparation method and application, which relate to the field of pesticides. The raw materials thereof include the following components by weight percentage: chlorothalonil 10 - 60%, tebuconazole 1 - 10%, picoxystrobin 1 - 10%, dispersant 1 - 15%, wetting agent 1 - 10%, stabilizer 1 - 20%, and filler 20% - 80%. The wettable powder of the present invention has a control effect of over 90% in the control of grape downy mildew and wheat powdery mildew. The adjuvant formulation of the present invention can not only ensure physical stability, but also has an obvious synergistic effect with the active pesticide ingredients, reducing the amount of drug used and improving the drug efficacy.

Description

Technical Field

[0001] The present invention relates to the technical field of pesticides, and particularly to a wettable powder for pesticide sterilization, a preparation method thereof, a using method thereof, and an application thereof in preventing and controlling farmland plant diseases. Background Art

[0002] Chlorothalonil is a non-systemic broad-spectrum fungicide. It can react with 3-phosphoglyceraldehyde dehydrogenase in fungal cells, bind to the protein containing cysteine in the enzyme body, destroy the activity of the enzyme, and disrupt the metabolism of fungal cells, causing them to lose vitality. When plants have been invaded by pathogens and the pathogens have entered the plants, the bactericidal effect is small. Chlorothalonil has no systemic conduction effect and will not be absorbed from the spraying site or the roots of plants. Chlorothalonil has good adhesion on the surface of plants and is not easily washed away by rainwater, etc., so it has a long drug efficacy period. Control objects: used to control various fungal diseases, also used as an industrial preservative or fruit preservative. Suitable crops: wheat, soybean, peanut, rice, vegetables, fruit trees, etc. Chlorothalonil: The pure product is a colorless and odorless crystalline solid, and the technical material has a slightly pungent odor. Melting point 252.1 °C. Partition coefficient logP = 2.92 (25 °C). Relative density 2.0. Solubility in water (25 °C) 0.81 mg / L. Stability: Stable when stored at room temperature, stable to ultraviolet irradiation in weakly alkaline and acidic aqueous solutions. Slowly hydrolyzes at pH>9.

[0003] Tebuconazole is a sterol biosynthesis inhibitor. It can be rapidly absorbed by the growing parts of plants and mainly transferred to the top. It not only has bactericidal activity but also can promote plant growth, making the roots developed, the leaf color dark green, the plants strong, and the effective tillering increased, thus increasing the yield. Control objects: can control diseases caused by fungi such as Blumeria, Puccinia, Rhynchosporium, Pyrenophora, and Septoria, such as wheat powdery mildew, rice loose smut, wheat sheath blight, sorghum head smut, wheat snow rot, wheat take-all, wheat bunt, barley leaf blotch, barley loose smut, barley sheath blight, maize head smut, soybean rust, rape sclerotinia, banana leaf spot, tea blister blight, apple blotch leaf spot, pear black rot, and grape black mold. Suitable crops: wheat, barley, oats, rye, maize, sorghum, peanut, banana, grape, tea, fruit trees, etc. Tebuconazole: This product is a racemic mixture, and the pure product is a colorless crystal (the technical material is a light brown powder). Melting point 105 °C, vapor pressure: 1.7×10-3 mPa (20 °C). Partition coefficient logP = 3.7 (20 °C). Relative density 1.25. Solubility in water 36 mg / L (pH 5-9, 20 °C), solubility in organic solvents (g / l, 20 °C): methylene chloride > 200, isopropanol, toluene 50-100, hexane < 0.1. Hydrolysis half-life DT50 > 1a (pH 4-9, 22 °C).

[0004] Picoxystrobin is a mitochondrial respiration inhibitor, that is, it inhibits mitochondrial respiration by inhibiting the electron transfer between cytochrome b and C1, and is effective against strains resistant to 14-demethylase inhibitors, benzamides, dicarboximides and benzimidazoles. Control object: Broad-spectrum, systemic fungicide. It is mainly used to control foliar diseases of wheat such as leaf blight, leaf rust, glume blotch, powdery mildew, etc. Compared with existing strobilurin fungicides, it has a stronger therapeutic effect on wheat leaf blight, net blotch and eyespot. Suitable crops: Wheat, barley, oats and rye; safe for crops and without phytotoxicity at recommended doses. Picoxystrobin: The pure product is a white powdery solid, with a melting point of 75 °C. Relative density 1.4 (20 °C). Vapor pressure 5.5*10-6 Pa, partition coefficient KowlogP = 3.6 (20 °C). Henry constant 6.5*10-4 Pam3mol-1. Solubility in water 3.1 mg / L (20 °C). Stable under pH 5 and 7 conditions.

[0005] Single active ingredient fungicide varieties often have different degrees of defects in the control of agricultural diseases. For example, after continuous use, the pathogenic bacteria are prone to develop drug resistance, and the increase in the number of uses will aggravate environmental pollution. In addition, the original drug of picoxystrobin has a low melting point (melting point 75 °C), and it is easy to agglomerate after heat storage. There are a large number of fine powders that do not pass through the sieve in the wet sieve test, which brings certain difficulties to the formulation of wettable powders.

[0006] Therefore, it is necessary to develop a bactericidal composition that can solve the above problems. Summary of the Invention

[0007] Object of the Invention

[0008] To overcome the above deficiencies, the purpose of the present invention is to provide a wettable powder for pesticide bactericidal, its preparation method and application. The wettable powder of the present invention has a control effect of more than 90% in the control of grape downy mildew and wheat powdery mildew. The adjuvant formulation of the present invention can not only ensure physical stability, but also has an obvious synergistic effect with the active ingredient of the pesticide, reducing the amount of drug used and improving the drug effect.

[0009] Solution

[0010] To achieve the purpose of the present invention, the technical solution adopted by the present invention is as follows:

[0011] In the first aspect, the present invention provides a wettable powder for pesticide bactericidal, which comprises the following raw materials in weight percentage: chlorothalonil 10-60%, tebuconazole 1-10%, picoxystrobin 1-10%, dispersant 1-15%, wetting agent 1-10%, stabilizer 1-20%, filler 20%-80%.

[0012] Further, the wettable powder for pesticide bactericidal action comprises raw materials in the following weight percentages: chlorothalonil 10-60%, tebuconazole 1-10%, picoxystrobin 1-10%, dispersant 3-10%, wetting agent 2-6%, stabilizer 2-7%, and filler 20%-70%.

[0013] Further, the wettable powder for pesticide bactericidal action comprises raw materials in the following weight percentages: chlorothalonil 10-60%, tebuconazole 1-10%, picoxystrobin 1-10%, dispersant 3-9%, wetting agent 3-6%, stabilizer 3-6%, and filler 20%-70%.

[0014] Further, the wettable powder for pesticide bactericidal action comprises raw materials in the following weight percentages: chlorothalonil 10-60%, tebuconazole 1-10%, picoxystrobin 1-10%, dispersant 3-7%, wetting agent 3-6%, stabilizer 3-6%, and filler 22%-48%.

[0015] Further, it comprises raw materials in the following weight percentages: chlorothalonil 30-60%, tebuconazole 1-10%, picoxystrobin 1-10%, dispersant 3-7%, wetting agent 3-6%, stabilizer 3-6%, and filler 22%-48%.

[0016] Further, it comprises raw materials in the following weight percentages: chlorothalonil 30-54%, tebuconazole 1-6%, picoxystrobin 1-5%, dispersant 3-7%, wetting agent 3-6%, stabilizer 3-6%, and filler 20%-56%;

[0017] Further, it comprises raw materials in the following weight percentages: chlorothalonil 30-54%, tebuconazole 1-6%, picoxystrobin 1-5%, dispersant 3-7%, wetting agent 3-6%, stabilizer 3-6%, and filler 22%-48%;

[0018] Among them, the dispersant is selected from at least two of sodium salt of naphthalene sulfonic acid formaldehyde condensate, formaldehyde condensate of alkyl naphthalene sulfonate, sodium lignin sulfonate, and sodium salt of styrene acrylic acid copolymer; optionally, in the above wettable powder for pesticide bactericidal action, the dispersant comprises sodium salt of naphthalene sulfonic acid formaldehyde condensate and formaldehyde condensate of alkyl naphthalene sulfonate, and the weight ratio of sodium salt of naphthalene sulfonic acid formaldehyde condensate to formaldehyde condensate of alkyl naphthalene sulfonate is (1-4):2, optionally (1-3):2, and optionally 3:2; and / or, the dispersant comprises sodium salt of styrene acrylic acid copolymer and sodium lignin sulfonate, and the weight ratio of sodium salt of styrene acrylic acid copolymer to sodium lignin sulfonate is 1:(1-3), preferably 1:2; optionally, the wetting agent is selected from one or more of sodium diisooctyl sulfosuccinate, polymer of olefin and maleic anhydride, and sodium diisobutyl naphthalene sulfonate; optionally, it is one or two of sodium diisooctyl sulfosuccinate and polymer of olefin and maleic anhydride.

[0019] Furthermore, it comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 5%, dispersant 3 - 5%, wetting agent 3 - 4%, stabilizer 5 - 6%, filler 22% - 48%. Among them, the dispersant includes sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate, and the weight ratio of sodium naphthalene sulfonate formaldehyde condensate to alkyl naphthalene sulfonate formaldehyde condensate is (1 - 4):2, optionally (1 - 3):2, optionally 3:2 or 1:2, and optionally the weight percentages of sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate are 3 - 5%; optionally, the wetting agent is selected from one or more of sodium diisooctyl sulfosuccinate, the polymer of olefin and maleic anhydride, and sodium diisobutyl naphthalene sulfonate; optionally one or two of sodium diisooctyl sulfosuccinate and the polymer of olefin and maleic anhydride.

[0020] Furthermore, it comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 3.3%, dispersant 3 - 5%, wetting agent 3 - 4%, stabilizer 5 - 6%, filler 22.7% - 48%. Among them, the dispersant includes sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate, and the weight ratio of sodium naphthalene sulfonate formaldehyde condensate to alkyl naphthalene sulfonate formaldehyde condensate is (1 - 4):2, optionally (1 - 3):2, optionally 3:2 or 1:2, and optionally the weight percentages of sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate are 3 - 5%; optionally, the wetting agent is selected from one or two of sodium diisooctyl sulfosuccinate and the polymer of olefin and maleic anhydride.

[0021] Furthermore, it comprises raw materials with the following weight percentages: chlorothalonil 50%, tebuconazole 1 - 5%, picoxystrobin 1 - 5%, dispersant 5 - 9%, wetting agent 4 - 6%, stabilizer 3 - 5%, filler 22% - 48%. Optionally, the dispersant includes sodium styrene acrylate copolymer and sodium lignosulfonate, and the weight ratio of sodium styrene acrylate copolymer to sodium lignosulfonate is 3:(2 - 6), optionally 3:(2 - 4), optionally 3:2 or 3:4, and optionally the weight percentages of sodium styrene acrylate copolymer and sodium lignosulfonate are 5 - 9%; optionally, the wetting agent is selected from one or two of sodium diisobutyl naphthalene sulfonate and sodium diisooctyl sulfosuccinate.

[0022] Furthermore, it comprises raw materials with the following weight percentages: chlorothalonil 50%, tebuconazole 1%, picoxystrobin 1%, dispersant 5 - 7%, wetting agent 4 - 6%, stabilizer 3 - 5%, filler 22% - 48%; optionally, the dispersant includes sodium styrene acrylate copolymer and sodium lignosulfonate, and the weight ratio of sodium styrene acrylate copolymer to sodium lignosulfonate is 3:

[0023] (2 - 6), optionally 3: (2 - 4), optionally 3: 2 or 3: 4, optionally the weight percentage content of sodium styrene acrylate copolymer and sodium lignosulfonate is 5 - 7%; optionally, the wetting agent is selected from one or two of sodium diisobutylnaphthalene sulfonate and sodium diisooctyl sulfosuccinate.

[0024] Optionally, the wettable powder for pesticide bactericidal includes raw materials with the following weight percentage contents: chlorothalonil 50%, tebuconazole 1 - 5%, picoxystrobin 1 - 5%, sodium styrene acrylate copolymer 3%, sodium lignosulfonate 2 - 6%, wetting agent 4 - 6%, silica white 3 - 5%, and talcum powder to make up 100%; optionally, the wetting agent is selected from one or two of sodium diisooctyl sulfosuccinate and sodium diisobutylnaphthalene sulfonate;

[0025] Optionally, the wettable powder for pesticide bactericidal includes raw materials with the following weight percentage contents: chlorothalonil 50%, tebuconazole 1%, picoxystrobin 1%, sodium styrene acrylate copolymer 3%, sodium lignosulfonate 2 - 4%, sodium diisooctyl sulfosuccinate 4 - 6%, silica white 3 - 5%, and talcum powder to make up 100%.

[0026] Optionally, the wettable powder for pesticide bactericidal includes raw materials with the following weight percentage contents: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 3.3%, sodium naphthalene sulfonate formaldehyde condensate 1 - 3%, alkylnaphthalene sulfonate formaldehyde condensate 2 - 4% (or 2%), wetting agent 3 - 4%, silica white 3 - 6%, and talcum powder 22.7% - 48%; optionally, the wetting agent is selected from one or more of sodium diisooctyl sulfosuccinate, polymer of olefin and maleic anhydride, and sodium diisobutylnaphthalene sulfonate; optionally one or two of sodium diisooctyl sulfosuccinate and polymer of olefin and maleic anhydride;

[0027] Optionally, the wettable powder for pesticide bactericidal includes raw materials with the following weight percentage contents: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 3.3%, sodium naphthalene sulfonate formaldehyde condensate 1 - 3%, alkylnaphthalene sulfonate formaldehyde condensate 2 - 4% (or 2%), wetting agent 3 - 4%, silica white 5 - 6%, and talcum powder 22.7% - 48%; optionally, the wetting agent is selected from one or more of sodium diisooctyl sulfosuccinate and polymer of olefin and maleic anhydride;

[0028] Optionally, the wettable powder for pesticide bactericidal includes raw materials with the following weight percentage contents: chlorothalonil 54%, tebuconazole 6%, picoxystrobin 3.3%, sodium naphthalene sulfonate formaldehyde condensate 3%, alkylnaphthalene sulfonate formaldehyde condensate 2%, sodium diisooctyl sulfosuccinate 4%, silica white 5%, and talcum powder 22.7%.

[0029] Further, the wettable powder for pesticide bactericidal action comprises raw materials in the following weight percentages: chlorothalonil 54%, tebuconazole 6%, picoxystrobin 3.3%, dispersant 5%, wetting agent 4%, stabilizer 5%, and filler 22.7%.

[0030] Further, the wettable powder for pesticide bactericidal action comprises raw materials in the following weight percentages: chlorothalonil 54%, tebuconazole 6%, picoxystrobin 3.3%, sodium naphthalene sulfonate formaldehyde condensate 3%, alkyl naphthalene sulfonate formaldehyde condensate 2%, sodium diisooctyl sulfosuccinate 4%, silica white 5%, and talcum powder 22.7%.

[0031] In the above wettable powder for pesticide bactericidal action, the dispersant is selected from at least one or more of sodium naphthalene sulfonate formaldehyde condensate, alkyl naphthalene sulfonate formaldehyde condensate, sodium lignosulfonate, sodium styrene acrylate copolymer, methyl naphthalene sulfonate formaldehyde condensate sulfate, sodium methylene naphthalene sulfonate dibutyl naphthalene sulfonate formaldehyde condensate, N-methyl fatty acyl taurine sodium salt, and alkylphenol polyoxyethylene ether formaldehyde condensate sulfate;

[0032] Optionally, in the above wettable powder for pesticide bactericidal action, the dispersant is selected from at least two of sodium naphthalene sulfonate formaldehyde condensate, alkyl naphthalene sulfonate formaldehyde condensate, sodium lignosulfonate, and sodium styrene acrylate copolymer;

[0033] Optionally, in the above wettable powder for pesticide bactericidal action, the dispersant comprises sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate, and the weight ratio of sodium naphthalene sulfonate formaldehyde condensate to alkyl naphthalene sulfonate formaldehyde condensate is (1 - 4):2, optionally (1 - 3):2, optionally 3:2 or 1:2; and / or, the dispersant comprises sodium styrene acrylate copolymer and sodium lignosulfonate, and the weight ratio of sodium styrene acrylate copolymer to sodium lignosulfonate is 3:(2 - 6), optionally 3:(2 - 4), optionally 3:2 or 3:4;

[0034] In the above wettable powder for pesticide bactericidal action, the wetting agent is selected from one or more of sodium diisooctyl sulfosuccinate, polymer of olefin and maleic anhydride, sodium diisobutyl naphthalene sulfonate, sodium dodecyl sulfate, methyl a-sulfo fatty acid ester, sodium tetradecyl sulfate, sodium dodecylbenzenesulfonate, alkyl naphthalene sulfonate, a-olefin sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, fatty acid sulfate, and fatty acid ester sulfate;

[0035] Optionally, in the above wettable powder for pesticide bactericidal action, the wetting agent is selected from one or more of sodium diisooctyl sulfosuccinate, polymer of olefin and maleic anhydride, and sodium diisobutyl naphthalene sulfonate; optionally one or two of sodium diisooctyl sulfosuccinate and polymer of olefin and maleic anhydride.

[0036] In the above-mentioned wettable powder for pesticide bactericidal, the stabilizer is one or more of corn starch, urea, CMC, and silica white; optionally it is silica white, and optionally it is ordinary silica white.

[0037] In the above-mentioned wettable powder for pesticide bactericidal, the filler includes one or more of talcum powder and diatomaceous earth; optionally it is talcum powder.

[0038] In the above-mentioned wettable powder for pesticide bactericidal, the weight ratio of the dispersant, wetting agent and stabilizer is (3 - 9):(3 - 6):

[0039] (3 - 6), optionally (3 - 7):(3 - 6):(3 - 6), optionally (3 - 5):(3 - 4):(5 - 6), optionally (5 - 9):(4 - 6):(3 - 5), optionally (5 - 7):(4 - 6):(3 - 5), optionally 5:4:5.

[0040] In the above-mentioned wettable powder for pesticide bactericidal, the dispersant includes sodium styrene acrylate copolymer and sodium lignosulfonate, and the wetting agent includes sodium diisobutylnaphthalene sulfonate.

[0041] And / or, in the above-mentioned wettable powder for pesticide bactericidal, the dispersant includes sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate, and the wetting agent includes one or several of sodium diisobutylnaphthalene sulfonate, polymer of olefin and maleic anhydride, and sodium diisooctyl sulfosuccinate.

[0042] In the second aspect, the present invention provides a preparation method of the wettable powder for pesticide bactericidal according to the first aspect, including:

[0043] Mix chlorothalonil, tebuconazole, picoxystrobin, dispersant, wetting agent, stabilizer, and filler evenly, carry out ultrafine air flow pulverization, and carry out secondary mixing on the obtained fine powder to obtain the wettable powder of chlorothalonil, tebuconazole and picoxystrobin; optionally, the fine powder with a particle size of 400 - 800 meshes is obtained after ultrafine air flow pulverization.

[0044] In the third aspect, the present invention provides a using method of the wettable powder for pesticide bactericidal according to the second aspect or the wettable powder for pesticide bactericidal prepared by the preparation method according to the second aspect. The wettable powder is diluted with water and applied by spraying. Optionally, the dilution multiple is 500 - 750 times.

[0045] In the fourth aspect, the present invention provides an application of the wettable powder according to the first aspect or the wettable powder prepared by the preparation method according to the second aspect in preventing and controlling farmland plant diseases; optionally, the plant diseases include one or several of downy mildew, powdery mildew, gray mold, and rust; optionally, it includes one or several of grape downy mildew, wheat powdery mildew, and soybean rust.

[0046] Advantageous Effects

[0047] (1) The wettable powder of the present invention has a control effect of over 90% in controlling grape downy mildew and wheat powdery mildew. The adjuvant formulation of the present invention can not only ensure physical stability, but also has an obvious synergistic effect with the active ingredient of the pesticide, reducing the amount of drug used and improving the drug efficacy.

[0048] (2) By adding alkylnaphthalenesulfonate formaldehyde condensate type adjuvants, the present invention improves the adsorption of the adjuvant to the active ingredient, better isolates the active ingredient through small molecule adjuvants to improve the agglomeration situation, and effectively improves the wettability by adding sodium diisooctyl sulfosuccinate, improving the situation that tebuconazole has strong lipophilicity and is difficult to wet. At the same time, the formulation has the advantages of adapting to various water qualities, low foaming property, high suspension rate, etc. The preparation of the present invention is environmentally friendly, has low processing cost, is convenient to process and use, and has functions such as protecting and preventing diseases and treating diseases. Detailed implementation manners

[0049] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention.

[0050] In addition, to better illustrate the present invention, numerous specific details are given in the following detailed implementation manners. Those skilled in the art should understand that the present invention can be implemented without some specific details. In some embodiments, the raw materials, schemes, methods, means, etc. well-known to those skilled in the art are not described in detail to highlight the gist of the present invention.

[0051] Unless otherwise clearly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "having" etc. will be understood to include the stated elements or components, without excluding other elements or other components.

[0052] The above-mentioned bactericidal composition provides a new choice for controlling plant diseases. The following further illustrates the present disclosure through examples, but the present disclosure is not limited thereby.

[0053] In the following examples, chlorothalonil, picoxystrobin and tebuconazole can all be obtained commercially, and other adjuvants are also commercially available products.

[0054] The following further details the present invention through examples.

[0055] In the research and development of the wettable powder of chlorothalonil, picoxystrobin, and tebuconazole, picoxystrobin has a relatively low melting point and is prone to caking after heat storage. There is also a situation where a large amount of fine powder fails to pass through the sieve in the wet sieve test, which brings certain difficulties to the research and development of the wettable powder.

[0056] The inventors conducted a large number of screening works on the adjuvant system and finally obtained the system with the best matching degree among the above components. In particular, the screening and combination of components such as dispersants and wetting agents, stabilizers and fillers greatly improved the stability of the dosage form, with advantages such as adaptability to various water qualities, low foaming property, and high suspension rate, effectively solving the problem of poor thermal storage stability of the product. Specifically, the formulations of some examples are shown in Table 1:

[0057] Table 1 Formulations of Each Example

[0058]

[0059]

[0060] In the above examples and comparative examples, the adjuvants and technical materials are all commercially available. For example, sodium salt of styrene acrylic acid copolymer is purchased from Solvay Chemicals, sodium salt of naphthalene sulfonic acid formaldehyde condensate is purchased from BASF Co., Ltd., formaldehyde condensate of alkyl naphthalene sulfonate is purchased from Nouryon Chemicals, polymer of olefin and maleic anhydride is purchased from Shanghai Moqin New Materials Co., Ltd., sodium diisooctyl sulfosuccinate is purchased from Weifang Elite Chemical Co., Ltd., the silica is ordinary silica commonly used in pesticide adjuvants, and the talcum powder is a commonly used filler in pesticide adjuvants, specifically 800-mesh talcum powder.

[0061] The preparation method of the wettable powder of the above Examples 1-10 includes the following steps: Mix chlorothalonil, tebuconazole, picoxystrobin, dispersant, wetting agent, stabilizer, and filler evenly, and perform ultrafine air flow pulverization. Preferably, fine powder with a particle size of 400-800 meshes is obtained. After the obtained fine powder is subjected to secondary mixing, the wettable powder product of chlorothalonil, tebuconazole, and picoxystrobin is obtained.

[0062] The performance of the wettable powder prepared in the above examples was tested, and the results are shown in Table 2 below.

[0063] The suspension rate in different water qualities (C water: hardness is 500 mg / L, pH = 7.0 - 8.0; 3WHO water: hardness is 1026 mg / L, pH = 6.0 - 7.0, hardness refers to the total concentration of calcium and magnesium ions in water) was detected according to CIPAC MT15.1, the wettability was detected according to CIPAC MT53.3, the screening (wet sieve test) was detected according to CIPAC MT185, the persistent foaming property was detected according to CIPAC MT47.1, and the thermal storage stability was determined according to the requirements of solid preparations in GB / T 19136.

[0064] Wettability (refer to CIPAC MT53.3) is expressed by measuring the length of wetting time. Generally, less than 120s is qualified. The determination method is: take 342mg / L hard water (100±1)ml, inject it into a 250ml beaker, place the beaker in a constant temperature water bath at (25±1)℃, and make the seventeen pages flush with the horizontal surface of the water bath. When the hard water reaches (25±1)℃, weigh (5±0.1)g of the sample with a watch glass, and pour all the samples evenly from the level of the beaker mouth onto the liquid surface of the beaker at once, but do not disturb the liquid surface excessively. When adding the sample, use a stopwatch to time it immediately until the paper sample is completely wetted. Record the wetting time. Repeat this five times and take the average value as the wetting time of the sample.

[0065] Table 2 Performance test results of wettable powders prepared by compounding thiophanate-methyl, tebuconazole and picoxystrobin

[0066]

[0067] It can be seen from the data in Table 2 that the suspension rate of the wettable powders prepared in Examples 4 to 9 before and after hot storage still maintains a high level of more than 90%, even reaching 94% and higher, no fine powder is screened, the hot storage stability is good, the wetting time is fast, and the persistent foaming is relatively low. In particular, the physical properties such as suspension, wettability, and wetting time of Examples 5 to 9 are better; the quality of Examples 1 to 3 and 8 before and after hot storage is not good, especially the quality after hot storage has obviously deteriorated.

[0068] In Examples 4 to 9, when the preferred adjuvants were selected, the performance of the obtained wettable powders was similar when the content of the active drug ingredients varied within the preferred ratio range, which indicates that the drug content had little effect on the performance of the formulation when the preferred adjuvant ingredients and contents were used. From Examples 1 to 3 and 8, it can be seen that when non-preferred adjuvants were used, the performance of the obtained wettable powders was relatively poor, which indicates that the ingredients and contents of the preferred adjuvants significantly improved the performance of the compound wettable powders of thiophanate-methyl, tebuconazole and picoxystrobin, while non-preferred adjuvants did not.

[0069] Field test example 1

[0070] The experiment was arranged to be carried out in a grape-growing greenhouse and wheat field of a farmer's household in the suburbs of Weifang City, Shandong Province. The experiment was set up in different planting areas, and the pesticides were sprayed. The test plots were randomly arranged. The experiment set up blank control treatment and pesticide treatment. There were 4 treatments in total, namely: Treatment 1: clean water spray, blank control; Treatment 2: the thiophanate-methyl·tebuconazole·picoxystrobin wettable powder obtained in Examples 1-10; Treatment 3: Comparative Example 1 (75% tebuconazole·picoxystrobin wettable powder (commercially purchased from Shanghai Yuelian Biotechnology Co., Ltd.)); Treatment 4: Comparative Example 2 (75% tebuconazole·thiophanate-methyl wettable powder (commercially purchased from Limin Chemical Co., Ltd.)).

[0071] At the initial stage of the onset of grape downy mildew in the grape greenhouse, control spray treatment was carried out. In Example 2 of the treatment, spray treatment was carried out at an active ingredient dosage of 1000 g / ha; in Treatment 3, spray treatment was carried out at an active ingredient of 1500 g / ha; in Treatment 4, spray treatment was carried out at an active ingredient of 1600 g / ha. The pesticide was applied once with a Gongnong-16 type knapsack manual sprayer. The liquid medicine was prepared by diluting with 750 L of water per hectare of the preparation dosage, and the liquid medicine amount in the plot was converted for uniform spraying. A randomized block design was adopted with 4 replicates, and the plot area was 20 m 2 (10 m × 2 m).

[0072] At the initial stage of the onset of wheat powdery mildew in the wheat field, control spray treatment was carried out. In Example 2 of the treatment, spray treatment was carried out at an active ingredient dosage of 800 g / ha; in Treatment 3, spray treatment was carried out at an active ingredient of 1200 g / ha; in Treatment 4, spray treatment was carried out at an active ingredient of 1400 g / ha. The pesticide was applied once with a Gongnong-16 type knapsack manual sprayer. The liquid medicine was prepared by diluting with 750 L of water per hectare of the preparation dosage, and the liquid medicine amount in the plot was converted for uniform spraying. A randomized block design was adopted with 4 replicates, and the plot area was 50 m 2 (10 m × 5 m).

[0073] Investigation method: Fix 4 points in each plot, 4 m at each point 2 , and the disease index in this area was investigated 30 days after pesticide application, and its control effect was calculated. The calculation formula is as follows:

[0074] The disease index investigation method was carried out according to the following grading standard and disease index calculation formula:

[0075] Grade 0: No disease spots;

[0076] Grade 1: The diseased spot area accounts for less than 5% of the entire leaf area;

[0077] Grade 3: The diseased spot area accounts for 6% - 10% of the entire leaf area;

[0078] Grade 5: The diseased spot area accounts for 11% - 25% of the entire leaf area;

[0079] Grade 7: The diseased spot area accounts for 26% - 50% of the entire leaf area;

[0080] Grade 9: The diseased spot area accounts for more than 50% of the entire leaf area

[0081] Disease index = 100 × ∑(number of diseased leaves at each level × representative value at each level) / (total number of leaves investigated × representative value of the highest level)

[0082] Control effect, % = ((disease index in the control plot - disease index in the treatment plot) / disease index in the control plot) * 100

[0083] Table 3 Control effect results of each treatment agent against Plasmopara viticola and Blumeria graminis f. sp. tritici

[0084]

[0085]

[0086] From the test results in Table 3 above, it can be seen that the wettable powders of chlorothalonil, tebuconazole, and picoxystrobin have good control effects against Plasmopara viticola and Blumeria graminis f. sp. tritici. Comparing Example 1 and 2 with Example 4, and Example 3 with Example 7, the ratios of the active ingredients of the pesticides are the same, mainly differing in the types and ratios of the auxiliaries. The bactericidal and control effects of Example 4 are about 5% higher than those of Example 1 and 2, and the bactericidal and control effects of Example 7 are more than 10% higher than those of Example 3. This shows that the specific auxiliaries of the present invention not only ensure good physical properties of the wettable powder, but also have an obvious synergistic effect between the active ingredients of the pesticide and the auxiliaries, improving the control effect of the pesticide. The specific auxiliaries of the present invention can make the wettable powders of chlorothalonil, tebuconazole, and picoxystrobin achieve a control effect of more than 90% in the control of Plasmopara viticola and Blumeria graminis f. sp. tritici. The composition ratio of the present invention can better exert the synergistic effect of the drug, reduce the amount of drug used, and improve the drug efficacy.

[0087] The present invention improves the adsorption of the auxiliaries to the active ingredients by adding alkylnaphthalenesulfonate formaldehyde condensate auxiliaries, better isolates the active ingredients through small molecule auxiliaries to improve the agglomeration situation, and effectively improves the wettability by adding sodium diisooctyl sulfosuccinate, improving the situation that tebuconazole has strong lipophilicity and is difficult to wet.

[0088] The auxiliary system screened by the present invention can not only adapt to various water qualities, has low foaming property and high suspension rate, but also solves the problem that picoxystrobin has a low original melting point and is thermally unstable during storage. The preparation of the present invention is environmentally friendly, has low processing cost, is convenient for processing and use, and has functions such as protection and treatment.

[0089] The wettable powder provided by the present invention has a relatively high content of active ingredients, which can reduce the dosage and application frequency of the fungicide, thereby reducing the agent cost.

[0090] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A wettable powder for pesticide bactericidal action, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 10 - 60%, tebuconazole 1 - 10%, picoxystrobin 1 - 10%, dispersant 1 - 15%, wetting agent 1 - 10%, stabilizer 1 - 20%, filler 20% - 80%; The dispersant is selected from sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate with a weight ratio of (1 - 4):2, or the dispersant is selected from sodium styrene acrylic copolymer and sodium lignosulfonate with a weight ratio of 3:(2 - 6); The wetting agent is selected from one of sodium diisooctyl sulfosuccinate, polymer of olefin and maleic anhydride, and sodium diisobutyl naphthalene sulfonate; The stabilizer is silica white; the filler is talcum powder; The weight ratio of the dispersant, wetting agent and stabilizer is (3 - 9):(3 - 6):(3 - 6).

2. The wettable powder for pesticide sterilization according to claim 1, wherein It comprises raw materials with the following weight percentages: chlorothalonil 10 - 60%, tebuconazole 1 - 10%, picoxystrobin 1 - 10%, dispersant 3 - 10%, wetting agent 2 - 6%, stabilizer 2 - 7%, filler 20% - 70%.

3. The wettable powder for pesticide sterilization according to claim 1, characterized in that It comprises raw materials with the following weight percentages: chlorothalonil 10 - 60%, tebuconazole 1 - 10%, picoxystrobin 1 - 10%, dispersant 3 - 9%, wetting agent 3 - 6%, stabilizer 3 - 6%, filler 20% - 70%.

4. The wettable powder for pesticide bactericidal action according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 10 - 60%, tebuconazole 1 - 10%, picoxystrobin 1 - 10%, dispersant 3 - 7%, wetting agent 3 - 6%, stabilizer 3 - 6%, filler 22% - 48%.

5. The wettable powder for pesticide sterilization according to claim 1, wherein, It comprises raw materials with the following weight percentages: chlorothalonil 30 - 60%, tebuconazole 1 - 10%, picoxystrobin 1 - 10%, dispersant 3 - 7%, wetting agent 3 - 6%, stabilizer 3 - 6%, filler 22% - 48%.

6. The wettable powder for pesticide bactericidal action according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 5%, dispersant 3 - 7%, wetting agent 3 - 6%, stabilizer 3 - 6%, filler 20% - 56%.

7. The wettable powder for pesticide sterilization according to claim 1, characterized in that It comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 5%, dispersant 3 - 7%, wetting agent 3 - 6%, stabilizer 3 - 6%, filler 22% - 48%.

8. The wettable powder for pesticide bactericidal action according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 5%, dispersant 3 - 5%, wetting agent 3 - 4%, stabilizer 5 - 6%, filler 22% - 48%.

9. The wettable powder for pesticide sterilization according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 3.3%, dispersant 3 - 5%, wetting agent 3 - 4%, stabilizer 5 - 6%, filler 22.7% - 48%.

10. The wettable powder for pesticide sterilization according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 50%, tebuconazole 1 - 5%, picoxystrobin 1 - 5%, dispersant 5 - 9%, wetting agent 4 - 6%, stabilizer 3 - 5%, filler 22% - 48%.

11. The wettable powder for pesticide sterilization according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 50%, tebuconazole 1%, picoxystrobin 1%, dispersant 5 - 7%, wetting agent 4 - 6%, stabilizer 3 - 5%, filler 22% - 48%.

12. The wettable powder for pesticide bactericidal action according to claim 1, characterized in that, It comprises raw materials with the following weight percentages: chlorothalonil 54%, tebuconazole 6%, picoxystrobin 3.3%, dispersant 5%, wetting agent 4%, stabilizer 5%, filler 22.7%.

13. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The weight ratio of sodium naphthalene sulfonate formaldehyde condensate to alkyl naphthalene sulfonate formaldehyde condensate is (1 - 3):

2.

14. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The weight ratio of sodium naphthalene sulfonate formaldehyde condensate to alkyl naphthalene sulfonate formaldehyde condensate is 3:

2.

15. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The weight ratio of sodium naphthalene sulfonate formaldehyde condensate to alkyl naphthalene sulfonate formaldehyde condensate is 1:

2.

16. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that, The weight ratio of sodium styrene acrylic copolymer to sodium lignosulfonate is 3:(2 - 4).

17. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that, The weight ratio of sodium styrene acrylic copolymer to sodium lignosulfonate is 3:

2.

18. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that The weight ratio of sodium styrene acrylic copolymer to sodium lignosulfonate is 3:

4.

19. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The stabilizer is common silica white.

20. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The weight ratio of the dispersant, wetting agent and stabilizer is (3 - 7):(3 - 6):(3 - 6).

21. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The weight ratio of the dispersant, wetting agent and stabilizer is (3 - 5):(3 - 4):(5 - 6).

22. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that The weight ratio of the dispersant, wetting agent and stabilizer is (5 - 9):(4 - 6):(3 - 5).

23. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that, The weight ratio of the dispersant, wetting agent and stabilizer is (5 - 7):(4 - 6):(3 - 5).

24. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The weight ratio of the dispersant, wetting agent and stabilizer is 5:4:

5.

25. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that The wettable powder for pesticide sterilization comprises raw materials with the following weight percentages: chlorothalonil 50%, tebuconazole 1 - 5%, picoxystrobin 1 - 5%, sodium styrene acrylic copolymer 3%, sodium lignosulfonate 2 - 6%, wetting agent 4 - 6%, silica white 3 - 5%, and talcum powder to make up 100%.

26. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that, The wettable powder for pesticide sterilization comprises raw materials with the following weight percentages: chlorothalonil 50%, tebuconazole 1%, picoxystrobin 1%, sodium styrene acrylic copolymer 3%, sodium lignosulfonate 2 - 4%, sodium diisooctyl sulfosuccinate 4 - 6%, silica white 3 - 5%, and talcum powder to make up 100%.

27. The wettable powder for pesticide bactericidal action according to any one of claims 1 to 12, characterized in that, The wettable powder for pesticide sterilization comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 3.3%, sodium naphthalene sulfonate formaldehyde condensate 1 - 3%, alkyl naphthalene sulfonate formaldehyde condensate 2 - 4%, wetting agent 3 - 4%, silica white 3 - 6%, and talcum powder 22.7% - 48%.

28. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that, The wettable powder for pesticide sterilization comprises raw materials with the following weight percentages: chlorothalonil 30 - 54%, tebuconazole 1 - 6%, picoxystrobin 1 - 3.3%, sodium naphthalene sulfonate formaldehyde condensate 1 - 3%, alkyl naphthalene sulfonate formaldehyde condensate 2 - 4%, wetting agent 3 - 4%, silica white 5 - 6%, and talcum powder 22.7% - 48%.

29. The wettable powder for pesticide sterilization according to any one of claims 1 to 12, characterized in that The wettable powder for pesticide sterilization comprises raw materials with the following weight percentages: chlorothalonil 54%, tebuconazole 6%, picoxystrobin 3.3%, sodium naphthalene sulfonate formaldehyde condensate 3%, alkyl naphthalene sulfonate formaldehyde condensate 2%, sodium dioctyl sulfosuccinate 4%, white carbon black 5%, and talcum powder 22.7%.

30. A method for preparing the wettable powder for pesticide bactericidal action according to any one of claims 1 to 29, characterized in that, Comprising: Mix chlorothalonil, tebuconazole, picoxystrobin, dispersant, wetting agent, stabilizer, and filler evenly, and perform ultrafine air flow pulverization. After mixing the obtained fine powder, a wettable powder of chlorothalonil, tebuconazole, and picoxystrobin is obtained.

31. The preparation method according to claim 30, wherein, After ultrafine air flow pulverization, fine powder with a particle size of 400 - 800 mesh is obtained.

32. A method for using the wettable powder for pesticide sterilization according to any one of claims 1 to 29 or the wettable powder for pesticide sterilization prepared by the preparation method according to claim 30 or 31, characterized in that, The wettable powder is diluted with water and applied by spraying.

33. The usage method according to claim 32, characterized in that, The dilution multiple is 500 - 750 times.

34. Application of the wettable powder according to any one of claims 1 to 29, or the wettable powder prepared by the preparation method according to claim 30 or 31 in preventing and controlling farmland plant diseases, wherein the plant diseases include one or more of downy mildew, powdery mildew, gray mold, and rust.

35. The application according to claim 34, wherein The plant diseases include one or more of grape downy mildew, wheat powdery mildew, and soybean rust.

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