A pesticide composition containing validamycin a and prothioconazole and a preparation method thereof

Abstract

This application relates to the technical field of pesticide formulations, and in particular to a pesticide composition containing jinggangmycin and prothioconazole and its preparation method; a pesticide composition comprising the following raw materials in parts by weight: 2-8 parts jinggangmycin, 8-15 parts prothioconazole, 2-6 parts capsule wall material, 1-5 parts emulsifier, 3-6 parts dispersant, 1-15 parts solvent, 0.1-0.8 parts thickener, 1-5 parts film-forming agent, 2-5 parts antifreeze, 0.1-0.5 parts preservative, and 50-80 parts water; this application combines jinggangmycin and prothioconazole, and through the synergistic effect of jinggangmycin and prothioconazole, it has a good control effect on wheat scab; the pesticide composition containing jinggangmycin and prothioconazole prepared in this application has no adverse effects on wheat growth, preventing wheat from being attacked by pathogens during growth, thus exhibiting good growth and increased yield.

Description

Technical Field

[0001] This application relates to the technical field of pesticide formulations, and in particular to a pesticide composition containing jinggangmycin and prothioconazole and a method for preparing the same. Background Technology

[0002] Wheat is an important food crop widely cultivated globally, with a large planting scale and wide application. Wheat scab is a typical fungal disease that is extremely harmful. Affected by multiple factors such as climate change and changes in field farming methods, the occurrence range of this disease continues to expand and the frequency of outbreaks continues to increase, seriously affecting the stability of wheat yield and the quality of wheat grains.

[0003] Currently, chemical control is the core method for controlling wheat scab in the field. Multi-component compound fungicides, with their synergistic effects, have become the mainstream products for pesticide registration and field application. Among them, prothioconazole and jinggangmycin are representative agents for controlling wheat scab, but both have significant technical defects when applied alone, and cannot meet the needs of efficient, stable, and green field control.

[0004] Prothioconazole, as a novel triazole thion fungicide, possesses excellent systemic activity and disease control efficacy, and is highly effective in controlling wheat scab. However, long-term, single, and continuous application can easily induce high resistance in pathogens, leading to a gradual decline in the efficacy of the agent. At the same time, the ability of prothioconazole alone to inhibit DON toxin in wheat grains is limited, and it cannot fundamentally solve the problem of excessive toxin levels, indicating a significant weakness in the control system.

[0005] Jinggangmycin, a natural biological antibiotic fungicide, can control diseases by inhibiting chitin synthesis in pathogens and inducing disease resistance in wheat plants. It also has a certain inhibitory effect on DON toxin, demonstrating significant advantages in its green and safe properties. However, when applied alone, this agent suffers from weak fungicidal activity, poor speed of action, and short duration of effect. As a single agent, it is difficult to effectively curb the infection and spread of Fusarium head blight, resulting in poor overall control in the field.

[0006] To compensate for the shortcomings of single-agent applications, research on compound formulations has emerged in the existing technology. However, existing compound formulations suffer from several core technical drawbacks. On the one hand, most compound formulation designs lack scientific rigor and specificity, with unreasonable ratio parameters, preventing the two agents from achieving synergistic effects, resulting in insignificant improvements in disease control and unsatisfactory treatment of drug resistance and toxin inhibition. On the other hand, existing compound product systems exhibit extremely poor stability, with problems such as uneven drug dispersion, easy stratification, easy sedimentation, and easy aggregation of active ingredients.

[0007] The aforementioned defects result in a significant decrease in the dispersibility and adhesion to crop surfaces of existing compound formulations when applied in the field. This not only severely reduces the actual control effect of wheat scab, but also fails to effectively inhibit the accumulation of DON toxin and delay the development of pathogen resistance. Furthermore, uneven dispersion of the agent can lead to localized excessive pesticide residues, increasing the pressure on the agricultural ecological environment and making it difficult to meet the industry's development needs for efficient control of wheat scab, pesticide reduction, and green and safe production.

[0008] Therefore, how to effectively solve the technical problems of poor control effect of single agents, easy development of drug resistance, weak inhibition of DON toxin, and poor stability of compound formulation systems has become an urgent technical problem to be solved in the field of green and efficient control of wheat scab. Summary of the Invention

[0009] To address the shortcomings of existing technologies, this application provides a pesticide composition containing jinggangmycin and prothioconazole, which has a scientific formulation, excellent stability, and a reasonable preparation process, and can achieve synergistic effects, significant toxicity reduction, and environmentally friendly dosage reduction, as well as a method for its preparation.

[0010] In a first aspect, this application provides a pesticide composition, which adopts the following technical solution: A pesticide composition comprising the following raw materials in parts by weight: 2-8 parts of jinggangmycin, 8-15 parts of prothioconazole, 2-6 parts of capsule wall material, 1-5 parts of emulsifier, 3-6 parts of dispersant, 1-15 parts of solvent, 0.1-0.8 parts of thickener, 1-5 parts of film-forming agent, 2-5 parts of antifreeze, 0.1-0.5 parts of preservative, and 50-80 parts of water.

[0011] By adopting the above technical solution, this application uses a combination of jinggangmycin and prothioconazole. The two have complementary mechanisms of action. Jinggangmycin inhibits the synthesis of chitin in pathogens, induces disease resistance in wheat, and inhibits the synthesis of DON toxin. Prothioconazole inhibits the synthesis of ergosterol in pathogens and has protective, curative, and eradicative activities. The synergistic effect is significant. Compared with the use of prothioconazole alone, the dosage of prothioconazole can be reduced, which not only reduces the cost of medication but also effectively delays the development of drug resistance in pathogens. The combined agent has a significant synergistic effect.

[0012] This application uses a combination of jinggangmycin and prothioconazole. This ratio was determined through extensive indoor toxicity tests and field efficacy trials, achieving optimal synergistic effects and overcoming the shortcomings of single-component formulations. The combination of bio-derived jinggangmycin and the chemical fungicide prothioconazole aligns with the policy requirements of pesticide reduction and green development, reducing the use of chemical pesticides, lowering pesticide residues and environmental pressure, and having no adverse effects on wheat growth. In fact, it promotes robust wheat growth, achieving multiple benefits including disease prevention, toxicity reduction, pesticide use reduction, and yield increase.

[0013] Preferably, the film-forming agent comprises the following raw materials in parts by weight: 2-8 parts carboxymethyl cellulose, 1-5 parts glycerol (first part), 0.5-1.5 parts expanded perlite, 0.1-0.5 parts gallnut tannin, 3-7 parts corn starch, 8-12 parts glycerol (second part), 30-50 parts chitosan, 0.3-0.7 parts titanium dioxide, and 1-2 parts silane coupling agent.

[0014] Preferably, the preparation method of the film-forming agent includes the following steps: Carboxymethyl cellulose and the first portion of glycerol were mixed, and then expanded perlite and gallnut tannin were added and mixed to obtain the first mixture; After gelatinizing the corn starch, add the second part of glycerol and mix. Then add chitosan and titanium dioxide and mix to obtain the second mixture. The first mixture, the second mixture, and the silane coupling agent are mixed to obtain a film-forming agent.

[0015] By adopting the above technical solution, in the preparation of the first mixture, carboxymethyl cellulose and glycerol are compounded to form a basic polymer matrix, and hydrogen bonding is carried out with the polyphenolic hydroxyl structure of gallnut tannin to construct a rigid skeleton with high initial viscoelasticity and cohesive strength; in the preparation of the second mixture, corn starch is gelatinized to form a flexible gel network, which, together with the cationic film-forming properties of chitosan and the nano-reinforcing effect of titanium dioxide, constructs a tough barrier with excellent flexibility and photothermal shielding function.

[0016] This application combines a first mixture with a second mixture, and under the chemical mediation of a silane coupling agent, achieves a structural leap from heterogeneous blending to a through-penetrating polymer network. The silane coupling agent plays a key role as a molecular bridge; its hydrolyzed silanol groups undergo dehydration condensation with the hydroxyl groups on the surfaces of expanded perlite and titanium dioxide, respectively, forming strong Si-O-Si or Si-O-Ti covalent bonds to anchor the inorganic phase. At the same time, its organic functional groups undergo covalent cross-linking or strong hydrogen bonding with the active sites of carboxymethyl cellulose, gelatinized starch, and chitosan, completely eliminating organic-inorganic interface defects and significantly improving stress transfer efficiency. This synergistic film-forming mechanism not only promotes the close packing of large-sized expanded perlite and small-sized titanium dioxide in the continuous phase, effectively blocking the permeation paths of gas and moisture, but also endows the final product with both high strength and high toughness. At the same time, the cross-linking and binding of the multi-network structure effectively inhibits the slippage and cold flow of polymer chain segments. Combined with the photothermal stability of titanium dioxide and the antioxidant properties of tannins, this film-forming agent can form a dense protective film with excellent barrier properties, mechanical strength and long-term service stability in complex environments.

[0017] Preferably, the emulsifier is at least one of castor oil polyoxyethylene ether, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monostearate, sodium alkylphenol ether sulfosuccinate, calcium dodecylbenzene sulfonate, phenethylphenol polyoxyethylene ether, and tea polyphenols.

[0018] Preferably, the dispersant is at least one of sodium lignosulfonate, calcium lignosulfonate, sodium methylnaphthalenesulfonate formaldehyde condensate, dispersant powder, polycarboxylate, alkylnaphthalenesulfonate, and sodium methylenebismethylnaphthalenesulfonate polymer.

[0019] Preferably, the solvent is at least one of S-200# solvent oil, S-100# solvent oil, toluene, and xylene.

[0020] Preferably, the thickener is at least one selected from xanthan gum, polyvinyl alcohol, magnesium aluminum silicate, gum arabic, sodium alginate, fatty alcohol polyoxyethylene ether, polyacrylamide, and bentonite.

[0021] Preferably, the antifreeze is at least one of ethylene glycol, propylene glycol, and glycerin.

[0022] Preferably, the preservative is at least one of potassium sorbate, benzoic acid, methylparaben, 1,2-benzisothiazolin-3-one, methylisothiazolinone, and Kathon.

[0023] Secondly, this application provides an application of an agricultural fungicide containing a pesticide composition in the control of wheat scab, employing the following technical solution: Application of an agricultural fungicide containing the above-mentioned pesticide composition in the control of wheat scab.

[0024] Preferably, the agricultural fungicide is a microcapsule suspension or a microcapsule suspension-suspension.

[0025] Preferably, when the agricultural fungicide is a microcapsule suspension, the preparation method steps are as follows: (1) Weigh each ingredient according to the formula; (2) Add prothioconazole, capsule wall material, and emulsifier to a solvent and mix to obtain an oil phase; (3) Mix the dispersant and water to obtain an aqueous phase; (4) The oil phase is added to the aqueous phase for shear emulsification to obtain an emulsion with an average particle size between 0.5 and 2 μm; (5) Add jinggangmycin, film-forming agent, antifreeze and preservative to the emulsion and mix, then add thickener and mix to obtain microcapsule suspension containing jinggangmycin and prothioconazole.

[0026] Preferably, when the agricultural fungicide is a microcapsule suspension, the capsule wall material includes capsule wall material one and capsule wall material two.

[0027] Preferably, the preparation method of the microcapsule suspension-suspension agent includes the following steps: (a) Weigh each ingredient according to the formula; (b) Mix capsule wall material one and castor oil in 0.1-1 parts by weight to obtain modified capsule wall material one; (c) Mix the emulsifier, 1 / 2 dispersant, and water to obtain an aqueous phase; (d) Mix prothioconazole and solvent to obtain an oil phase. Add modified capsule wall material I and aqueous phase to the oil phase, mix and emulsify, then add capsule wall material II and stir to solidify to obtain a primary emulsion. (e) Add jinggangmycin, film-forming agent, antifreeze, 1 / 2 dispersant and preservative to the colostrum and mix, then add thickener and mix to obtain microcapsule suspension-suspension containing jinggangmycin and prothioconazole.

[0028] In summary, this application includes at least one of the following beneficial technical effects: This application combines jinggangmycin and prothioconazole, and through the synergistic effect of jinggangmycin and prothioconazole, it has a good control effect on wheat scab. This application significantly improves the stability of compound pesticide compositions by selecting and proportioning specific compound adjuvants and combining them with optimized preparation processes; The pesticide composition containing jinggangmycin and prothioconazole prepared in this application has no adverse effects on wheat growth, preventing wheat from being attacked by pathogens during its growth process, thus exhibiting good growth and increasing yield. Detailed Implementation

[0029] The technical solutions of this application are further illustrated by specific embodiments below. These specific embodiments do not represent a limitation on the scope of protection of this application. Any non-essential modifications and adjustments made by others based on the concept of this application still fall within the scope of protection of this application.

[0030] All raw materials involved in this application are commercially available products, among which, Carboxymethyl cellulose, purchased from Merck; Expanded perlite, 50-100μm, Xinyang Guangtong Engineering Technology Co., Ltd. Gallnut tannin, CAS No.: 1401-55-4; Corn starch, food grade, Shanghai Guoran Seasoning Food Co., Ltd. Chitosan, degree of deacetylation 80%-95%, Sinopharm Chemical Reagent Co., Ltd. Titanium dioxide, nano titanium dioxide, Shanghai Zhanyun Chemical Co., Ltd.; Sodium methylnaphthalene sulfonate formaldehyde condensate (dispersant MF), CAS No. 9084-06-4; Xanthan gum, CAS No.: 11138-66-2; Diphenylmethane diisocyanate, CAS No.: 26447-40-5; Phenethylphenol polyoxyethylene ether, pesticide emulsifier 600#; The present application will be further described in detail below with reference to embodiments and comparative examples.

[0031] Preparation Example 1:

[0032] The preparation method of the film-forming agent is as follows: Mix 5 kg of carboxymethyl cellulose, 3 kg of glycerol, and 100 kg of water at 50°C for 30 minutes, cool to room temperature, add 1 kg of expanded perlite and 0.3 kg of gallnut tannin, and mix for 20 minutes to obtain the first mixture; Mix 5 kg of corn starch and 100 kg of water, gelatinize at 85°C for 45 minutes, cool to room temperature, add 10 kg of glycerin and mix for 40 minutes, then add 40 kg of chitosan, 0.5 kg of titanium dioxide and 300 kg of water and mix to obtain the second mixture. The first mixture, the second mixture, and 1.5 kg of silane coupling agent KH-560 were mixed to obtain a film-forming agent.

[0033] Preparation Example 2:

[0034] The preparation method of the film-forming agent is as follows: 2 kg of carboxymethyl cellulose, 1 kg of glycerol, and 100 kg of water were mixed at 50°C for 30 minutes, cooled to room temperature, and then 0.5 kg of expanded perlite and 0.1 kg of gallnut tannin were added and mixed for 20 minutes to obtain the first mixture. Mix 3 kg of corn starch and 100 kg of water, gelatinize at 85°C for 45 minutes, cool to room temperature, add 8 kg of glycerol and mix for 40 minutes, then add 30 kg of chitosan, 0.3 kg of titanium dioxide and 300 kg of water and mix to obtain the second mixture; The first mixture, the second mixture, and 1 kg of silane coupling agent KH-560 were mixed to obtain a film-forming agent.

[0035] Preparation Example 3:

[0036] The preparation method of the film-forming agent is as follows: Mix 8 kg of carboxymethyl cellulose, 5 kg of glycerol, and 100 kg of water at 50°C for 30 minutes, cool to room temperature, add 1.5 kg of expanded perlite and 0.5 kg of gallnut tannin, and mix for 20 minutes to obtain the first mixture; Mix 7 kg of corn starch and 100 kg of water, gelatinize at 85°C for 45 minutes, cool to room temperature, add 12 kg of glycerol and mix for 40 minutes, then add 50 kg of chitosan, 0.7 kg of titanium dioxide and 300 kg of water and mix to obtain the second mixture. The first mixture, the second mixture, and 2 kg of silane coupling agent KH-560 were mixed to obtain a film-forming agent.

[0037] Example 1:

[0038] A microcapsule suspension containing jinggangmycin and prothioconazole, the microcapsule suspension comprising the following raw materials: 5 kg jinggangmycin, 12 kg prothioconazole, 4 kg capsule wall material, 3 kg emulsifier, 5 kg dispersant, 4 kg solvent, 0.4 kg thickener, 3 kg film-forming agent, 4 kg antifreeze, 0.3 kg preservative, and 65 kg water.

[0039] The capsule wall material is polymethylene polyphenyl isocyanate (PM-200).

[0040] The emulsifier is Tween 60.

[0041] The dispersant is sodium methylnaphthalene sulfonate formaldehyde condensate (dispersant MF).

[0042] The solvent is S-200# solvent oil.

[0043] The thickener is xanthan gum.

[0044] The antifreeze is a mixture of propylene glycol and glycerin; the mass ratio of propylene glycol to glycerin is 1:1.5.

[0045] The preservative is benzoic acid.

[0046] The film-forming agent was prepared in Preparation Example 1.

[0047] A method for preparing a microcapsule suspension containing jinggangmycin and prothioconazole, comprising the following steps: Step 1: Weigh out each ingredient according to the recipe; Step 2: Add prothioconazole, capsule wall material, and emulsifier to the solvent and mix to obtain the oil phase; Step 3: Mix the dispersant and water to obtain the aqueous phase; Step 4: Pour the oil phase into the aqueous phase and shear emulsify at a speed ≥2000 r / min to obtain an emulsion with an average particle size between 0.5-2 μm; Step 5: After reacting the emulsion at 30℃ and 250r / min for 1 hour, the temperature is raised to 35℃ and reacted for 0.5 hours, and then raised to 40℃ and reacted for 1.5 hours. Jinggangmycin, film-forming agent, antifreeze agent, and preservative are added and stirred for 1 hour. Thickener is then added and stirring is continued for 1.5 hours to obtain a microcapsule suspension containing jinggangmycin and prothioconazole.

[0048] Example 2:

[0049] A microcapsule suspension containing jinggangmycin and prothioconazole, the microcapsule suspension comprising the following raw materials: 2 kg jinggangmycin, 8 kg prothioconazole, 2 kg capsule wall material, 1 kg emulsifier, 3 kg dispersant, 1 kg solvent, 0.1 kg thickener, 1 kg film-forming agent, 2 kg antifreeze, 0.1 kg preservative, and 50 kg water.

[0050] The capsule wall material is capsule wall material PM-200.

[0051] The emulsifier is Tween 60; The dispersant is dispersant MF; The solvent is S-200# solvent oil; The thickener is xanthan gum; The antifreeze is a mixture of propylene glycol and glycerin; the mass ratio of propylene glycol to glycerin is 1:1.5.

[0052] The preservative is benzoic acid.

[0053] The film-forming agent was prepared in Preparation Example 2.

[0054] A method for preparing a microcapsule suspension containing jinggangmycin and prothioconazole, comprising the following steps: Step 1: Weigh out each ingredient according to the recipe; Step 2: Add prothioconazole, capsule wall material, and emulsifier to the solvent and mix to obtain the oil phase; Step 3: Mix the dispersant and water to obtain the aqueous phase; Step 4: Pour the oil phase into the aqueous phase and shear emulsify at a speed ≥2000 r / min to obtain an emulsion with an average particle size between 0.5-2 μm; Step 5: After reacting the emulsion at 30℃ and 250r / min for 1 hour, the temperature is raised to 35℃ and reacted for 0.5 hours, and then raised to 40℃ and reacted for 1.5 hours. Jinggangmycin, film-forming agent, antifreeze agent, and preservative are added and stirred for 1 hour. Thickener is then added and stirring is continued for 1.5 hours to obtain a microcapsule suspension containing jinggangmycin and prothioconazole.

[0055] Example 3:

[0056] A microcapsule suspension containing jinggangmycin and prothioconazole, the microcapsule suspension comprising the following raw materials: 8 kg of jinggangmycin, 15 kg of prothioconazole, 6 kg of capsule wall material, 5 kg of emulsifier, 6 kg of dispersant, 8 kg of solvent, 0.8 kg of thickener, 5 kg of film-forming agent, 5 kg of antifreeze, 0.5 kg of preservative, and 80 kg of water.

[0057] The capsule wall material is capsule wall material PM-200.

[0058] The emulsifier is Tween 60.

[0059] The dispersant is dispersant MF.

[0060] The solvent is S-200# solvent oil.

[0061] The thickener is xanthan gum.

[0062] The antifreeze is a mixture of propylene glycol and glycerin; the mass ratio of propylene glycol to glycerin is 1:1.5.

[0063] The preservative is benzoic acid.

[0064] The film-forming agent was prepared in Preparation Example 3.

[0065] A method for preparing a microcapsule suspension containing jinggangmycin and prothioconazole, comprising the following steps: Step 1: Weigh out each ingredient according to the recipe; Step 2: Add prothioconazole, capsule wall material, and emulsifier to the solvent and mix to obtain the oil phase; Step 3: Mix the dispersant and water to obtain the aqueous phase; Step 4: Pour the oil phase into the aqueous phase and shear emulsify at a speed ≥2000 r / min to obtain an emulsion with an average particle size between 0.5-2 μm; Step 5: After reacting the emulsion at 30℃ and 250r / min for 1 hour, the temperature is raised to 35℃ and reacted for 0.5 hours, and then raised to 40℃ and reacted for 1.5 hours. Jinggangmycin, film-forming agent, antifreeze agent, and preservative are added and stirred for 1 hour. Thickener is then added and stirring is continued for 1.5 hours to obtain a microcapsule suspension containing jinggangmycin and prothioconazole.

[0066] Example 4:

[0067] The difference from Example 1 is that the amount of film-forming agent added is 1 kg.

[0068] Example 5:

[0069] The difference from Example 1 is that the amount of film-forming agent added is 5 kg.

[0070] Example 6:

[0071] A microcapsule suspension-suspension agent containing jinggangmycin and prothioconazole comprises the following raw materials: 6 kg of jinggangmycin, 11 kg of prothioconazole, 4 kg of capsule wall material, 3 kg of emulsifier, 4 kg of dispersant, 13 kg of solvent, 0.5 kg of thickener, 3 kg of film-forming agent, 3 kg of antifreeze, 0.3 kg of preservative, and 65 kg of water.

[0072] The capsule wall material includes 2 kg of capsule wall material one and 2 kg of capsule wall material two; The capsule wall material is diphenylmethane diisocyanate; The second capsule wall material is ethylenediamine; The emulsifier is composed of calcium dodecylbenzenesulfonate and phenylethylphenol polyoxyethylene ether in a mass ratio of 1:0.5.

[0073] The dispersant is sodium lignosulfonate; The solvent is S-200# solvent oil; The thickener is xanthan gum; The antifreeze is a mixture of propylene glycol and glycerin; the mass ratio of propylene glycol to glycerin is 1:1.5.

[0074] The preservative is benzoic acid.

[0075] The film-forming agent was prepared in Preparation Example 1.

[0076] The preparation method of the microcapsule suspension-suspension agent includes the following steps: Step 1: Mix capsule wall material 1 and 0.5 kg of castor oil to obtain modified capsule wall material 1; Step 2: Stir the emulsifier, 1 / 2 dispersant, and 40 kg of water at 2500 rpm at 35°C for 15 minutes to obtain the aqueous phase; Step 3: Stir the prothioconazole and solvent evenly to obtain the oil phase; add the modified capsule wall material 1 to the oil phase and mix, then add the aqueous phase and mix, emulsify at 6000 rpm for 20 minutes to obtain the emulsion; Step 4: Mix the second cell wall material with 5 kg of water to obtain a dilute solution. Add the dilute solution dropwise to the emulsion and stir at 550 rpm for 2 hours to solidify, thus obtaining the primary emulsion. Step 5: Add jinggangmycin, film-forming agent, antifreeze, 1 / 2 dispersant, and preservative to the colostrum and mix. Then add thickener and the remaining water and mix at 500 rpm for 40 minutes to obtain a microcapsule suspension containing jinggangmycin and prothioconazole.

[0077] Example 7:

[0078] A microcapsule suspension-suspension agent containing jinggangmycin and prothioconazole comprises the following raw materials: 2 kg of jinggangmycin, 8 kg of prothioconazole, 2 kg of capsule wall material, 1 kg of emulsifier, 3 kg of dispersant, 10 kg of solvent, 0.1 kg of thickener, 1 kg of film-forming agent, 2 kg of antifreeze, 0.1 kg of preservative, and 50 kg of water.

[0079] The capsule wall material includes 1 kg of capsule wall material one and 1 kg of capsule wall material two.

[0080] The capsule wall material is diphenylmethane diisocyanate; The second capsule wall material is ethylenediamine; The emulsifier is composed of calcium dodecylbenzenesulfonate and phenylethylphenol polyoxyethylene ether in a mass ratio of 1:0.5.

[0081] The dispersant is sodium lignosulfonate.

[0082] The solvent is S-200# solvent oil; The thickener is xanthan gum; The antifreeze is a mixture of propylene glycol and glycerin; the mass ratio of propylene glycol to glycerin is 1:1.5.

[0083] The preservative is benzoic acid.

[0084] The film-forming agent was prepared in Preparation Example 2.

[0085] The preparation method of the microcapsule suspension-suspension agent includes the following steps: Step 1: Mix capsule wall material 1 and 0.5 kg of castor oil to obtain modified capsule wall material 1; Step 2: Stir the emulsifier, 1 / 2 dispersant, and 30 kg of water at 2500 rpm at 35°C for 15 minutes to obtain the aqueous phase; Step 3: Stir the prothioconazole and solvent evenly to obtain the oil phase; add the modified capsule wall material 1 to the oil phase and mix, then add the aqueous phase and mix, emulsify at 6000 rpm for 20 minutes to obtain the emulsion; Step 4: Mix the second cell wall material with 5 kg of water to obtain a dilute solution. Add the dilute solution dropwise to the emulsion and stir at 550 rpm for 2 hours to solidify, thus obtaining the primary emulsion. Step 5: Add jinggangmycin, film-forming agent, antifreeze, 1 / 2 dispersant, and preservative to the colostrum and mix. Then add thickener and the remaining water and mix at 500 rpm for 40 minutes to obtain a microcapsule suspension containing jinggangmycin and prothioconazole.

[0086] Example 8:

[0087] A microcapsule suspension-suspension agent containing jinggangmycin and prothioconazole comprises the following raw materials: 8 kg of jinggangmycin, 15 kg of prothioconazole, 6 kg of capsule wall material, 5 kg of emulsifier, 6 kg of dispersant, 15 kg of solvent, 0.8 kg of thickener, 5 kg of film-forming agent, 5 kg of antifreeze, 0.5 kg of preservative, and 80 kg of water.

[0088] The capsule wall material includes 3 kg of capsule wall material one and 3 kg of capsule wall material two.

[0089] The capsule wall material is diphenylmethane diisocyanate; The second capsule wall material is ethylenediamine; The emulsifier is composed of calcium dodecylbenzenesulfonate and phenylethylphenol polyoxyethylene ether in a mass ratio of 1:0.5.

[0090] The dispersant is sodium lignosulfonate.

[0091] The solvent is S-200# solvent oil; The thickener is xanthan gum; The antifreeze is a mixture of propylene glycol and glycerin; the mass ratio of propylene glycol to glycerin is 1:1.5.

[0092] The preservative is benzoic acid.

[0093] The film-forming agent was prepared in Preparation Example 3.

[0094] The preparation method of the microcapsule suspension-suspension agent includes the following steps: Step 1: Mix capsule wall material 1 and 0.5 kg of castor oil to obtain modified capsule wall material 1; Step 2: Stir the emulsifier, 1 / 2 dispersant, and 45 kg of water at 2500 rpm at 35°C for 15 minutes to obtain the aqueous phase; Step 3: Stir the prothioconazole and solvent evenly to obtain the oil phase; add the modified capsule wall material 1 to the oil phase and mix, then add the aqueous phase and mix, emulsify at 6000 rpm for 20 minutes to obtain the emulsion; Step 4: Mix the second cell wall material with 5 kg of water to obtain a dilute solution. Add the dilute solution dropwise to the emulsion and stir at 550 rpm for 2 hours to solidify, thus obtaining the primary emulsion. Step 5: Add jinggangmycin, film-forming agent, antifreeze, 1 / 2 dispersant, and preservative to the colostrum and mix. Then add thickener and the remaining water and mix at 500 rpm for 40 minutes to obtain a microcapsule suspension containing jinggangmycin and prothioconazole.

[0095] Example 9:

[0096] The difference from Example 6 is that the amount of film-forming agent added is 1 kg.

[0097] Example 10:

[0098] The difference from Example 6 is that the amount of film-forming agent added is 5 kg.

[0099] Comparative Example 1:

[0100] The difference from Example 1 is that no film-forming agent is added.

[0101] Comparative Example 2:

[0102] The difference from Example 1 is that the amount of film-forming agent added is 0.9 kg.

[0103] Comparative Example 3:

[0104] The difference from Example 1 is that the amount of film-forming agent added is 5.1 kg.

[0105] Comparative Example 4:

[0106] The difference from Example 6 is that no film-forming agent is added.

[0107] Comparative Example 5:

[0108] The difference from Example 6 is that the amount of film-forming agent added is 0.9 kg.

[0109] Comparative Example 6:

[0110] The difference from Example 6 is that the amount of film-forming agent added is 5.1 kg.

[0111] Performance testing:

[0112] 1. Thermal storage stability (1) Thermal storage stability of microencapsulated suspensions The test method was based on GB / T14825-2006 standard. The encapsulation efficiency and suspension rate of the microcapsule suspension are shown in Table 1.

[0113] Table 1 Thermal storage stability of microcapsule suspensions

[0114] As can be seen from Table 1 above, the microcapsule suspension prepared in the embodiments of this application has good thermal storage stability.

[0115] Based on the test results of Example 1 and Comparative Example 1, it can be seen that the test results of Example 1 are better than those of Comparative Example 1. This indicates that the added coating agent tightly coats the surface of the pesticide active ingredient, forming a dense physical barrier that effectively blocks the intrusion of external high temperature and moisture and inhibits the degradation of the active ingredient, thereby further improving the thermal storage stability of the microcapsule suspension.

[0116] Based on the test results of Examples 1, 4, 5, Comparative Examples 2 and 3, it can be seen that the amount of film-forming agent added affects the test results, and the microcapsule suspension exhibits the best thermal storage stability when the amount of film-forming agent added is 1-5 parts by mass.

[0117] (2) Thermal storage stability of microcapsule suspension-suspension agent Determination of suspension rate: The procedure was carried out in accordance with the specific steps in the national standard GB / T 14825-2006 "Determination of Pesticide Suspension Rate".

[0118] Determination of encapsulation efficiency: Take the microcapsule suspension-suspension samples prepared in the examples and comparative examples, disperse them in 100 mL of xylene, shake vigorously for 1 minute to mix, and then centrifuge. Transfer the supernatant to a 50 L volumetric flask, dilute with anhydrous methanol and bring to volume to obtain test solution A. Add sufficient anhydrous methanol to the precipitate at the bottom of the centrifuge tube, and sonicate to fully release and dissolve the pesticide inside the capsules. Then bring to volume with anhydrous methanol to obtain test solution B. Determine the concentration of pesticide technical in the two test solutions using high performance liquid chromatography (HPLC).

[0119] The encapsulation ratio is calculated using the following formula: Encapsulation efficiency (%) = (1 - content of free active ingredients outside the capsule / total amount of active ingredients) × 100%.

[0120] Table 2 Thermal storage stability of microcapsule suspensions-suspension agents

[0121] As can be seen from Table 2 above, the microcapsule suspension-suspension agent prepared in the embodiments of this application has good thermal storage stability.

[0122] Based on the test results of Example 6 and Comparative Example 4, it can be seen that the test results of Example 6 are better than those of Comparative Example 4. This indicates that the added coating agent tightly coats the surface of the pesticide active ingredient, forming a dense physical barrier that effectively blocks the intrusion of external high temperature and moisture, and inhibits the degradation of the active ingredient, thereby further improving the thermal storage stability of the microcapsule suspension.

[0123] Based on the test results of Examples 6, 9, 10, Comparative Example 5, and Comparative Example 6, it can be seen that the amount of film-forming agent added affects the test results, and the microcapsule suspension-suspension agent exhibits the best thermal storage stability when the amount of film-forming agent added is 1-5 parts by mass.

[0124] 2. Field efficacy verification (1) Experimental crops and target pests The experimental crop was wheat, and the target disease to be controlled was wheat scab (Fusarium graminearum).

[0125] (2) Overview of the experimental area and cultivation management The experiment was conducted on standard farmland with flat terrain, medium loam soil, moderate soil fertility, and a measured soil pH of 7.1. Throughout the entire growth period of the experimental crop (including fertilization, irrigation, and weed control), the conventional agronomical practices for high-yield wheat cultivation in the local area were strictly followed to ensure environmental consistency.

[0126] (3) Test reagents and experimental design Treatment setup: The test reagents were the samples prepared in the examples and comparative examples; a water treatment group was set up as a blank control (CK).

[0127] Dosage and plot size: The effective ingredient dosage was 12 g / mu. The experiment was conducted using a randomized block design with four replicates, and each plot was 30 m².

[0128] Application: Use a conventional backpack sprayer for foliar spraying. The application window is at the early flowering stage of wheat, with a second application 7 days later. The water dosage is fixed at 45 kg per acre (equivalent to 650 L / hectare), ensuring that the droplets evenly cover both sides of the leaves during spraying.

[0129] (4) Survey methods and efficacy evaluation The final efficacy assessment will be conducted 14 days after the last application of the pesticide.

[0130] Grading standards: Based on the agricultural industry standard "NY / T 1464.15-2007", a 5-level grading method is adopted (Level 0: whole ear healthy; Level 1: diseased ear area ≤ 1 / 4; Level 3: diseased ear area 1 / 4-1 / 2; Level 5: diseased ear area 1 / 2-3 / 4; Level 7: diseased ear area ≥ 3 / 4).

[0131] Sampling method: Each plot is sampled using a five-point diagonal sampling method, with 100-200 ears of grain checked at each point.

[0132] The disease grading standards are as follows: Grade 0: Disease-free entire ear of grain; Grade 1: The area of ​​dead ears accounts for less than 1 / 4 of the total ear area; Grade 3: The area of ​​withered ears accounts for 1 / 4 to 1 / 2 of the total ear area; Grade 5: The area of ​​withered ears accounts for 1 / 2-3 / 4 of the total ear area; Grade 7: The area of ​​dead ears accounts for more than 3 / 4 of the total ear area.

[0133] Calculation formula: Disease index = [Σ(number of diseased ears at each level × relative level value) / (total number of ears surveyed × 7)] × 100; Prevention and control effect (%) = (disease index in blank control area - disease index in drug-treated area) / disease index in blank control area × 100; (5) Prevention and control effects: (5.1) The preventive and therapeutic effects of microcapsule suspensions: Table 3. Results of the prevention and control efficacy test of microcapsule suspension.

[0134] As shown in Table 3, the microcapsule suspension prepared in the embodiments of this application has a good control effect on wheat scab.

[0135] Based on the test results of Example 1 and Comparative Example 1, it can be seen that the test results of Example 1 are better than those of Comparative Example 1. This indicates that with the addition of the film-forming agent, the coating agent coats the surface of the pesticide active ingredient, forming a dense polymer protective layer. This structure can not only significantly reduce the photolysis and volatilization of the active ingredient in the environment, but also extend the duration of the agent's effect by regulating its release rate, thereby greatly improving the control effect of microcapsule suspension on wheat scab.

[0136] Based on the test results of Examples 1, 4, 5, Comparative Example 2, and Comparative Example 3, it can be seen that the amount of film-forming agent added affects the prevention and control effect of microcapsule suspension, and the prevention and control effect of microcapsule suspension is best when the amount of film-forming agent added is 1-5 parts by weight.

[0137] (5.2) The preventive and therapeutic effects of microcapsule suspensions: Table 4. Results of the test on the prevention and control effects of microcapsule suspensions / suspensions

[0138] As shown in Table 4, the microcapsule suspension prepared in the embodiments of this application has a good control effect on wheat scab.

[0139] Based on the test results of Example 6 and Comparative Example 4, it can be seen that the test results of Example 6 are better than those of Comparative Example 4. This indicates that with the addition of the film-forming agent, the coating agent coats the surface of the pesticide active ingredient, forming a dense polymer protective layer. This structure can not only significantly reduce the photolysis and volatilization of the active ingredient in the environment, but also extend the duration of the agent's effect by regulating its release rate, thereby greatly improving the control effect of microcapsule suspension-suspension on wheat scab.

[0140] Based on the test results of Examples 6, 9, 10, Comparative Example 5, and Comparative Example 6, it can be seen that the amount of film-forming agent added affects the control effect, and the control effect of microcapsule suspension is best when the amount of film-forming agent added is 1-5 parts by mass.

[0141] Production increase rate test results The test samples were coated with the standard dosage of 12g of the preparation for 12kg of seeds. The control group was coated with water only. All seeds were thoroughly dried after mixing before sowing.

[0142] The experiment was conducted in leveled fields with a historically uniform incidence of Fusarium head blight, and the soil was neutral (pH 6.0). Five treatments were administered, each replicated three times, with plots randomly arranged and an area of ​​30 m². 2 Sowing density should be in accordance with local standard (120 kg / hm). 2 The implementation of these measures is consistent with that of field production, except for monitoring the control effectiveness and yield composition of stem base rot and Fusarium head blight.

[0143] Yield measurement and analysis were conducted during the harvest stage: 5 sample points were randomly selected from each plot (diagonally distributed), and each point was measured and harvested at a rate of 1 m³. 2 Finally, the yield per hectare is converted and the yield increase rate is calculated.

[0144] Yield increase rate (%) = [(Production in treatment area - Production in control area) / Production in control area] × 100%.

[0145] Results of yield increase test: (1) Results of yield increase test of microcapsule suspension Table 5. Results of yield increase test for microcapsule suspensions

[0146] As shown in Table 3, the microcapsule suspension prepared in the embodiments of this application prevents wheat from being attacked by pathogens during its growth, thereby exhibiting good growth and increasing yield.

[0147] Based on the test results of Example 1 and Comparative Example 1, it can be seen that the test results of Example 1 are better than those of Comparative Example 1, indicating that the added film-forming agent can provide a long-lasting and stable protective layer in the early stage of wheat growth, and realize the slow release of internal active ingredients.

[0148] (2) Results of yield increase test of microcapsule suspension-suspension agent Table 6 Results of Yield Increase Detection

[0149] As shown in Table 6, the microcapsule suspension prepared in the embodiments of this application prevents wheat from being attacked by pathogens during its growth, thus exhibiting good growth and increasing yield.

[0150] Based on the test results of Example 6 and Comparative Example 4, it can be seen that the test results of Example 6 are better than those of Comparative Example 4, indicating that the added film-forming agent can provide a long-lasting and stable protective layer in the early stage of wheat growth, and realize the slow release of internal active ingredients.

Claims

1. A pesticide composition, characterized in that: The raw materials include the following parts by weight: 2-8 parts of jinggangmycin, 8-15 parts of prothioconazole, 2-6 parts of capsule wall material, 1-5 parts of emulsifier, 3-6 parts of dispersant, 1-15 parts of solvent, 0.1-0.8 parts of thickener, 1-5 parts of film-forming agent, 2-5 parts of antifreeze, 0.1-0.5 parts of preservative, and 50-80 parts of water.

2. The pesticide composition according to claim 1, characterized in that: The film-forming agent comprises the following raw materials in parts by weight: 2-8 parts carboxymethyl cellulose, 1-5 parts glycerol (first part), 0.5-1.5 parts expanded perlite, 0.1-0.5 parts gallnut tannin, 3-7 parts corn starch, 8-12 parts glycerol (second part), 30-50 parts chitosan, 0.3-0.7 parts titanium dioxide, and 1-2 parts silane coupling agent.

3. The pesticide composition according to claim 2, characterized in that: The preparation method of the film-forming agent includes the following steps: Carboxymethyl cellulose and the first portion of glycerol were mixed, and then expanded perlite and gallnut tannin were added and mixed to obtain the first mixture; After gelatinizing the corn starch, add the second part of glycerol and mix. Then add chitosan and titanium dioxide and mix to obtain the second mixture. The first mixture, the second mixture, and the silane coupling agent are mixed to obtain a film-forming agent.

4. The pesticide composition according to claim 1, characterized in that: The emulsifier is at least one of castor oil polyoxyethylene ether, polyoxyethylene dehydrated sorbitan monooleate, polyoxyethylene dehydrated sorbitan monostearate, sodium alkylphenol ether sulfosuccinate, calcium dodecylbenzene sulfonate, phenethylphenol polyoxyethylene ether, and tea polyphenols. The dispersant is at least one of sodium lignosulfonate, calcium lignosulfonate, sodium methylnaphthalenesulfonate formaldehyde condensate, dispersant powder, polycarboxylate, alkylnaphthalenesulfonate, and sodium methylenebismethylnaphthalenesulfonate polymer; The solvent is at least one of S-200# solvent oil, S-100# solvent oil, toluene, and xylene; The thickener is at least one of xanthan gum, polyvinyl alcohol, magnesium aluminum silicate, gum arabic, sodium alginate, fatty alcohol polyoxyethylene ether, polyacrylamide, and bentonite. The antifreeze is at least one of ethylene glycol, propylene glycol, and glycerin. The preservative is at least one of potassium sorbate, benzoic acid, methylparaben, 1,2-benzisothiazolin-3-one, methylisothiazolinone, and Kathon.

5. The use of an agricultural fungicide containing the pesticide composition according to any one of claims 1-4 in the control of wheat scab.

6. The application according to claim 5, characterized in that: The agricultural fungicide is a microcapsule suspension or a microcapsule suspension-suspension agent.

7. The application according to claim 6, characterized in that: When the agricultural fungicide is a microcapsule suspension, the preparation method steps are as follows: (1) Weigh each ingredient according to the formula; (2) Add prothioconazole, capsule wall material, and emulsifier to a solvent and mix to obtain an oil phase; (3) Mix the dispersant and water to obtain an aqueous phase; (4) The oil phase is added to the aqueous phase for shear emulsification to obtain the emulsion; (5) Add jinggangmycin, film-forming agent, antifreeze and preservative to the emulsion and mix, then add thickener and mix to obtain microcapsule suspension containing jinggangmycin and prothioconazole.

8. The application according to claim 6, characterized in that: When the agricultural fungicide is a microcapsule suspension, the capsule wall material includes capsule wall material one and capsule wall material two.

9. The application according to claim 8, characterized in that: The preparation method of the microcapsule suspension-suspension agent includes the following steps: (a) Weigh each ingredient according to the formula; (b) Mix capsule wall material one and castor oil in 0.1-1 parts by weight to obtain modified capsule wall material one; (c) Mix the emulsifier, 1 / 2 dispersant, and water to obtain an aqueous phase; (d) Mix prothioconazole and solvent to obtain an oil phase. Add modified capsule wall material I and aqueous phase to the oil phase, mix and emulsify, then add capsule wall material II and stir to solidify to obtain a primary emulsion. (e) Add jinggangmycin, film-forming agent, antifreeze, 1 / 2 dispersant and preservative to the colostrum and mix, then add thickener and mix to obtain microcapsule suspension-suspension containing jinggangmycin and prothioconazole.

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