Hexaflutole-containing composition as well as preparation method and application thereof
By preparing compositions containing hexiflozolidamamide and adding composite decentralized agents and composite efficiency increase agents, the problem of low suspension rate of existing pesticide suspension agents and poor dispersion have significantly improved the utilization and prevention effect of pesticides, reducing The cost of medication.
Patent Information
- Application Number
- CN202411908484.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-24
- Publication Date
- 2025-01-24
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing suspension agents of nitrile and hexafluorazamide have low floating rate, poor dispersion and low pesticide adhesion. The suspension rate decreases during long-term storage, which affects product stability and utilization.
By preparing a composition containing hexopromazoamide, active ingredients, surfactants, ethylene glycol, thickening agent, composite efficiency increase agent, composite dispersant, propeller, propylene glycolin acid Mix the specific proportion of esters and water, add composite decentralized agents and composite efficiency agents to increase suspension rates and decentralization.
It significantly improves the suspension rate, decentralization and pesticide attachment rate of pesticide suspension, reduce the evaporation of the surface of the surface of the crop, increase the internal absorption of the pharmaceutical agent, improve the utilization rate and prevention effect of pesticides, and reduce the cost of medication.
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Abstract
Description
Technical Field
[0001] The present application relates to the technical field of pesticides, and in particular to a composition containing hexaflufenamide and a preparation method and application thereof. Background Art
[0002] As people's living standards improve, the requirements for agricultural products are also constantly increasing. The chemical name of chlorfenapyr is 4-bromo-2-(4-chlorophenyl)-1-ethoxymethyl-5-trifluoromethylpyrrole-3-carbonitrile, which is a new type of pyrrole compound. It mainly acts on insect mitochondria, inhibits the conversion of adenosine diphosphate into adenosine triphosphate, reduces the energy required to maintain the body, and thus exerts its efficacy. The chemical name of tolfenpyrad is N-{2-[3-chloro-5-(trifluoromethyl)-2-pyridyl]ethyl}-α,α,α-trifluoro-O-toluamide, with a molecular formula of C16H11ClF6N2O and a relative molecular mass of 396.76. Hexaflutazole is an excellent fungicide, mainly used in agriculture and horticulture to prevent and control a variety of diseases. The mechanism of action of hexaflutamide is mainly to interfere with the function of the ecdysone receptor of pests, affecting their normal growth and development, and at the same time acting on the nervous system of pests, causing abnormal nerve conduction, and ultimately leading to paralysis and death of the pests. This dual mechanism of action makes hexaflutamide have a strong killing power against pests, while having little impact on non-target organisms and the environment. In addition, hexaflutamide also has the characteristics of a wide insecticide spectrum, rapid insecticide, long-lasting effect, low toxicity and rapid degradation. It mainly kills by contact, can kill eggs, inhibit egg laying, and does not have systemic conduction. Insecticides such as cypermethrin and hexaflutamide have the advantages of high efficiency, safety and low toxicity, and have been widely used and developed.
[0003] The current suspension concentrates such as chlorfenapyr and hexaflutazole have low floating rates, poor dispersibility and low pesticide adhesion rates. At the same time, they are prone to turbidity and a decrease in suspension rate during long-term storage, with the suspension rate even decreasing by more than 20%, affecting the storage stability and shelf life of the product. At the same time, there are also problems such as rapid evaporation of the agent on the crop surface and poor adsorption of the agent on the crop surface, resulting in low utilization of the pesticide and poor control effect. Summary of the invention
[0004] The purpose of this application is to provide a composition containing hexafluazole worm amide and its preparation method and application in view of the deficiencies of the current technology. The composition containing hexafluazole worm amide prepared in this application has the advantages of synergistic enhancement, high selectivity, environmental compatibility, reduced environmental pollution, cost saving, etc. in preventing and controlling thrips pests, beet armyworms and diamondback moths. By adding a composite dispersant, the suspension rate, dispersibility and pesticide adhesion rate of the pesticide suspension can be significantly improved; by adding a composite synergist, the evaporation of the liquid on the surface of the crop can be significantly reduced, while the systemic absorption of the agent on the surface of the crop can be increased, the utilization rate of the pesticide can be improved, the control effect of pests and diseases can be improved, and the cost of the drug can be reduced; at the same time, the added surfactant has hydrophilic and lipophilic characteristics, low viscosity, good spreadability, and can make the agent better adhere to the surface of the leaf and penetrate into the internal tissue of the leaf, significantly improving the control effect of pests and diseases.
[0005] In the first aspect, the present application provides a composition containing hexaflufenamide, using the following technical solution: A composition containing fluazifop-butyl, comprising the following raw materials by weight: 15-18 parts of active ingredients, 4-6 parts of surfactants, 2-3 parts of ethylene glycol, 4-5 parts of thickeners, 0.3-0.5 parts of defoamers, 4-5 parts of composite synergists, 2-3 parts of composite dispersants, 0.5-0.8 parts of preservatives, 5-6 parts of propylene glycol methyl ether acetate, and 70-75 parts of water; wherein the active ingredient is prepared by mixing fluazifop-butyl and cypermethrin in a weight ratio of 3:2, and the composite dispersant is prepared by mixing modified acrylate and modified lignin.
[0006] By adopting the above technical scheme, the composition containing hexaflufenamide can effectively control pests such as thrips, beet armyworm and diamondback moth through carefully selected components. Active ingredients (hexaflufenamide and chlorfenapyr): they are mixed in a specific ratio, have a synergistic effect, and can improve the control effect of thrips, beet armyworm and diamondback moth. Surfactant: It has hydrophilic and lipophilic properties, low viscosity, good spreadability, and can make the agent better adhere to the surface of the leaves and penetrate into the inner part of the leaf tissue, significantly improving the control effect of pests and diseases. Ethylene glycol: As an antifreeze agent, it maintains the stability of the composition under low temperature conditions and prevents stratification or crystallization caused by temperature changes. Thickener: Increase the viscosity of the pesticide composition, and the prepared composition containing hexaflufenamide has good suspension stability. At the same time, it can also help the active ingredients of the pesticide to be evenly distributed in the liquid, prevent its precipitation or stratification, and ensure that the pesticide can maintain stable efficacy during use. Defoamer: Eliminate bubbles in the pesticide composition and improve the stability and use effect of the product. Composite synergist: significantly reduce the evaporation of the liquid medicine on the surface of crops, increase the absorption of the medicine on the surface of crops, improve the utilization rate of pesticides, improve the control effect of pests and diseases, and thus reduce the cost of medicine. Composite dispersant (modified acrylate and modified lignin): by adding composite dispersant, the suspension rate, dispersibility and pesticide adhesion rate of pesticide suspension can be significantly improved; modified lignin provides steric hindrance, so as to maintain the stability of suspension, and by modifying lignin with tartaric acid, the compatibility of lignin with other materials can be improved, thereby improving the dispersibility and stability of pesticide suspension. Modified acrylate has good biocompatibility and biodegradability due to the introduction of polyethylene glycol, which is conducive to the formation of stable liposomes in water and increases the viscosity of pesticide composition. Preservative: prevent the pesticide composition from deteriorating during storage and use. Propylene glycol methyl ether acetate: as a harmless solvent, it has extremely strong dissolving ability and has multiple functional groups. It has better compounding effect with other materials, making the overall performance of the product more stable. Through the synergistic effect of the above components, the composition containing hexaflufenamide in the present application has the advantages of synergistic effect, high selectivity, environmental compatibility, reduced environmental pollution, cost savings, etc. in preventing and controlling thrips pests, beet armyworms and diamondback moths.
[0007] Preferably, the mass ratio of the modified acrylate to the modified lignin is 4:3.
[0008] By adopting the above technical scheme, firstly, the modified acrylic acid ester has good biocompatibility and biodegradability due to the introduction of polyethylene glycol, which is conducive to forming stable liposomes in water, increasing the viscosity of the pesticide composition, and the prepared composition containing hexaflufenamide has good suspension stability. At the same time, it can also help the pesticide active ingredients to be evenly distributed in the liquid, prevent them from precipitation or stratification, and ensure that the pesticide can maintain stable efficacy during use. Secondly, the natural reticular macromolecular structure of the modified lignin provides a steric hindrance, thereby maintaining the stability of the suspension. By modifying lignin with tartaric acid, the compatibility of lignin with others can be improved, thereby improving the dispersibility and stability of the pesticide suspension. When the modified acrylic acid ester and the modified lignin are mixed in a ratio of 4:3, the coordination between them can be maximized. On the one hand, the modified acrylic acid ester can improve the viscosity and suspension stability of the pesticide composition, so that the active ingredient particles are more evenly distributed in the suspension; on the other hand, the modified lignin can provide a steric hindrance to prevent the agglomeration phenomenon between particles, so that each component can achieve efficient and stable mixing. This synergistic effect is beneficial to improving the good control effect of the composition containing hexaflufenamide.
[0009] Preferably, the preparation method of the modified acrylate comprises the following steps: S31, according to the mass fraction, take 10 parts of polyethylene glycol, heat it to 130°C, add 1 part of octyl polyoxyethylene ether, stir and react for 45 minutes, the stirring speed is 270r / min, after the addition is completed, continue to keep the temperature at 110°C for 25 minutes to obtain a polyethylene glycol emulsion; S32. According to the mass proportions, take 0.75 parts of octyl polyoxyethylene ether and 1 part of deionized water and mix them evenly. After stirring to dissolve, add 5 parts of methyl acrylate and 0.3 parts of potassium persulfate and stir and emulsify for 40 minutes. Add polyethylene glycol emulsion and heat to 120°C. Continue stirring and reacting for 2 hours. When the reaction temperature is reduced to 90°C, perform vacuum distillation to obtain modified acrylate.
[0010] By adopting the above technical scheme, the modified acrylic ester prepared has good biocompatibility and biodegradability due to the introduction of polyethylene glycol. This makes the pesticide composition have less impact on the environment during use, which is beneficial to environmental protection. The modified acrylic ester can form stable liposomes in water, thereby increasing the viscosity of the pesticide composition. This helps the pesticide active ingredients to be evenly distributed in the liquid, prevents them from precipitating or stratifying, and ensures that the pesticide can maintain a stable efficacy during use. Through the synergistic effect of the modified acrylic ester and the modified lignin, the agglomeration phenomenon between the particles can be effectively reduced, so that the particles of the active ingredients are more evenly distributed in the suspension. This is conducive to improving the good prevention and control effect of the composition containing hexafluthrin. The modified acrylic ester has good suspension stability, which can help the pesticide active ingredients to be evenly distributed in the liquid, prevent them from precipitating or stratifying. This helps to ensure that the pesticide can maintain a stable efficacy during use. The synergistic effect of the modified acrylic ester and the modified lignin can significantly improve the suspension rate, dispersibility and pesticide adhesion rate of the pesticide suspension. In summary, the modified acrylate plays a variety of important roles in the present application, and synergizes with other components to jointly improve the control effect and performance of the composition containing hexaflufenamide.
[0011] Preferably, the preparation method of the modified lignin is as follows: 1 part of tartaric acid, 0.3 part of sodium hypophosphite and 50 parts of deionized water are added to a reactor according to their mass fractions, 12 parts of alkaline lignin are added after stirring evenly, the temperature is raised to 90° C., and after reacting for 6 hours, the modified lignin is filtered, washed and dried to obtain the modified lignin.
[0012] By adopting the above technical solution, the prepared modified lignin has a natural reticular macromolecular structure, which can provide steric hindrance, thereby maintaining the stability of the suspension. By modifying lignin with tartaric acid, the compatibility of lignin with other ingredients can be improved, thereby improving the dispersibility and stability of the pesticide suspension. It works synergistically with modified acrylate to reduce the agglomeration phenomenon between particles, so that the active ingredient particles are more evenly distributed in the suspension, achieving efficient and stable mixing, which is conducive to improving the good control effect of the composition containing hexaflufenamide.
[0013] Preferably, the composite synergist is prepared by mixing trimethylglycine and silicone emulsion in a mass ratio of 2:3.
[0014] By adopting the above technical scheme, trimethylglycine has excellent emulsification, dispersion and wetting properties, can significantly reduce the surface tension of the liquid medicine, so that the liquid medicine forms a stable liquid film on the surface of the crop, and reduces the evaporation loss of the active ingredient. At the same time, trimethylglycine can also enhance the affinity between the liquid medicine and the surface of the crop, improve the adhesion and spreadability of the liquid medicine on the surface of the plant, thereby improving the utilization rate and control effect of the agent. Silicone emulsion has good stability and biocompatibility, and can play a role in thickening, stabilizing and improving suspension in the pesticide composition. Through the synergistic effect with trimethylglycine, the silicone emulsion can further improve the suspension rate and dispersibility of the pesticide composition, so that the active ingredients are more evenly distributed in the suspension, and the efficacy is improved. In addition, the silicone emulsion can also reduce the surface tension of the product, so that the agent can be fully spread on the crop, increase the contact area between the agent and the crop, enhance the residence time of the liquid medicine on the plant surface, reduce the loss of active ingredients, and make the efficacy more significant. In summary, the coordination between trimethylglycine and silicone emulsion is mainly reflected in the following aspects: improving the utilization rate of pesticide compositions and the efficacy of active ingredients per unit of pesticides. The synergistic effect with trimethylglycine can significantly improve the effect of pesticide compositions. It reduces the surface tension of the product, allowing the agent to spread completely on the crop, increases the contact area between the agent and the crop, increases the residence time of the liquid on the plant surface, reduces the loss of active ingredients, and makes the efficacy more significant. It forms a good water-in-oil silicone microemulsion, so that the silicone microemulsion has a good spreading effect in the composition formula containing hexaflufenamic acid, and significantly improves the efficacy.
[0015] Preferably, the preparation method of the silicone emulsion is as follows: 23 parts of hydroxy silicone oil and 18 parts of amino polyether block silicone oil are mixed according to mass parts, stirred for 30 minutes, then 4 parts of XL-40 and 3 parts of XL-70 are added, the temperature is raised to 45°C, and the mixture is fully stirred for 18 minutes. 1 part of acetic acid is added, and after stirring for 20 minutes, water is slowly dripped in while stirring, 40 parts of water are added at a dripping speed of 0.01 parts / 10s, and then 1 part of acetic acid is added, and 0.5 parts of silicone defoamer are added, and the mixture is stirred for 5 minutes to obtain the silicone emulsion.
[0016] By adopting the above technical scheme, the prepared silicone emulsion is prepared by the reaction of hydroxy silicone oil, amino polyether block silicone oil, XL-40 and XL-70. Among them, hydroxy silicone oil and amino polyether block silicone oil are the main active ingredients, and XL-40 and XL-70 are isomeric alcohol ether products used to adjust the stability and spreadability of the emulsion. The main functions of the silicone emulsion are as follows: 1. Improve the utilization rate of the pesticide composition and the efficacy of the unit pesticide active ingredient. Through the synergistic effect with trimethylglycine, the effect of the pesticide composition can be significantly improved. 2. Reduce the surface tension of the product, so that the agent can be fully spread on the crop, increase the contact area between the agent and the crop, enhance the residence time of the liquid on the plant surface, reduce the loss of active ingredients, and make the efficacy more significant. 3. Form a good water-in-oil silicone microemulsion, so that the silicone microemulsion has a good spreadability effect in the composition formula containing hexaflufenamic acid, and significantly improve the efficacy.
[0017] Preferably, the surfactant is composed of lauramide propyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate in a mass ratio of 1:1.
[0018] By adopting the above technical scheme, the surfactant helps to reduce the surface tension of water, so that the pesticide particles can be more evenly dispersed in the water, thereby improving the suspension rate and stability of the suspension. This is crucial to ensure that the pesticide can maintain consistent efficacy during use. Lauramide propyl hydroxysulfonyl betaine has good wetting properties, which enables the agent to better adhere to the surface of plant leaves, while tristyrylphenol polyoxyethylene ether phosphate provides additional wetting properties. The combination of the two can significantly improve the coverage of the agent on the leaf surface and increase the chance of contact between the agent and pests. By adding these two surfactants, the systemicity of the agent on the crop surface can be increased, which means that more agents can be absorbed by the crop and transported to the parts that need protection, thereby improving the control effect. The coordination between lauramide propyl hydroxysulfonyl betaine and tristyrylphenol polyoxyethylene ether phosphate not only improves the physical properties of the agent, but also may enhance the mechanism of action of the agent on pests through chemical interactions, thereby achieving a synergistic effect. In summary, the combination of lauramidopropyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate as a surfactant can enable the agent to better adhere to the leaf surface and penetrate into the leaf tissue, significantly improving the control effect of pests and diseases.
[0019] Preferably, the thickener is gum arabic; the preservative is potassium sorbate; and the defoaming agent is an organosilicon defoaming agent.
[0020] In a second aspect, the present application provides a method for preparing a composition containing hexaflufenamide, using the following technical solution: As a general technical concept, the present application also provides a method for preparing the above-mentioned composition containing hexaflufenamide, comprising the following steps: S91. Mix the active ingredient, surfactant, ethylene glycol, thickener, defoamer, composite synergist, composite dispersant, preservative, propylene glycol methyl ether acetate and water according to their weight fractions, and pre-disperse and shear at a speed of 3000 rpm for 30 min to obtain a mixed solution; S92, subjecting the mixed solution to ultrafine grinding, grinding at a rotation speed of 2500 rpm for 3 hours, detecting the particle size D90 ≤ 0.5 μm, and filtering to obtain a composition containing hexaflufenamide.
[0021] In a third aspect, the present application provides an application of a composition containing hexaflufenamide, using the following technical solution: As a general technical concept, the present application also provides the above-mentioned composition containing hexaflufenamide for use in crops to control thrips pests, beet armyworm and diamondback moth.
[0022] In summary, the beneficial technical effects of this application are: 1. Synergistic effect: By mixing hexaflufenamide and chlorfenapyr in a specific ratio, a synergistic control effect can be achieved on pests such as thrips, beet armyworm and diamondback moth. This synergistic effect can improve the utilization rate of pesticides and reduce the cost of medication.
[0023] 2. High selectivity: The composition of the present application is highly selective and can effectively control specific pests, reduce the impact on other organisms, and reduce environmental pollution.
[0024] 3. Improve the suspension rate, dispersibility and pesticide adhesion rate of pesticide suspension concentrates: By adding composite dispersants (modified acrylates and modified lignin), the suspension rate, dispersibility and pesticide adhesion rate of pesticide suspension concentrates can be significantly improved, thereby improving the utilization rate and control effect of pesticides.
[0025] 4. Reduce the evaporation of pesticide solution and improve the systemic absorption of pesticide on the crop surface: By adding composite enhancers (such as trimethylglycine and silicone emulsion), the evaporation of pesticide solution on the crop surface can be significantly reduced, while the systemic absorption of pesticide on the crop surface can be increased, thereby improving the utilization rate of pesticides and the control effect.
[0026] 5. Enhance the affinity between the liquid medicine and the crop surface: Trimethylglycine can enhance the affinity between the liquid medicine and the wax layer on the crop surface, reduce the contact angle between the liquid medicine and the crop surface, and enable the liquid medicine sprayed on the crop surface to spread quickly, reducing the loss caused by droplets rolling into the water or the field.
[0027] 6. Improve the utilization rate of pesticide compositions and the efficacy of active ingredients per unit of pesticides: Silicone emulsions can improve the utilization rate of pesticide compositions and the efficacy of active ingredients per unit of pesticides, reduce the surface tension of the product, allow the agent to spread completely on the crops, increase the contact area between the agent and the crops, increase the residence time of the agent on the plant surface, and reduce the loss of active ingredients.
[0028] 7. Maintain the stability of the suspension concentrate: The introduction of modified lignin provides steric hindrance, which can maintain the stability of the suspension concentrate. Modification of lignin with tartaric acid can improve the compatibility of lignin with other substances, thereby improving the dispersibility and stability of the pesticide suspension concentrate.
[0029] 8. Good biocompatibility and biodegradability: The modified acrylate has good biocompatibility and biodegradability due to the introduction of polyethylene glycol, which is conducive to the formation of stable liposomes in water and increases the viscosity of the pesticide composition. The prepared composition containing hexaflufenamide has good suspension stability. DETAILED DESCRIPTION
[0030] The embodiments of the present application will be described in detail below in conjunction with the examples, but those skilled in the art will appreciate that the following examples are only used to illustrate the present application and should not be considered to limit the scope of the present application. If the specific conditions are not specified in the examples, they are carried out according to conventional conditions or 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, and XL-40 and XL-70 are isomeric alcohol ether products of BASF.
[0031] In the following examples and preparation examples, 1 part means 100 g.
[0032] Preparation Example 1 Preparation of modified acrylate The preparation method of modified acrylate comprises the following steps: S31, according to the mass fraction, take 10 parts of polyethylene glycol, heat it to 130°C, add 1 part of octyl polyoxyethylene ether, stir and react for 45 minutes, the stirring speed is 270r / min, after the addition is completed, continue to keep the temperature at 110°C for 25 minutes to obtain a polyethylene glycol emulsion; S32. According to the mass proportions, take 0.75 parts of octyl polyoxyethylene ether and 1 part of deionized water and mix them evenly. After stirring to dissolve, add 5 parts of methyl acrylate and 0.3 parts of potassium persulfate and stir and emulsify for 40 minutes. Add polyethylene glycol emulsion and heat to 120°C. Continue stirring and reacting for 2 hours. When the reaction temperature is reduced to 90°C, perform vacuum distillation to obtain modified acrylate.
[0033] Preparation Example 2 Preparation of modified lignin The preparation method of modified lignin is as follows: according to the mass proportions, 1 part of tartaric acid, 0.3 parts of sodium hypophosphite and 50 parts of deionized water are added into a reactor, 12 parts of alkaline lignin are added after stirring evenly, the temperature is raised to 90° C., and after reacting for 6 hours, the modified lignin is filtered, washed and dried to obtain the modified lignin.
[0034] Preparation Example 3 Preparation of silicone emulsion The preparation method of the silicone emulsion is as follows: 23 parts of hydroxy silicone oil and 18 parts of amino polyether block silicone oil are mixed according to the mass parts, and after stirring for 30 minutes, 4 parts of XL-40 and 3 parts of XL-70 are added, the temperature is raised to 45°C, and the mixture is fully stirred for 18 minutes. 1 part of acetic acid is added, and after stirring for 20 minutes, water is slowly dripped in while stirring, 40 parts of water are added at a dripping speed of 0.01 parts / 10s, and then 1 part of acetic acid is added, and 0.5 parts of silicone defoaming agent are added, and the mixture is stirred for 5 minutes to obtain the silicone emulsion. Example 1
[0035] A composition containing fluazifop-butyl, comprising the following raw materials by weight: 15 parts of active ingredient, 4 parts of surfactant, 2 parts of ethylene glycol, 4 parts of gum arabic, 0.3 parts of silicone defoamer, 4 parts of composite synergist, 2 parts of composite dispersant, 0.5 parts of potassium sorbate, 5 parts of propylene glycol methyl ether acetate, and 70 parts of water; wherein the active ingredient is prepared by mixing fluazifop-butyl and chlorfenapyr in a weight ratio of 3:2, the composite dispersant is prepared by mixing modified acrylate and modified lignin in a weight ratio of 4:3; the composite synergist is prepared by mixing trimethylglycine and silicone emulsion in a weight ratio of 2:3, and the surfactant is composed of lauramide propyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate in a weight ratio of 1:1; The preparation method of the above-mentioned composition containing hexaflufenamide comprises the following steps: S91. Mix the active ingredient, surfactant, ethylene glycol, gum arabic, silicone defoamer, composite synergist, composite dispersant, potassium sorbate, propylene glycol methyl ether acetate and water according to their weight fractions, and pre-disperse and shear at a speed of 3000 rpm for 30 min to obtain a mixed solution; S92, subjecting the mixed solution to ultrafine grinding, grinding at a rotation speed of 2500 rpm for 3 hours, detecting the particle size D90 ≤ 0.5 μm, and filtering to obtain a composition containing hexaflufenamide. Example 2
[0036] A composition containing fluazifop-butyl, comprising the following raw materials by weight: 18 parts of active ingredients, 6 parts of surfactants, 3 parts of ethylene glycol, 5 parts of gum arabic, 0.5 parts of silicone defoamers, 5 parts of composite synergists, 3 parts of composite dispersants, 0.8 parts of potassium sorbate, 6 parts of propylene glycol methyl ether acetate, and 75 parts of water; wherein the active ingredient is prepared by mixing fluazifop-butyl and chlorfenapyr in a weight ratio of 3:2, the composite dispersant is prepared by mixing modified acrylate and modified lignin in a weight ratio of 4:3; the composite synergist is prepared by mixing trimethylglycine and silicone emulsion in a weight ratio of 2:3, and the surfactant is composed of lauramide propyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate in a weight ratio of 1:1; The preparation method of the above-mentioned composition containing hexaflufenamide comprises the following steps: S91. Mix the active ingredient, surfactant, ethylene glycol, gum arabic, silicone defoamer, composite synergist, composite dispersant, potassium sorbate, propylene glycol methyl ether acetate and water according to their weight fractions, and pre-disperse and shear at a speed of 3000 rpm for 30 min to obtain a mixed solution; S92, subjecting the mixed solution to ultrafine grinding, grinding at a rotation speed of 2500 rpm for 3 hours, detecting the particle size D90 ≤ 0.5 μm, and filtering to obtain a composition containing hexaflufenamide. Example 3
[0037] A composition containing fluazifop-butyl, comprising the following raw materials by weight: 17 parts of active ingredient, 5 parts of surfactant, 2.5 parts of ethylene glycol, 4.5 parts of gum arabic, 0.4 parts of silicone defoamer, 4.5 parts of composite synergist, 2.5 parts of composite dispersant, 0.7 parts of potassium sorbate, 5.5 parts of propylene glycol methyl ether acetate, and 73 parts of water; wherein the active ingredient is prepared by mixing fluazifop-butyl and chlorfenapyr in a weight ratio of 3:2, the composite dispersant is prepared by mixing modified acrylate and modified lignin in a weight ratio of 4:3; the composite synergist is prepared by mixing trimethylglycine and silicone emulsion in a weight ratio of 2:3, and the surfactant is composed of lauramide propyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate in a weight ratio of 1:1; The preparation method of the above-mentioned composition containing hexaflufenamide comprises the following steps: S91. Mix the active ingredient, surfactant, ethylene glycol, gum arabic, silicone defoamer, composite synergist, composite dispersant, potassium sorbate, propylene glycol methyl ether acetate and water according to their weight fractions, and pre-disperse and shear at a speed of 3000 rpm for 30 min to obtain a mixed solution; S92, subjecting the mixed solution to ultrafine grinding, grinding at a rotation speed of 2500 rpm for 3 hours, detecting the particle size D90 ≤ 0.5 μm, and filtering to obtain a composition containing hexaflufenamide.
[0038] Comparative Example 1 The same as Example 3, except that the composite dispersant is modified acrylate.
[0039] Comparative Example 2 The same as Example 3, except that the composite dispersant is modified lignin.
[0040] Comparative Example 3 The same as Example 3, except that the composite synergist is trimethylglycine.
[0041] Comparative Example 4 The same as Example 3, except that the composite synergist is an organosilicon emulsion.
[0042] Comparative Example 5 The same as Example 3, except that the surfactant is lauramide propyl hydroxysulfobetaine.
[0043] Comparative Example 6 The same as Example 3, except that the surfactant is tristyrylphenol polyoxyethylene ether phosphate.
[0044] 1. Performance testing The compositions containing hexaflufenamide prepared in Examples 1 to 3 and Comparative Examples 1 to 6 were sampled and subjected to the following tests. The test results are shown in Table 1.
[0045] Suspension rate detection: Test according to GB / T14825-2006 pesticide suspension rate determination method; Pesticide adhesion rate detection: a cover glass (2 cm×2 cm) was vertically immersed in the composition containing fluazifop-butyl prepared in Examples 1 to 3 and Comparative Examples 1 to 6 for 1 minute, and then the amount of pesticide on the cover glass was measured after being vertically taken out and tilted at 50° for 2 minutes, and the pesticide adhesion rate was calculated; Low temperature stability: refer to GB / T19137-2003 standard to conduct low temperature stability test, observe the appearance change of the sample for 3 hours, and record the measured results in Table 1; Extended area test: A composition containing fluazifop-butyl was added to the droplet generator to generate a single pesticide droplet with a diameter of 340-360 μm and released onto the cabbage leaf surface, which was then observed under a microscope (16x focal length); the droplet area was measured using the Image-proplu6.0 image processing software.
[0046] Table 1 Performance test
[0047] 2. Field trials for the prevention and control of cabbage diamondback moth The efficacy test of the compositions containing hexaflufenamide prepared in Examples 1 to 3 and Comparative Examples 1 to 6 was conducted. The test was conducted with 10 treatments, one of which was a blank control CK. Each treatment was repeated 4 times, with a total of 40 areas, each area of about 20 m 2 , each treatment was randomly arranged. The experimental field was flat, the cabbage was in the early stage of rosette, and the growth was good. It was cloudy on the day of application, the temperature was 22-27℃, and the northerly wind was 3-4. From the application of the pesticide to the end of the investigation, there were 6 cloudy days, 1 cloudy day, and no precipitation. The front and back of the cabbage leaves were evenly sprayed, and the blank control CK was sprayed with an equal amount of clean water. Only one pesticide was applied during the experiment, the dosage was 25mL / mu, and the dilution multiple was 500 times. 18d before the application of the pesticide, the experimental field used highly effective cypermethrin to control the diamondback moth once. The survey method adopted the five-point sampling method. 10 cabbages were randomly selected in each area. The insect population density was investigated before and 1, 3, and 7d after the application of the pesticide, and the data was recorded to calculate the insect population reduction rate and the corrected control effect. During the experiment, it was observed whether the agent caused phytotoxicity to the cabbage and had an effect on the diamondback moth pest. The formula for calculating the insect population reduction rate and control effect is as follows: Insect population reduction rate = (insect population base - number of live insects after application) × 100% / insect population base; Corrected control effect = (insect population reduction rate in the pesticide treatment area - insect population reduction rate in the blank control area) × 100% / (100 - insect population reduction rate in the blank control area); The test results are shown in Table 2.
[0048] Table 2 Field test results of controlling cabbage diamondback moth
[0049] Analyzing the data in Table 1 and Table 2, we can see that: 1) The compositions containing hexaflufenamide prepared in Examples 1 to 3 have the advantages of synergistic enhancement, high selectivity, environmental compatibility, reduced environmental pollution, and cost savings in preventing and controlling thrips pests, beet armyworms, and diamondback moths. By adding a composite dispersant, the suspension rate, dispersibility, and pesticide adhesion rate of the pesticide suspension can be significantly improved; by adding a composite synergist, the evaporation of the liquid on the surface of the crop can be significantly reduced, while the systemicity of the agent on the surface of the crop can be increased, the utilization rate of the pesticide can be improved, and the control effect of pests and diseases can be improved, thereby reducing the cost of the drug; at the same time, the added surfactant has hydrophilic and lipophilic properties, low viscosity, and good spreadability, which can make the agent better adhere to the surface of the leaf and penetrate into the interior of the leaf tissue, significantly improving the control effect of pests and diseases.
[0050] 2) The performance comparison analysis of the composition containing hexaflufenamide prepared in combination with Example 3 and Comparative Examples 1-2 shows that the composite dispersant is prepared by mixing modified acrylate and modified lignin in a mass ratio of 4:3. The coordination between them can significantly improve the suspension rate, dispersibility and pesticide adhesion rate of the pesticide suspension concentrate. At the same time, this synergistic effect is conducive to improving the good control effect of the composition containing hexaflufenamide.
[0051] 3) The performance comparison analysis of the composition containing hexafluazole worm amide prepared in combination with Example 3 and Comparative Examples 3-4 shows that the composite synergist is prepared by mixing trimethylglycine and silicone emulsion in a mass ratio of 2:3. Trimethylglycine has excellent emulsification, dispersion and wetting properties, can significantly reduce the surface tension of the liquid, so that the liquid forms a stable liquid film on the surface of the crop, and reduces the evaporation loss of the active ingredient. At the same time, trimethylglycine can also enhance the affinity of the liquid to the surface of the crop, improve the adhesion and spreadability of the liquid on the surface of the plant, thereby improving the utilization rate and control effect of the agent. Silicone emulsion has good stability and biocompatibility, and can play a role in thickening, stabilizing and improving suspension in the pesticide composition. By utilizing the synergistic effect between them, the evaporation of the liquid on the surface of the crop can be significantly reduced, while increasing the systemicity of the agent on the surface of the crop, improving the utilization rate of the pesticide, and improving the control effect of pests and diseases, thereby reducing the cost of medication.
[0052] 4) The performance comparison analysis of the composition containing hexaflufenamide prepared in combination with Example 3 and Comparative Examples 5-6 shows that the surfactant is composed of lauryl amide propyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate in a mass ratio of 1:1. By utilizing the synergistic effect between them, the agent can be better attached to the leaf surface and penetrate into the leaf tissue, thereby significantly improving the control effect of pests and diseases.
[0053] 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 composition containing hexaflufenamide, characterized in that: The preparation raw materials include the following by weight: 15-18 parts of active ingredients, 4-6 parts of surfactants, 2-3 parts of ethylene glycol, 4-5 parts of thickeners, 0.3-0.5 parts of defoamers, 4-5 parts of composite synergists, 2-3 parts of composite dispersants, 0.5-0.8 parts of preservatives, 5-6 parts of propylene glycol methyl ether acetate, and 70-75 parts of water; wherein the active ingredient is prepared by mixing hexaflufenacil and cypermethrin in a weight ratio of 3:2, and the composite dispersant is prepared by mixing modified acrylate and modified lignin.
2. A composition containing hexaflufenamide according to claim 1, characterized in that: The mass ratio of the modified acrylic ester to the modified lignin is 4:
3.
3. A composition containing hexaflufenamide according to claim 1, characterized in that: The preparation method of the modified acrylate comprises the following steps: S31, according to the mass fraction, take 10 parts of polyethylene glycol, heat it to 130°C, add 1 part of octyl polyoxyethylene ether, stir and react for 45 minutes, the stirring speed is 270r / min, after the addition is completed, continue to keep the temperature at 110°C for 25 minutes to obtain a polyethylene glycol emulsion; S32. According to the mass proportions, take 0.75 parts of octyl polyoxyethylene ether and 1 part of deionized water and mix them evenly. After stirring to dissolve, add 5 parts of methyl acrylate and 0.3 parts of potassium persulfate and stir and emulsify for 40 minutes. Add polyethylene glycol emulsion and heat to 120°C. Continue stirring and reacting for 2 hours. When the reaction temperature is reduced to 90°C, perform vacuum distillation to obtain modified acrylate.
4. A composition containing hexaflufenamide according to claim 1, characterized in that: The preparation method of the modified lignin is as follows: according to the mass fractions, 1 part of tartaric acid, 0.3 parts of sodium hypophosphite and 50 parts of deionized water are added into a reactor, 12 parts of alkaline lignin are added after stirring evenly, the temperature is raised to 90° C., reacted for 6 hours, filtered, washed and dried to obtain the modified lignin.
5. A composition containing hexaflufenamide according to claim 1, characterized in that: The composite synergist is prepared by mixing trimethylglycine and silicone emulsion in a mass ratio of 2:
3.
6. A composition containing hexaflufenamide according to claim 5, characterized in that: The preparation method of the silicone emulsion is as follows: 23 parts of hydroxy silicone oil and 18 parts of amino polyether block silicone oil are mixed according to the weight parts, stirred for 30 minutes, and then 4 parts of XL-40 and 3 parts of XL-70 are added, the temperature is raised to 45° C., and the mixture is fully stirred for 18 minutes. Then, 1 part of acetic acid is added, and the mixture is stirred for 20 minutes. Then, water is slowly dripped into the mixture while stirring, and 40 parts of water are added at a dripping speed of 0.01 parts / 10s. Then, 1 part of acetic acid is added, and 0.5 parts of silicone defoamer are added, and the mixture is stirred for 5 minutes to obtain the silicone emulsion.
7. A composition containing hexaflufenamide according to claim 1, characterized in that: The surfactant is composed of lauramide propyl hydroxysulfobetaine and tristyrylphenol polyoxyethylene ether phosphate in a mass ratio of 1:
1.
8. A composition containing hexaflufenamide according to claim 1, characterized in that: The thickener is gum arabic; the preservative is potassium sorbate; and the defoaming agent is an organosilicon defoaming agent.
9. A method for preparing a composition containing hexaflufenamide according to any one of claims 1 to 8, characterized in that: The following steps are involved: S91. Mix the active ingredient, surfactant, ethylene glycol, thickener, defoamer, composite synergist, composite dispersant, preservative, propylene glycol methyl ether acetate and water according to their weight fractions, and pre-disperse and shear at a speed of 3000 rpm for 30 min to obtain a mixed solution; S92, subjecting the mixed solution to ultrafine grinding, grinding at a rotation speed of 2500 rpm for 3 hours, detecting the particle size D90 ≤ 0.5 μm, and filtering to obtain a composition containing hexaflufenamide.
10. Use of a composition containing hexaflufenamide according to any one of claims 1 to 8, characterized in that: The composition containing hexaflufenamide is used for crops to control thrips pests, beet armyworm and diamondback moth.
Citation Information
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