A suspension containing flubendiamide and bifenazate, and its preparation method and application

Abstract

The present application relates to the field of pesticide technology, and more particularly to a suspension containing flubenzquinoxaline and bifenazate and its preparation method and application. The suspension is made up of the following components by mass percentage: flubenzquinoxaline 10%, bifenazate 10-20%, organic thickener 1.2-1.5%, dispersant 0.6-0.9%, preservative 0.5-0.7%, stabilizer 2-4%, antifreeze 1-1.5%, defoamer 0.5-0.7%, composite synergist 3-3.5%, deionized water is supplemented to 100%. The suspension containing flubenzquinoxaline and bifenazate prepared by the present application has excellent prevention and control effect, good dispersibility and high suspension rate. The suspension shows excellent spreading, permeability and adhesion ability on the surface of the plant body, and is resistant to rain scouring; It can be slowly and effectively distributed twice under humid conditions, so that the drug effect is significant and lasting.

Description

Technical Field

[0001] The present application relates to the technical field of pesticides, and in particular to a suspension containing flubendiamide and bifenazate, and a preparation method and application thereof. Background Art

[0002] Red spider mites are also known as cotton spider mites, commonly known as big spiders, big dragons, sand dragons, etc. Their scientific name is spider mites. The species in my country are mainly cinnabarinus spider mites, belonging to the Arachnida, Acarina, and Tetranychidae. They are widely distributed and have a mixed diet. They can harm more than 110 species of plants, including apples, hawthorns, pears, peaches, cherry blossoms, and elms. Red spider mites often feed on the buds and juice in the leaves of crops. The leaves affected by insects show white-gray spots, which then gradually expand to the entire leaf. In severe cases, the leaves of the entire tree will fall off, causing a significant reduction in fruit yields. At present, red spider mites in apple trees occur very frequently, and the use of pesticides has problems such as old pesticides and large dosages, making the prevention and control of red spider mites in apple trees increasingly difficult.

[0003] Bifenazate, chemical name 3-(4-methoxybiphenyl-3-yl) isopropyl hydrazine, belongs to the bifenazate class of acaricides. Bifenazate is a new type of selective foliar spray acaricide. Its mechanism of action is a unique effect on the aminobutyric acid (GABA) receptors of the central nervous conduction system of mites. It is effective against all life stages of mites, has egg-killing activity and knockdown activity against adult mites (48-72h), and the duration of effect can reach 14d. It is safe for crops within the recommended dosage range. It has low risk for parasitic wasps, predatory mites, and lacewings. However, bifenazate has high use costs and the risk of gradually increasing resistance during use, and its duration of effect is short. Reasonable mixing with other ingredients plays an important role in extending the service life of bifenazate and reducing pesticide residues.

[0004] Flufenac is an efficient and environmentally friendly insecticide with many advantages. It can be widely used in agriculture, forestry, gardening and other fields to control a variety of pests, such as aphids, whiteflies, planthoppers, spider mites, etc. At the same time, flufenac can also be used to control household pests, such as ants, cockroaches, fleas, etc. Flufenac can be used in a variety of ways, including spraying, painting, irrigation, etc., with flexibility and adaptability.

[0005] Chinese patent CN104522010A provides a synergistic acaricidal composition containing cypermethrin and bifenazate, the weight ratio of cypermethrin and bifenazate is 20:1-1:20, and the weight percentage of the total weight of cypermethrin and bifenazate in the acaricidal composition is 5%-85%. The two active ingredients of the invention have obvious synergistic effects, and have excellent control effects on various mite pests on crops such as fruit trees, vegetables, cotton, tea trees, and flowers; the invention improves the control effect; reduces the amount of pesticide used, thereby reducing costs and reducing environmental pollution, which is beneficial to the resistance control of harmful mites, and its promotion and application have great economic and social benefits. In the process of making the active ingredients in the patent into a suspension, the raw material components are added in sequence and mixed with the water dispersion system. In order to improve the performance of the pesticide suspension, it is usually necessary to add a thickener to increase the viscosity of the suspension. After the viscosity of the system increases, the sedimentation rate of the pesticide particles can be reduced, thereby maintaining good suspension stability. The thickener has a large viscosity. During the process of adding the thickener, it is difficult to disperse it in a short time by simple physical stirring. Some thickeners aggregate to form a continuous phase, resulting in the viscosity distribution of the water dispersion system being non-uniform and stable, which is not conducive to maintaining the suspension stability of the pyraclostrobin-bifenazate pesticide suspension concentrate and the effective use of the pesticide. Summary of the invention

[0006] The purpose of the present application is to provide a suspension containing quinacridone and bifenazate, and a preparation method and application thereof, in view of the deficiencies of the current technology. In the suspension containing quinacridone and bifenazate prepared in the present application, quinacridone and bifenazate are used in combination, and the component content is optimized to make the component structure more reasonable, and the suspension has excellent control effect on red spider diseases. The prepared suspension containing quinacridone and bifenazate has good dispersibility and high suspension rate, excellent spreading, penetration and adhesion on the surface of plants, and is resistant to rain erosion; under humid conditions, it can also slowly and effectively carry out secondary distribution, and the efficacy is significant and lasting.

[0007] In the first aspect, the present application provides a suspension containing flubendiamide and bifenazate, using the following technical solution:

[0008] A suspension containing flufenac and bifenazate is prepared from the following components by mass percentage: 10% flufenac, 10-20% bifenazate, 1.2-1.5% organic thickener, 0.6-0.9% dispersant, 0.5-0.7% preservative, 2-4% stabilizer, 1-1.5% antifreeze, 0.5-0.7% defoamer, 3-3.5% composite synergist, and deionized water supplemented to 100%, wherein the composite synergist is prepared by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant.

[0009] By adopting the above technical scheme, flubendiquinoxaline and bifenazate: as active ingredients, have insecticidal effects and have excellent control effects on pests such as red spider mites. The combination of the two has obvious synergistic effects, which can effectively improve the control effect, reduce the amount of active ingredients, and thus reduce costs. Organic thickener: a polyurethane film is formed on the surface, and the hydrophilic polyether chains in the polyurethane film are used to attract water molecules to penetrate the membrane layer and enter the internal structure. The entry of water molecules causes the structure of the membrane layer to change and the internal volume to increase; under the interaction of the two, the polyurethane film swells and ruptures in the water, so that the thickening components are released and dissolved in the water. The thickening components form a three-dimensional network structure in the water dispersion system, increase the viscosity of the mixed system, and optimize the anti-sedimentation performance of the original drug in the suspension containing flubendiquinoxaline and bifenazate. The efficacy of flubendiquinoxaline and bifenazate is fully utilized to improve the control effect on red spider mites. Dispersant: helps to evenly disperse the active ingredients in the suspension, improve the suspension rate, and ensure the stability and durability of the efficacy. Preservatives: Prevent the suspension from spoiling during storage and extend the service life of the product. Stabilizer: Epicatechin has multiple hydroxyl groups that interact with flufenac and bifenazate, and its own macromolecular structure provides steric hindrance, thereby improving the stability of the suspension containing flufenac and bifenazate. Antifreeze: Maintain the stability of the suspension under low temperature conditions to prevent stratification or crystallization caused by temperature changes. Defoamer: Eliminate bubbles in the suspension and improve the appearance quality of the product. Composite synergist: Made by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant. Improve the permeability, wettability and surface tension of the suspension, and significantly enhance the efficacy of the suspension, thereby improving the efficiency of pesticide use, reducing the amount of pesticide used, and reducing the cost of farmers' medicine use, while benefiting the environment and food safety and environmental protection. In summary, the components in the present application cooperate with each other and play a synergistic role together, so that the suspension containing flubendiamide and bifenazate has excellent control effect, is simple to prepare, easy to use, environmentally friendly, and meets the safety requirements of pesticide suspensions.

[0010] Preferably, the mass ratio of the cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant is 5:4:8.

[0011] By adopting the above technical scheme, cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine: This is a non-ionic surfactant with good emulsification, dispersing and wetting properties. In the present application, it helps to improve the dispersibility and stability of the suspension, so that the active ingredients can be evenly distributed in the suspension, thereby improving the efficacy. Naphthalenesulfonate formaldehyde condensate: This is an anionic surfactant with strong wetting and penetration abilities. It interacts with flubendiamide and bifenazate to improve the permeability and wettability of the suspension, making it easier for the agent to enter the plant body, thereby improving the prevention and control effect. Modified polysiloxane surfactant: It can reduce the surface tension of the suspension, improve the spreading and penetration properties of the agent on the plant surface, make the agent easier to adhere to the plant surface, thereby improving the efficacy. The synergistic effect between these three surfactants is mainly reflected in the following aspects: Improving the dispersibility and stability of the suspension: Cocoamidopropyl-ethylhydroxy-3-sulfopropyl betaine, as a non-ionic surfactant, works together with the anionic surfactant naphthalenesulfonate formaldehyde condensate to improve the dispersibility and stability of the suspension, so that the active ingredients can be evenly distributed in the suspension. Improving the permeability and wettability of the suspension: Naphthalenesulfonate formaldehyde condensate works together with modified polysiloxane surfactants to reduce the surface tension of the suspension, improve the spreading and penetration performance of the agent on the plant surface, and make the agent easier to adhere to the plant surface. Improving the efficacy: Through the synergistic effect of the three surfactants, the active ingredients in the suspension can better exert their efficacy and improve the control effect on pests such as red spider mites. In conclusion, the synergistic effect between cocamidopropyl-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant can significantly improve the dispersibility, stability, permeability and wettability of the suspension concentrate, thereby improving the efficacy, reducing the amount of pesticide used, and alleviating the cost of pesticides for farmers, while also being beneficial to the environment and food safety.

[0012] Preferably, the preparation method of the modified polysiloxane surfactant is as follows: under nitrogen protection, 8 mmol methyl stearate, 4 mmol 1,1,1,3,5,5,5-heptamethyltrisiloxane, 0.15 mmol catalyst nano Au / TiO2 and 7 mL toluene are added to a reactor equipped with a stirrer, the mixture is stirred evenly, the temperature is raised to 132°C, the reaction is carried out for 16 hours, and the modified polysiloxane surfactant is obtained by distillation under reduced pressure, wherein the mass content of Au in the catalyst nano Au / TiO2 is 3.5%.

[0013] By adopting the above technical scheme, the preparation method of the modified polysiloxane surfactant comprises the following steps: under nitrogen protection, 8mmol methyl stearate, 4mmol 1,1,1,3,5,5,5-heptamethyltrisiloxane, 0.15mmol catalyst nano Au / TiO2 and 7mL toluene are added to a reactor equipped with a stirrer. These raw materials are mixed in the reactor. After the mixture is stirred evenly, the temperature is raised to 132°C and reacted at this temperature for 16 hours. This step is critical because it allows chemical reactions between the raw materials to form the desired modified polysiloxane surfactant. After the reaction is completed, the unreacted raw materials and by-products are removed by vacuum distillation to obtain a pure modified polysiloxane surfactant. Nano Au / TiO2 is an efficient catalyst, in which the mass content of Au is 3.5%. This catalyst can accelerate the reaction between methyl stearate and 1,1,1,3,5,5,5-heptamethyltrisiloxane, and improve the selectivity and yield of the reaction. The modified polysiloxane surfactant prepared by this method can significantly improve the permeability, wettability and surface tension of the suspension, thereby improving the efficiency of pesticide use, reducing the amount of pesticide used, and reducing the cost of pesticide use for farmers, while also being beneficial to the environment and food safety. This surfactant can also significantly improve the control effect of suspension containing flubendiamide and bifenazate on red spider mites.

[0014] Preferably, the method for preparing the organic thickener comprises the following steps:

[0015] S41, dissolving 3 parts of N-isopropylacrylamide and 12 parts of acrylamide in 10 parts of water according to their weight, and adjusting the pH to 8.5 to obtain a polymerization monomer solution for later use; mixing 4 parts of sorbitan oleate and 11 parts of petroleum ether to obtain a dispersion for later use;

[0016] S42, mixing the polymerization monomer solution and the dispersion liquid and subjecting them to homogenization treatment, the homogenization speed is 3500 rpm, the treatment time is 20 min, to obtain a polymerization reaction liquid; adding 0.002 parts of ammonium persulfate and conducting a polymerization reaction under anaerobic conditions, the reaction temperature of the polymerization reaction is 56° C., the reaction time is 3 h, to obtain a polymer emulsion, which is reserved;

[0017] S43. Dissolve 0.8 parts of 4,4'-dicyclohexylmethane diisocyanate and 3.5 parts of polyethylene glycol in 4 parts of petroleum ether to obtain a prepolymerization solution; after mixing the prepolymerization solution and the polymer emulsion, add 0.003 parts of stannous isooctanoate and 0.4 parts of diethylene glycol, raise the temperature to 62°C and carry out polymerization reaction under anaerobic conditions for 3.5 hours, filter the reaction product to obtain a filter cake, wash with petroleum ether, and dry to obtain an organic thickener.

[0018] By adopting the above technical scheme, the prepared organic thickener plays a key role in the suspension containing flubendiquinoxaline and bifenazate. The preparation process involves multiple steps, and the organic thickener finally obtained can significantly improve the performance of the suspension. The organic thickener forms a three-dimensional network structure, increases the viscosity of the mixed system, makes the original drug particles evenly distributed in the suspension, effectively prevents sedimentation, and thus improves the stability and suspension rate of the suspension. The network structure formed by the thickening component in the water dispersion system helps to evenly disperse the drug particles, avoid aggregation, and ensure that the suspension has excellent dispersibility during use. By optimizing the physical properties of the suspension, such as viscosity and stability, the organic thickener helps the spreading, penetration and adhesion of the drug on the surface of the plant body, improves the efficacy and prolongs the duration of the effect. The use of the thickener enhances the adhesion of the suspension on the surface of the plant body, and can maintain a good control effect even under humid conditions or when it is washed by rain. Improving the efficiency of pesticide use and reducing the amount of pesticide used not only reduces the cost of farmers' medicine use, but also reduces the impact on the environment, which meets the development requirements of green agriculture. The combination of organic thickeners and two active ingredients not only improves the overall performance of the suspension, but also may enhance the stability and bioavailability of the active ingredients through physical or chemical effects, further improving the control effect. The composite synergist improves the permeability and wettability of the suspension, while the organic thickener provides the necessary viscosity and stability. The two work together to make the suspension cover the plant surface more uniform and the efficacy more lasting. The stabilizer epicatechin, by providing steric hindrance and hydrogen bonding, works with the organic thickener to maintain the stability of the suspension, ensuring that the active ingredients do not decompose or precipitate during long-term storage and use. In summary, the organic thickener not only plays an important role alone, but also works synergistically with other components to jointly improve the overall performance and application effect of the suspension containing flubendiamide and bifenazate, providing an efficient and environmentally friendly solution for agricultural production.

[0019] Preferably, the dispersant is composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1.

[0020] By adopting the above technical scheme, the main function of the dispersant in the suspension is to prevent the aggregation and sedimentation of particles. By adsorbing on the surface of solid particles to form a protective layer, a repulsive force is generated between the particles, thereby maintaining the stability of the suspension. The dispersant can reduce the surface tension of water, thereby improving the dispersibility and uniformity of the suspension. The dispersant can promote the effective ingredients in the suspension to better penetrate into the surface of plant leaves or insect bodies, thereby improving the efficacy. By improving the dispersibility and stability of the suspension, the effective ingredients are more evenly distributed on the surface of the plant or insect body, thereby improving the control effect. Synergistic effect between alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester: Alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester are different in molecular structure, the former has a strong lipophilicity, and the latter has a strong hydrophilicity. This difference allows them to be adsorbed on the surface of different types of particles, respectively, providing more comprehensive coverage and protection. The combination of the two can form a more stable protective layer on the surface of the particles, prevent aggregation and sedimentation between particles, and improve the stability of the suspension. The combination of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester can more effectively reduce the surface tension of water, improve the wettability of the suspension to plant leaves and insect bodies, and make the drug effect easier to play. By improving wettability, the combination of the two dispersants can also promote the effective ingredients in the suspension to better penetrate into the plant leaves or the inside of the insect body, thereby improving the control effect. Due to the synergistic effect of the two dispersants, the effective ingredients of the suspension can be more evenly distributed on the plant surface or the insect body, thereby improving the durability and stability of the drug effect. In summary, the dispersant composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1 significantly improves the performance of the suspension containing flubendiquinoxaline and bifenazate through complementary adsorption, enhanced stability, improved wettability, enhanced permeability and improved drug efficacy, so that it has a better control effect on pests such as red spider mites.

[0021] Preferably, the preservative is potassium sorbate.

[0022] Preferably, the stabilizer is epicatechin, the antifreeze agent is propylene glycol, and the defoaming agent is silicone 1522 from Momentive.

[0023] In a second aspect, the present application provides a method for preparing a suspension containing flubendiamide and bifenazate, using the following technical solution:

[0024] As a general technical concept, the present application also provides a method for preparing the above-mentioned suspension containing flubendiamide and bifenazate, comprising the following steps:

[0025] S81, adding flubendiamide, bifenazate and a dispersant into water according to a formula ratio, mixing evenly, and dispersing flubendiamide and bifenazate technical to micron level by shearing or sand milling to prepare an aqueous solution dispersion system;

[0026] S82, adding an organic thickener, a preservative, a stabilizer, an antifreeze agent, a defoaming agent, and a composite synergist to the aqueous solution dispersion system according to the formula ratio, mixing evenly, and then using a homogenizer to evenly disperse to obtain material A;

[0027] S83. After crushing material A with a colloid mill, grinding it with a sand mill until the particle size D98 is ≤ 0.8 μm, to obtain a suspension containing flubendiamide and bifenazate.

[0028] In a third aspect, the present application provides an application of a suspension containing flubendiamide and bifenazate, using the following technical solution:

[0029] As a general technical concept, the present application also provides the use of the above-mentioned suspension containing flubendiamide and bifenazate for controlling crop pests, wherein the pests are citrus red spider mites or apple red spider mites.

[0030] In summary, the beneficial technical effects of this application are:

[0031] 1. Improve the control effect: By combining flubendiamide and bifenazate and optimizing the component content, the ingredient structure is more reasonable, which has an excellent control effect on red spider disease.

[0032] 2. Good dispersibility and suspension: The prepared suspension has good dispersibility and high suspension rate, excellent spreading, penetration and adhesion on the plant surface, and is resistant to rain erosion; under humid conditions, it can also slowly and effectively carry out secondary distribution, and the efficacy is significant and long-lasting.

[0033] 3. Reduce costs: The composite synergist improves the permeability and wettability of the suspension concentrate, reduces the surface tension, and significantly enhances the efficacy of the suspension concentrate, thereby improving the efficiency of pesticide use, reducing the amount of pesticide used, and reducing farmers' drug costs.

[0034] 4. Environmental protection and safety: It is beneficial to the environment, food safety and environmental protection, and meets the safety requirements of pesticide suspension.

[0035] 5. Synergistic effect: The combination of flubendiamide and bifenazate has obvious synergistic effect, which can effectively improve the control effect, reduce the amount of active ingredients, thereby reducing the cost, and has excellent control effect on red spider mites.

[0036] 6. Increase the killing speed of pests: It can also increase the killing speed of pests, prolong the duration of insecticide, and delay resistance.

[0037] 7. Application of stabilizer: epicatechin is used as a stabilizer. It contains multiple hydroxyl groups that interact with flubendiamide and bifenazate, and its own macromolecular structure provides steric hindrance, thereby improving the stability of the suspension.

[0038] 8. Application of organic thickeners: Organic thickeners are used to form a polyurethane film on the surface, which expands and ruptures in water, releasing the thickening components and dissolving them in water. The thickening components form a three-dimensional network structure in the water dispersion system, increasing the viscosity of the mixed system, optimizing the anti-settling performance of the original drug, and facilitating the full exertion of the drug efficacy, thereby improving the control effect on red spider mites. DETAILED DESCRIPTION

[0039] The embodiments of the present application will be described in detail below in conjunction with the examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present application and should not be considered as limiting the scope of the present application. In the examples, if specific conditions are not specified, they are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0040] In the following Examples and Preparation Examples, 1 part means 10 g.

[0041] Preparation Example 1 Preparation of modified polysiloxane surfactant

[0042] The preparation method of the modified polysiloxane surfactant is as follows: under nitrogen protection, 8 mmol methyl stearate, 4 mmol 1,1,1,3,5,5,5-heptamethyltrisiloxane, 0.15 mmol catalyst nano Au / TiO2 and 7 mL toluene are added into a reactor equipped with a stirrer, the mixture is stirred evenly, the temperature is raised to 132° C., and after reacting for 16 hours, the mixture is distilled under reduced pressure to obtain the modified polysiloxane surfactant, wherein the mass content of Au in the catalyst nano Au / TiO2 is 3.5%.

[0043] Preparation Example 2 Preparation of organic thickener

[0044] The preparation method of the organic thickener comprises the following steps:

[0045] S41, dissolving 3 parts of N-isopropylacrylamide and 12 parts of acrylamide in 10 parts of water according to their weight, and adjusting the pH to 8.5 to obtain a polymerization monomer solution for later use; mixing 4 parts of sorbitan oleate and 11 parts of petroleum ether to obtain a dispersion for later use;

[0046] S42, mixing the polymerization monomer solution and the dispersion liquid and subjecting them to homogenization treatment, the homogenization speed is 3500 rpm, the treatment time is 20 min, to obtain a polymerization reaction liquid; adding 0.002 parts of ammonium persulfate and conducting a polymerization reaction under anaerobic conditions, the reaction temperature of the polymerization reaction is 56° C., the reaction time is 3 h, to obtain a polymer emulsion, which is reserved;

[0047] S43. Dissolve 0.8 parts of 4,4'-dicyclohexylmethane diisocyanate and 3.5 parts of polyethylene glycol in 4 parts of petroleum ether to obtain a prepolymerization solution; after mixing the prepolymerization solution and the polymer emulsion, add 0.003 parts of stannous isooctanoate and 0.4 parts of diethylene glycol, raise the temperature to 62°C and carry out polymerization reaction under anaerobic conditions for 3.5 hours, filter the reaction product to obtain a filter cake, wash with petroleum ether, and dry to obtain an organic thickener. Example 1

[0048] A suspension containing flufenac and bifenazate, which is prepared from the following components in percentage by mass: 10% flufenac, 10% bifenazate, 1.2% organic thickener, 0.6% dispersant, 0.5% potassium sorbate, 2% epicatechin, 1% propylene glycol, 0.5% defoamer, 3% composite synergist, and deionized water supplemented to 100%, wherein the composite synergist is prepared by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant in a mass ratio of 5:4:8, the dispersant is composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1, and the defoamer is organic silicon 1522 produced by Momentive Company;

[0049] The preparation method of the suspension containing flubendiamide and bifenazate comprises the following steps:

[0050] S81, adding flubendiamide, bifenazate and a dispersant into water according to a formula ratio, mixing evenly, and dispersing flubendiamide and bifenazate technical to micron level by shearing or sand milling to prepare an aqueous solution dispersion system;

[0051] S82, adding an organic thickener, potassium sorbate, epicatechin, propylene glycol, a defoamer, and a composite synergist to the aqueous solution dispersion system according to the formula ratio, mixing evenly, and then using a homogenizer to evenly disperse to obtain material A;

[0052] S83. After crushing material A with a colloid mill, grinding it with a sand mill until the particle size D98 of the material is 0.8 μm, to obtain a suspension containing flubendiamide and bifenazate. Example 2

[0053] A suspension containing flufenac and bifenazate, which is prepared from the following components in percentage by mass: 10% flufenac, 20% bifenazate, 1.5% organic thickener, 0.9% dispersant, 0.7% potassium sorbate, 4% epicatechin, 1.5% propylene glycol, 0.7% defoamer, 3.5% composite synergist, and deionized water supplemented to 100%, wherein the composite synergist is prepared by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant in a mass ratio of 5:4:8, the dispersant is composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1, and the defoamer is organic silicon 1522 produced by Momentive Company;

[0054] The preparation method of the suspension containing flubendiamide and bifenazate comprises the following steps:

[0055] S81, adding flubendiamide, bifenazate and a dispersant into water according to a formula ratio, mixing evenly, and dispersing flubendiamide and bifenazate technical to micron level by shearing or sand milling to prepare an aqueous solution dispersion system;

[0056] S82, adding an organic thickener, potassium sorbate, epicatechin, propylene glycol, a defoamer, and a composite synergist to the aqueous solution dispersion system according to the formula ratio, mixing evenly, and then using a homogenizer to evenly disperse to obtain material A;

[0057] S83. After crushing material A with a colloid mill, grinding it with a sand mill until the particle size D98 of the material is 0.5 μm, to obtain a suspension containing flubendiamide and bifenazate. Example 3

[0058] A suspension containing flufenac and bifenazate, which is prepared from the following components in percentage by mass: 10% flufenac, 15% bifenazate, 1.3% organic thickener, 0.8% dispersant, 0.6% potassium sorbate, 3% epicatechin, 1.3% propylene glycol, 0.6% defoamer, 3.3% composite synergist, and deionized water supplemented to 100%, wherein the composite synergist is prepared by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant in a mass ratio of 5:4:8, the dispersant is composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1, and the defoamer is organic silicon 1522 produced by Momentive Company;

[0059] The preparation method of the suspension containing flubendiamide and bifenazate comprises the following steps:

[0060] S81, adding flubendiamide, bifenazate and a dispersant into water according to a formula ratio, mixing evenly, and dispersing flubendiamide and bifenazate technical to micron level by shearing or sand milling to prepare an aqueous solution dispersion system;

[0061] S82, adding an organic thickener, potassium sorbate, epicatechin, propylene glycol, a defoamer, and a composite synergist to the aqueous solution dispersion system according to the formula ratio, mixing evenly, and then using a homogenizer to evenly disperse to obtain material A;

[0062] S83. After crushing material A with a colloid mill, grinding it with a sand mill until the particle size D98 of the material is 0.7 μm, to obtain a suspension containing flubendiamide and bifenazate.

[0063] Comparative Example 1

[0064] The same as Example 3, except that the composite synergist is cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine.

[0065] Comparative Example 2

[0066] The same as Example 3, except that the composite synergist is naphthalenesulfonate formaldehyde condensate.

[0067] Comparative Example 3

[0068] The same as Example 3, except that the composite synergist is a modified polysiloxane surfactant.

[0069] Comparative Example 4

[0070] The same as Example 3, except that the dispersant is alkylphenol polyoxyethylene ether.

[0071] Comparative Example 5

[0072] The same as Example 3, except that the dispersant is fatty acid polyoxyethylene ester.

[0073] Comparative Example 6

[0074] The same as Example 3, except that an equal amount of organic bentonite is used instead of the organic thickener.

[0075] Test Example 1

[0076] The efficacy of the suspension containing flubendiamide and bifenazate on apple red spider mite disease was tested through field trials. The test was conducted in the apple orchard of Huangya Village, Yedian Town, Mengyin County, Shandong Province in June 2024, with an orchard area of ​​0.8hm 2The apple variety is Red General, the tree age is 13 years, and the tree spacing is 4m×5m. The fertility of the test field is consistent, and the water and fertilizer management is medium. According to the number of embodiments, the test set up 9 areas and 1 clear water blank control area, with 2 trees in each area, and repeated 4 times. Each embodiment and comparative example corresponds to 9 areas. On June 5, the apple red spider eggs were initially hatched and applied once at a normal rate. The average temperature on the day of application was 29.3°C, there was no rainfall, and there was a light breeze. The spraying equipment was a backpack electric sprayer with a working pressure of 0.2-0.6MPa and a capacity of 20L. The agent was prepared by the secondary dilution method, and the suspension containing flubendiamide and bifenazate was diluted with water, and the dilution multiple was 4000 times.

[0077] 10 and 21 days after the application, the number of active ends on 10 leaves of each tree in each plot was investigated in the east, west, south, north and center. The leaves were checked with a handheld magnifying glass, the number of active ends was recorded, and the control effect was calculated. SPSS20.0 was used for analysis;

[0078]

[0079] In the formula, a0 is the number of the front end of the drug in the blank control area; a is the number of the back end of the drug in the blank control area; b0 is the number of the front end of the drug in the drug treatment area; b is the number of the back end of the drug in the drug treatment area. The test results are shown in Table 1.

[0080] Table 1 Field test results of the efficacy of apple red spider mites

[0081]

[0082] Note: a, b, c in the same column in Table 1 all indicate significant differences at the p<0.05 level.

[0083] Test Example 2

[0084] The suspension rate test of the suspension concentrate containing flubendiamide and bifenazate was carried out according to the specific steps in the national standard GB / T 14825-2006 "Method for Determining the Suspension Rate of Pesticides". The test method is method 2, the test temperature is 30°C, and the concentration of the active ingredient in the sample is consistent with the concentration after dilution in test example 1. The data processing of the test results complies with the provisions of the above national standards, and the suspension rate of the active ingredient ω1 (%) is calculated by the following formula:

[0085]

[0086] Where: 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 left at the bottom of the measuring cylinder, in grams (g);

[0087] The suspension concentrates containing flufenac and bifenazate prepared in each example and each comparative example were stored in a constant temperature oven at 54±2°C for 14 days, and then placed at room temperature for 14 days before the suspension rate test was performed. The test results are shown in Table 2.

[0088] Table 2 Suspension rate test results

[0089]

[0090] Analyzing the data in Table 1 and Table 2, we can see that:

[0091] 1) In the suspension concentrate containing quinacridone and bifenazate prepared in Example 1 to Example 3, quinacridone and bifenazate are used in combination, and the component content is optimized to make the component structure more reasonable, which has an excellent control effect on red spider mite diseases. The prepared suspension concentrate containing quinacridone and bifenazate has good dispersibility and high suspension rate, and has excellent spreading, penetration and adhesion ability on the surface of the plant body, and is resistant to rain erosion; under humid conditions, it can also slowly and effectively carry out secondary distribution, and the drug effect is significant and lasting.

[0092] 2) The performance comparison analysis of the suspension containing flubendiamide and bifenazate prepared in combination with Example 3 and Comparative Examples 1-3 shows that the composite synergist is prepared by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant in a mass ratio of 5:4:8, and the synergistic effect between them is utilized to improve the dispersibility and stability of the suspension: cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine as a nonionic surfactant, and anionic surfactant naphthalenesulfonate formaldehyde condensate, can improve the dispersibility and stability of the suspension, so that the effective ingredients can be evenly distributed in the suspension. Improve the permeability and wettability of the suspension: naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant work together to reduce the surface tension of the suspension, improve the spreading and penetration performance of the agent on the plant surface, and make the agent easier to adhere to the plant surface. Improve the efficacy of the drug: Through the synergistic effect of the three surfactants, the active ingredients in the suspension can better exert their efficacy and improve the control effect on pests such as red spider mites. In short, the synergistic effect between cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant can significantly improve the dispersibility, stability, permeability and wettability of the suspension, thereby improving the efficacy of the drug, reducing the amount of pesticides used, and reducing the cost of pesticides for farmers, while benefiting the environment and food safety and environmental protection.

[0093] 3) The performance comparison analysis of the suspension containing quinacridone and bifenazate prepared in combination with Example 3 and Comparative Examples 4-5 shows that the dispersant is composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1. The synergistic effect between them is utilized, and the synergistic effect of complementary adsorption, enhanced stability, improved wettability, enhanced permeability and improved efficacy is achieved. The performance of the suspension containing quinacridone and bifenazate is significantly improved, so that it has better control effect and stability against pests such as red spider mites.

[0094] 4) The performance comparison analysis of the suspension containing fluoroquinolones and bifenazate prepared in combination with Example 3 and Comparative Example 6 shows that the organic thickener prepared in the present application plays a key role in the suspension containing fluoroquinolones and bifenazate. The organic thickener increases the viscosity of the mixed system by forming a three-dimensional network structure, so that the original drug particles are evenly distributed in the suspension, effectively preventing sedimentation, thereby improving the stability and suspension rate of the suspension. The network structure formed by the thickening component in the water dispersion system helps the uniform dispersion of the drug particles, avoids aggregation, and ensures that the suspension has excellent dispersibility during use. By optimizing the physical properties of the suspension, such as viscosity and stability, the organic thickener helps the spreading, penetration and adhesion of the drug on the surface of the plant body, improves the drug effect and prolongs the lasting period. The use of the thickener enhances the adhesion of the suspension on the surface of the plant body, even under humid conditions or when it is washed by rain, it can also maintain a good prevention and control effect. Improving the efficiency of pesticide use and reducing the amount of pesticide used not only reduces farmers' pesticide costs, but also reduces the impact on the environment, which is in line with the development requirements of green agriculture.

[0095] The above embodiments are only used to explain the technical solutions of the present application rather than to limit them. Although the above embodiments provide a specific description of the present application, relevant technical personnel should understand that the specific implementation modes of the present invention can still be modified or replaced by equivalents, and any modifications and equivalent replacements that do not depart from the spirit and scope of the present application should be included in the scope of protection of the present application.

Claims

1. A suspension containing flubendiamide and bifenazate, characterized in that: The invention is prepared from the following components by mass percentage: 10% of flubendiamide, 10-20% of bifenazate, 1.2-1.5% of organic thickener, 0.6-0.9% of dispersant, 0.5-0.7% of preservative, 2-4% of stabilizer, 1-1.5% of antifreeze agent, 0.5-0.7% of defoamer, 3-3.5% of composite synergist, and deionized water is added to 100%, wherein the composite synergist is prepared by mixing cocamidopropyl-ethylhydroxy-3-sulfopropyl betaine, naphthalenesulfonate formaldehyde condensate and modified polysiloxane surfactant in a mass ratio of 5:4:8; The preparation method of the organic thickener comprises the following steps: S41. Dissolve 3 parts of N-isopropylacrylamide and 12 parts of acrylamide in 10 parts of water according to their mass fractions, and adjust the pH to 8.5 to obtain a polymerization monomer solution for later use; mix 4 parts of sorbitan oleate and 11 parts of petroleum ether to obtain a dispersion for later use; S42, mixing the polymerization monomer solution and the dispersion liquid and subjecting them to homogenization treatment, the homogenization speed is 3500 rpm, the treatment time is 20 min, to obtain a polymerization reaction liquid; adding 0.002 parts of ammonium persulfate and conducting a polymerization reaction under anaerobic conditions, the reaction temperature of the polymerization reaction is 56° C., the reaction time is 3 h, to obtain a polymer emulsion, which is reserved; S43, dissolving 0.8 parts of 4,4'-dicyclohexylmethane diisocyanate and 3.5 parts of polyethylene glycol in 4 parts of petroleum ether to obtain a prepolymerization solution; after mixing the prepolymerization solution and the polymer emulsion, adding 0.003 parts of stannous isooctanoate and 0.4 parts of diethylene glycol, raising the temperature to 62°C and performing a polymerization reaction under anaerobic conditions for 3.5 hours, filtering the reaction product to obtain a filter cake, washing with petroleum ether, and drying to obtain an organic thickener; The preparation method of the modified polysiloxane surfactant is as follows: under nitrogen protection, 8 mmol of methyl stearate, 4 mmol of 1,1,1,3,5,5,5-heptamethyltrisiloxane, 0.15 mmol of catalyst nano Au / TiO2 and 7 mL of toluene are added into a reactor equipped with a stirrer, and the mixture is stirred evenly, and then heated to 132° C., reacted for 16 hours, and then distilled under reduced pressure to obtain the modified polysiloxane surfactant, wherein the mass content of Au in the catalyst nano Au / TiO2 is 3.5%; The dispersant is composed of alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester in a mass ratio of 1:1; The preservative is potassium sorbate; The stabilizer is epicatechin, the antifreeze agent is propylene glycol, and the defoaming agent is silicone 1522; The preparation method of the suspension containing flubendiamide and bifenazate comprises the following steps: S81, adding flubendiamide, bifenazate and a dispersant into water according to a formula ratio, mixing evenly, and dispersing flubendiamide and bifenazate technical to micron level by shearing or sand milling to prepare an aqueous solution dispersion system; S82, adding an organic thickener, a preservative, a stabilizer, an antifreeze agent, a defoaming agent, and a composite synergist to the aqueous solution dispersion system according to the formula ratio, mixing evenly, and then using a homogenizer to evenly disperse to obtain material A; S83, crush material A with a colloid mill, and then grind it with a sand mill to a particle size of D 98 ≤0.8μm, a suspension containing flubendiamide and bifenazate was obtained; The suspension containing flubendiamide and bifenazate is used for preventing and controlling crop pests, and the pests are citrus red spider mites or apple red spider mites.

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