Fluxapyroxad-epoxiconazole suspending agent as well as preparation method and application thereof

Abstract

The invention belongs to the field of pesticide preparations, and particularly relates to a pydiflumetofen-epoxiconazole suspending agent as well as a preparation method and application thereof. The preparation consists of the following raw materials in percentage by mass: 3-40% of an active component, 6-10% of a dispersing agent, 1-3% of a penetrating agent, 1-3% of a thickening agent, 1.5-2% of a synergist, 3-5% of an anti-freezing agent, 0.2-0.3% of a defoaming agent, 0.2-0.5% of a pH regulator, 0.1-0.3% of an antioxidant and the balance of water. By screening a suspending agent system, the prepared pydiflumetofen-epoxiconazole suspending agent is excellent in stability, the influence of environmental change on the preparation in the storage process is effectively reduced, and the traditional problems of caking, devitrification and the like of the preparation are avoided to the greatest extent.

Description

Technical Field

[0001] The invention belongs to the field of pesticide preparations, and particularly relates to a fluopicolide-epoxiconazole suspension concentrate and a preparation method and application thereof. Background Art

[0002] The chemical name of pydiflumetofen (common name: pydiflumetofen; trade names: Adepidyn, Miravis, etc.) is: 3-(difluoromethyl)- N -methoxy-1-methyl- N -[( RS )-1-methyl-2-(2,4,6-trichlorophenyl)ethyl]-1 H -pyrazole-4-carboxamide. CAS registration number: 1228284-64-7; molecular formula: C 16 H 16 Cl3F2N3O2. Fluoxetine is a pathogen respiration inhibitor that inhibits mitochondrial function by interfering with the tricarboxylic acid cycle on complex II of the respiratory electron transport chain, preventing it from producing energy and inhibiting the growth of pathogens, ultimately leading to their death. Fluoxetine is highly effective and broad-spectrum, and is used in cereals (including wheat, barley, oats, rye, triticale, etc.), corn, soybeans, vegetables, peanuts, rapeseed, quinoa, melons, dry peas and beans, fruit trees, specialty crops, lawns, ornamental plants, etc. to control diseases caused by Fusarium ( Fusarium spp.), Cercospora ( Cercospora spp.), Botrytis cinerea ( Botrytis spp.), Alternaria ( Alternaria spp.) and many other diseases caused by pathogens, such as powdery mildew, leaf spot, brown spot, target spot, web spot, moire, leaf blight, gray mold, scab, bakanae, sclerotinia, black shank, early blight, black spot, and scab. It is mainly sprayed on the leaves and is also used for seed treatment.

[0003] Flupyraclostrobin has the highest activity against leaf spot and powdery mildew in crops, but its single site of action necessitates urgent solutions to expand its control spectrum and delay the development of resistance. Furthermore, currently available suspension concentrates of flupyraclostrobin exhibit poor suspension stability, and the technical product is prone to flocculation and aggregation. Summary of the Invention

[0004] In view of the problems existing in the prior art, the present invention provides a fluopicolide-epoxiconazole suspension concentrate.

[0005] The present invention also provides a preparation method of the above-mentioned fluopicolide-epoxiconazole suspension concentrate.

[0006] Another object of the present invention is to provide the use of the above-mentioned fluopicolide-epoxiconazole suspension concentrate in preventing and controlling peanut white rot.

[0007] The technical solutions adopted by the present invention to achieve the above-mentioned purpose are as follows: The invention provides a fluopicolide-epoxiconazole suspension concentrate, which is composed of the following raw materials in percentage by weight: 3-40% of active ingredient, 6-10% of dispersant, 1-3% of penetrant, 1-3% of thickener, 1.5-2% of synergist, 3-5% of antifreeze agent, 0.2-0.3% of defoamer, 0.2-0.5% of pH regulator, 0.1-0.3% of antioxidant, and the balance of water.

[0008] Preferably, the active ingredients are fluopicolide and epoxiconazole in a mass ratio of 1:1.

[0009] Preferably, the dispersant is composed of EO / PO block polyether and benzenesulfonate formaldehyde condensate in a mass ratio of 1-2:1.

[0010] Preferably, the penetrant is sodium salt of α-olefin sulfonate.

[0011] Preferably, the thickener is modified xanthan gum.

[0012] Preferably, the synergist is carvacrol.

[0013] Preferably, the antifreeze agent is propylene glycol; the defoaming agent is a silicone defoaming agent; the pH regulator is a phosphate buffer; and the antioxidant is tert-butylhydroquinone.

[0014] The present invention also provides a method for preparing the above-mentioned fluopicolide-epoxiconazole suspension concentrate, comprising the following steps: uniformly mixing an active ingredient, 50% of a dispersant, 50% of a defoamer, and 20-40% of water, and sand-milling the mixture; adding the remaining dispersant, defoamer, synergist, thickener, and antifreeze during the sand-milling process; and adding the remaining raw materials after the particle size D90 is less than 3 μm; and continuing to grind the mixture until the particle size D90 is less than 2 μm to obtain the suspension concentrate.

[0015] The present invention further provides the use of the above-mentioned fluopicolide-epoxiconazole suspension concentrate in preventing and controlling peanut white rot.

[0016] The modified xanthan gum used in the present invention is prepared by the following method: 2 parts of xanthan gum are added to 100 parts of deionized water, stirred and dissolved, and then pre-cooled (treated at -20°C for 20-24 hours), then restored to room temperature, and 0.1 parts of octyltrimethylammonium chloride are slowly added dropwise under stirring, heated to 45-50°C, and stirred for 3-4 hours to obtain the product.

[0017] The EO / PO block polyether used in the present invention was purchased from Kelong Co., Ltd.; its average molecular weight was 1850 and its viscosity (25° C.) was 310.

[0018] The beneficial effects of the present invention are: (1) The present invention significantly improves the control effect of peanut white rot by screening fluopicolide and epoxiconazole based on the different target sites of the two ingredients, and can reduce the amount of pesticides applied and slow down drug resistance; (2) The present invention screens the suspension system to prepare the fluopicolide-epoxiconazole suspension concentrate, which has excellent stability and effectively reduces the impact of environmental changes on the preparation during storage, and avoids the traditional problems of agglomeration and crystallization of the preparation to the greatest extent; (3) The present invention greatly improves the antibacterial effect of fluopicolide and epoxiconazole by creatively adding synergistic adjuvants, reduces the application amount of the agents, reduces the cost of use, and improves the dispersibility and suspension rate of the overall preparation. DETAILED DESCRIPTION

[0019] The technical content of the present invention is further explained below through specific examples, but the essence of the present invention is not limited to the following examples.

[0020] Example 1 A fluopicolide-epoxiconazole suspension concentrate is composed of the following raw materials in percentage by weight: 10% active ingredient (fluopicolide and epoxiconazole in a mass ratio of 1:1), 8% dispersant, 2% penetrant, 2.5% thickener, 2% synergist, 4% antifreeze, 0.2% defoamer, 0.2% pH regulator, 0.1% antioxidant, and the balance water.

[0021] The specific components of each raw material are shown in Table 1.

[0022] The specific preparation method is: the active ingredient, 50% dispersant, 50% defoaming agent and 40% water are mixed and stirred evenly, and sand-milled. During the sand-milling process, the remaining dispersant, defoaming agent, synergist, thickener and antifreeze are added. After the particle size D90 is less than 3 μm, the remaining raw materials are added and the grinding is continued until the particle size D90 is less than 2 μm.

[0023] Example 2-Example 3 and Comparative Example The suspension concentrates of Examples 2-3 and Comparative Examples 1-3 were prepared according to the ratio of the raw materials in Table 1. The specific preparation method was as described in Example 1.

[0024] Table 1 Effect Verification Example 1 The test was conducted according to Method 2 of the standard "Determination of Suspension Rate of Pesticides" (GB / T 14825-2006). The concentration of the active ingredient in each test sample provided by the present invention was prepared by diluting the composite formulations prepared in the Examples and Comparative Examples with water 4000 times using the double dilution method. The relevant data were processed according to the methods specified in the standard. The suspension rate was calculated as follows: ; Wherein: m1 is the mass of the active ingredient in the sample taken to prepare the suspension, in grams (g); m2 is the mass of the active ingredient in the 25mL suspension remaining at the bottom of the graduated cylinder, in grams (g); the suspensions prepared in each embodiment and comparative example were stored in a 54±2°C constant temperature oven for 14 days and then returned to room temperature before being tested for suspension rate; simultaneously, the suspensions were stored at 0±2°C constant temperature for 7 days and then returned to room temperature before being tested for fluidity. The test results are shown in Table 2.

[0025] Table 2 It can be seen from Table 2 that the suspending agent provided by the present invention can still maintain good fluidity and suspension rate after heat storage.

[0026] Effect Verification Example 2 (1) Test location and basic information: The experiment was conducted in Luojiazhuang Village, Yicheng Street, Yishui County, Linyi City, Shandong Province in 2024. The peanut variety was Shanhua 11, and it was sown on May 17, 2024.

[0027] Peanut planting specifications are: ridge spacing 80cm, ridge width 55cm, row spacing 30cm, hole spacing 16.5cm, and peanut density 135,000 holes / hm2 2 , 2 seeds per hole, covered with film for cultivation.

[0028] (II) Experimental treatment and method: The composite preparations prepared in Example 1 and Comparative Example 2 were added at 30 ml / mu; There were 3 treatments in total, each treatment was repeated 3 times, and there were 21 plots in total, with a plot area of ​​30 m 2 Prepare the solution at a rate of 200 L per mu (approximately 1.5 acres) and apply it by spraying the roots at the early stages of peanut white rot (early pod formation, July 15). Ten days after the first application (due to rainfall, the actual application was July 24), apply the solution again using the same method and dosage, for a total of two applications. A clear water control group was established.

[0029] (3) Survey content and methods (1) Safety investigation Observe the growth potential of peanuts in the pesticide-treated area and any pesticide damage that occurs.

[0030] (2) Investigation on the effectiveness of prevention and control Fifteen days after the second spraying, the incidence of white rot in each plot was investigated. The central three ridges of each plot were surveyed, with 50 holes in each ridge, for a total of 150 holes and 300 plants. Disease severity and control effectiveness were graded plant by plant, and the significance of control effectiveness was measured. The number of diseased plants at each level and the severity of disease were recorded. The disease grading scale, based on Dong Weibo's method, was used on a five-level scale from 0 to 7: Grade 0: no symptoms; Grade 1: lesions only at the base of the stem; Grade 3: constriction at the base of the stem, with less than one-third of the plant showing systemic symptoms (such as wilt, death, and wilting); Grade 5: less than two-thirds of the plant showing systemic symptoms; and Grade 7: more than two-thirds of the plant showing systemic symptoms. Disease index and control effectiveness were calculated.

[0031] Disease rate (%) = number of diseased plants / total number of plants surveyed × 100 Disease index (%) = [∑(disease level × number of diseased plants at that level) / (highest disease level × total number of plants surveyed)] × 100 Control effect (%) = [(control disease index - treatment disease index) / control disease index] × 100 (IV) Test results and analysis (1) Safety survey results The peanuts in the treatment areas of each drug grew well, and no symptoms of drug damage or growth inhibition were found.

[0032] (2) Effect of pesticide control Table 3 Test results of new pesticides for controlling peanut white rot

Claims

1. A fluopicolide-epoxiconazole suspension concentrate, characterized in that: The invention is composed of the following raw materials in percentage by weight: 3-40% active ingredient, 6-10% dispersant, 1-3% penetrant, 1-3% thickener, 1.5-2% synergist, 3-5% antifreeze, 0.2-0.3% defoaming agent, 0.2-0.5% pH regulator, 0.1-0.3% antioxidant and the balance water.

2. The oxapoxetine-epoxiconazole suspension concentrate according to claim 1, characterized in that The active ingredients are fluopicolide and epoxiconazole in a mass ratio of 1:

1.

3. The fluopicolide-epoxiconazole suspension concentrate according to claim 1 or 2, characterized in that The dispersant is composed of EO / PO block polyether and benzenesulfonate formaldehyde condensate in a mass ratio of 1-2:

1.

4. The oxaflor-epoxiconazole suspension concentrate according to any one of claims 1 to 3, characterized in that The penetrant is α-olefin sulfonic acid sodium salt.

5. The oxaflor-epoxiconazole suspension concentrate according to claim 1, characterized in that The thickener is modified xanthan gum.

6. The oxaflor-epoxiconazole suspension concentrate according to claim 1, characterized in that The synergist is carvacrol.

7. The oxaflor-epoxiconazole suspension concentrate according to claim 1, characterized in that The antifreeze agent is propylene glycol; the defoaming agent is an organosilicon defoaming agent; the pH regulator is a phosphate buffer; and the antioxidant is tert-butylhydroquinone.

8. A method for preparing the oxapoxetine-epoxiconazole suspension concentrate according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: mixing the active ingredient, 50% of a dispersant, 50% of a defoaming agent and 20-40% of water, stirring the mixture evenly, and sand-grinding the mixture; adding the remaining dispersant, defoaming agent, synergist, thickener and antifreeze during the sand-grinding process; adding the remaining raw materials after the particle size D90 is less than 3 μm; and continuing to grind the mixture until the particle size D90 is less than 2 μm.

9. Use of the fluopicolide-epoxiconazole suspension concentrate according to any one of claims 1 to 7 in preventing and controlling peanut white rot.

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