A pesticide composition containing glufosinate-ammonium and fluazifop-butyl and a preparation method thereof

Abstract

The present application relates to the field of pesticide technology, and more particularly to a pesticide composition containing refined glufosinate-ammonium and fluazifop-butyl and a preparation method thereof. A pesticide composition containing refined glufosinate-ammonium and fluazifop-butyl, by mass fraction, includes the following preparation raw materials: 25-30 parts of active ingredients, 5-6 parts of composite surfactants, 1-2 parts of glycerol, 2-3 parts of organic thickeners, 0.2-0.3 parts of defoamers, 4-5 parts of composite synergists, 1-1.3 parts of dispersants, 0.3-0.5 parts of preservatives, and 160-170 parts of water. The pesticide composition containing refined glufosinate-ammonium and fluazifop-butyl of the present application shows significant technical advantages in terms of synergistic enhancement, high selectivity, environmental compatibility, improving utilization and efficacy, and optimizing anti-settling performance.

Description

Technical Field

[0001] The present application relates to the technical field of pesticides, and in particular to a pesticide composition containing glufosinate-ammonium and fluazifop-butyl and a preparation method thereof. Background Art

[0002] Pesticides are important agricultural production materials, and are crucial for preventing diseases and controlling pests, and promoting stable and high yields of grain and agriculture. However, due to the large amount of pesticides used and the unscientific application methods, problems such as increased production costs, excessive residues in agricultural products, crop damage, and environmental pollution have arisen. In order to promote the transformation of agricultural development methods, effectively control the use of pesticides, ensure agricultural production safety, agricultural product quality safety, and ecological environment safety, and promote sustainable agricultural development.

[0003] Glufosinate-ammonium, international common name: Glufosinate-P, CA registration number: 35597-44-5, chemical name: (2S)-2-amino-4-[hydroxy(methyl)phosphinyl]butyric acid. Molecular formula C 5 H 12 NO 4 P, molecular weight: 181.23; mechanism of action is glutamine synthetase inhibitor, which leads to ammonium ion accumulation in plants, inhibits photosynthesis, and achieves weed control effect. Glufosinate ammonium has low toxicity and is relatively safe. It is easy to degrade in the soil, safe for crops, has small drift, and is safe for adjacent crops. It has a wide spectrum of weed control (effective against a variety of annual and perennial weeds), can control malignant weeds resistant to glyphosate, has high activity, kills weeds quickly (between glyphosate and paraquat), and has a long lasting effect. It mainly kills weeds by contact, will not be transferred to other places, and is safe for subsequent crops; it has very good water solubility, stable structure, convenient processing and mixing, low environmental pollution, and realizes higher refinement of pesticides; it has a wide range of applications and can be used in orchards, vineyards, rubber plantations, non-arable land and other plots to control a variety of annual and perennial broad-leaved weeds and grass weeds.

[0004] Fluoroglycofen, chemical name: 0-[5-(2-chloro-a,a,a-trifluoro-p-tolyloxy)-2-nitrobenzoyl] ethyl hydroxyacetate, molecular formula: C1 6 H 9 CIF 3 NO 7 Fluorosulfuron is a diphenyl ether herbicide, a selective, contact-type, post-emergence stem and leaf treatment agent, absorbed by the stems and leaves of weeds. This product is absorbed by plants and is effective only under light conditions. Its activity is less affected by ambient temperature. It can control a variety of broadleaf weeds, such as Polygonaceae, Amaranth, Xanthium, Solanum nigrum, Portulaca oleracea, Veronica, Shepherd's purse, Cirsium japonicum, etc. It is commonly used to remove broadleaf weeds in soybean fields, and can also be used for weeding in wheat, barley, peanuts, rice fields, etc.

[0005] At present, the existing pesticides containing glufosinate ammonium and fluazifop-butyl have poor hydrophilicity and permeability, which results in that the active ingredients in the pesticides cannot be efficiently adsorbed deep into the surface of weeds, resulting in poor weed control effect of the pesticide composition, large dosage and poor safety. Summary of the invention

[0006] The purpose of the present application is to provide a pesticide composition containing refined glufosinate-ammonium and fluazifop-butyl and a preparation method thereof in view of the deficiencies of the current technology. The pesticide composition containing refined glufosinate-ammonium and fluazifop-butyl prepared in the present application has the advantages of synergistic enhancement, high selectivity, environmental compatibility, reduced environmental pollution, cost savings, etc. At the same time, the added composite surfactant can effectively reduce the surface tension of the pesticide composition, the contact angle of the liquid on the plant surface and the penetration time, penetrate into the plant leaf tissue, kill weeds, and improve the utilization rate of the pesticide composition and the efficacy of the unit pesticide component.

[0007] In the first aspect, the present application provides a pesticide composition containing glufosinate-ammonium and fluazifop-butyl, which adopts the following technical scheme:

[0008] A pesticide composition containing glufosinate-ammonium and fluazifop-butyl, comprising the following raw materials by mass: 25-30 parts of active ingredients, 5-6 parts of composite surfactants, 1-2 parts of glycerol, 2-3 parts of organic thickeners, 0.2-0.3 parts of defoamers, 4-5 parts of composite synergists, 1-1.3 parts of dispersants, 0.3-0.5 parts of preservatives, and 160-170 parts of water, wherein the active ingredient is prepared by mixing glufosinate-ammonium and fluazifop-butyl in a mass ratio of 5:1.

[0009] By adopting the above technical scheme, the pesticide composition containing glufosinate and fluazifop-butyl in the present application achieves the advantages of synergy, high selectivity, environmental compatibility and cost-effectiveness by carefully selecting and proportioning various ingredients. Active ingredients (glufosinate and fluazifop-butyl): As the main herbicide ingredients, they are mixed in a mass ratio of 5:1, which can effectively kill weeds and be safe for crops. Glufosinate is a non-selective herbicide, while fluazifop-butyl provides selectivity. This combination can reduce damage to crops and improve the weed control effect. Composite surfactant: including coconut oil diethanolamide, lauramide propyl hydroxysulfobetaine, fatty alcohol polyoxyethylene ether sodium sulfate, methylpentyl alcohol polyoxyethylene ether and trihydroxyethylamine, etc. These ingredients cooperate with each other to reduce the surface tension and contact angle of the pesticide composition, promote the penetration of the liquid on the plant surface, and improve the efficacy. Glycerol: As an antifreeze agent, it helps to maintain the low-temperature stability of the pesticide composition. Organic thickener: By forming a polyurethane film and expanding and rupturing in water, the thickening components are released, a three-dimensional network structure is formed, the viscosity of the system is increased, the anti-settling performance of the pesticide composition is optimized, and the comprehensive performance is improved. Defoamer: It is used to eliminate the foam generated during production and use to ensure the quality and application effect of the product. Composite synergist (alkyl glycoside and silicone emulsion): Alkyl glycoside improves the effect and biodegradability of pesticides and reduces the surface tension of the product; XL-50 and XL-90 in silicone emulsion are used in combination to provide microemulsion effect and good stability, increase the residence time of the liquid on the plant surface, reduce the loss of active ingredients, and significantly improve the efficacy. Dispersant: Helps the active ingredients to be evenly dispersed in the pesticide composition to prevent precipitation and ensure consistent effects every time it is used. Preservative: Prevents microbial contamination and deterioration of the pesticide composition during storage. Water: As a solvent, it allows various ingredients to be evenly mixed for easy spraying and application. In summary, the pesticide composition in the present application not only improves the weed control effect but also enhances environmental compatibility and cost-effectiveness through the synergistic effect of various components, and is an efficient and environmentally friendly weed control solution.

[0010] Preferably, the composite synergist is prepared by mixing alkyl polyglycoside and silicone emulsion in a mass ratio of 2:3.

[0011] By adopting the above technical scheme, the composite synergist is prepared by mixing alkyl glycoside and silicone emulsion in a mass ratio of 2:3. The role in this application is to improve the utilization efficiency of the pesticide composition and the efficacy of the unit pesticide active ingredient. Alkyl glycoside is a surfactant with good biodegradability, which can reduce the surface tension of the product, enable the agent to be fully spread on the crop, make the contact area between the agent and the crop larger, enhance the residence time of the liquid on the plant surface, reduce the loss of active ingredients, and make the efficacy more significant. At the same time, alkyl glycoside can also improve the effect and biodegradability of pesticides. XL-50 and XL-90 in the silicone emulsion are isomeric alcohol ether products of BASF. The specific ratio of the two is compounded and used in the silicone emulsion, so that the silicone emulsion has a microemulsion effect and good stability. Hydroxyl silicone oil and amino polyether block silicone oil are compounded, and the pH value is adjusted with acetic acid, and water is slowly added to form a good water-in-oil silicone microemulsion. This microemulsion has a good spreading effect in the formulation of the pesticide composition containing glufosinate and fluazifop-butyl, and significantly improves the efficacy. Alkyl glycosides and silicone emulsions are used in a specific ratio. By utilizing the synergistic effect between them, they can be well conducted in the plant body, improving the utilization rate of the pesticide composition and the efficacy of the unit pesticide active ingredient. This synergistic effect is mainly reflected in the following aspects: Alkyl glycosides can reduce the surface tension of the product, so that the agent can be fully spread on the crop, so that the contact area between the agent and the crop is larger, and the residence time of the liquid on the plant surface can be enhanced, the loss of active ingredients is reduced, and the efficacy is more significant. The silicone emulsion can provide good spreading and stability, so that the pesticide composition forms a uniform film on the plant surface, which is conducive to the absorption and conduction of the agent. There are interactive forces between alkyl glycosides and silicone emulsions, such as hydrogen bonds, van der Waals forces, etc. These forces help to improve the stability and adhesion of the pesticide composition, thereby improving the utilization rate and efficacy of the pesticide. The molecular structures of alkyl glycoside and silicone emulsion are complementary. The hydrophilic groups in the alkyl glycoside molecules can interact with the hydrophobic groups in the silicone emulsion to form a stable complex, which is beneficial to the stability and conduction of the pesticide composition.

[0012] Preferably, the composite surfactant comprises the following raw materials, measured by mass: 10 parts of lauramide propyl hydroxysulfobetaine, 8 parts of sodium polyoxyethylene fatty alcohol ether sulfate, 12 parts of coconut acid diethanolamide, 25 parts of methylvaleryl alcohol polyoxyethylene ether, 10 parts of trihydroxyethylamine, and 10 parts of deionized water.

[0013] By adopting the above technical scheme, each component in the composite surfactant can effectively reduce the surface tension of the pesticide composition and the contact angle of the liquid on the plant surface. This helps the liquid to penetrate more easily into the plant leaf tissue, thereby improving the utilization rate and efficacy of the pesticide. By reducing the surface tension, the composite surfactant makes it easier for the liquid to penetrate into the internal structure of the plant leaves, which helps to kill weeds more effectively and improve the effect of the pesticide. The different components in the composite surfactant cooperate with each other to improve the stability of the pesticide composition and the spreadability on the plant surface. This helps the agent to be evenly distributed on the crop, increases the contact area between the agent and the crop, and thus improves the efficacy. There is a synergistic effect between the different components in the composite surfactant, which can enhance the effect of the pesticide, so that a lower dose of pesticide can achieve the expected weeding effect, thereby saving costs and reducing environmental pollution. The use of composite surfactants helps to improve the environmental compatibility of pesticides and reduce pollution to the environment. This is because they can help pesticides act more effectively on target weeds while reducing the impact on non-target organisms. In summary, the role of the composite surfactant in the present application is to effectively reduce the surface tension and contact angle of the pesticide composition, enhance permeability, and improve stability and spreadability through the synergistic effect between its components, thereby achieving the advantages of synergistic enhancement, high selectivity, environmental compatibility, reduced environmental pollution, and cost savings.

[0014] Preferably, the preparation method of the composite surfactant comprises the following steps:

[0015] S31, according to the mass parts, the fatty alcohol polyoxyethylene ether sodium sulfate and trihydroxyethylamine are mixed, stirred evenly, and then coconut acid diethanolamide is added and stirred evenly to obtain a mixed solution;

[0016] S32. Add lauramide propyl hydroxysulfobetaine, methylpentyl alcohol polyoxyethylene ether and deionized water to the mixed solution according to their mass fractions, stir and heat to 40°C, stir for 60 minutes, and cool to room temperature to obtain a composite surfactant.

[0017] Preferably, the preparation method of the methylpentynol polyoxyethylene ether is as follows: according to the mass fraction, under nitrogen protection, 98 parts of methylpentynol are slowly heated to 120°C, dehydrated and cooled by 30°C, 2 parts of sodium hydroxide are added, the temperature is again raised to 120°C and 484 parts of ethylene oxide are added, reacted at 120°C and 0.01MPa for 2 hours, cooled and discharged to obtain methylpentynol polyoxyethylene ether.

[0018] By adopting the above technical scheme, the prepared polyoxyethylene methyl pentyl alcohol ether can effectively reduce the surface tension of the pesticide composition, which makes it easier for the liquid to spread on the surface of plant leaves, increases the contact area between the agent and weeds, and thus improves the efficacy. By reducing the contact angle, polyoxyethylene methyl pentyl alcohol ether promotes the rapid spreading and penetration of the liquid on the plant surface, which helps the liquid to enter the plant leaf tissue faster, improves the utilization rate of the pesticide and the efficacy of the unit pesticide active ingredient. Due to its excellent permeability and spreadability, polyoxyethylene methyl pentyl alcohol ether can help pesticides kill weeds more effectively and improve the overall effect of pesticides. When used in conjunction with other surfactants such as coconut oil diethanolamide, lauramide propyl hydroxysulfobetaine, fatty alcohol polyoxyethylene ether sodium sulfate, etc., polyoxyethylene methyl pentyl alcohol ether can exert a better synergistic effect, further improving the utilization rate and efficacy of the pesticide composition. Due to the improved utilization rate and effect of pesticides, the amount of pesticides used can be reduced, thereby reducing the cost of farmers. In summary, methylpentyl alcohol polyoxyethylene ether not only has excellent surface activity itself, but also can synergize with other ingredients to significantly improve the overall performance of the pesticide composition, including improving efficacy, reducing costs and reducing environmental pollution.

[0019] 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 their mass fractions, stirred for 20 minutes, then 4 parts of XL-50 and 3 parts of XL-90 are added, the temperature is raised to 47°C, and the mixture is fully stirred for 8 minutes. Then, 1 part of acetic acid is added, and the mixture is stirred for 15 minutes. Then, 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 a silicone defoamer is added, and the mixture is stirred for 5 minutes to obtain a silicone emulsion.

[0020] By adopting the above technical scheme, the silicone emulsion in this application is composed of hydroxy silicone oil, amino polyether block silicone oil, XL-50 and XL-90. Among them, hydroxy silicone oil and amino polyether block silicone oil are the main active ingredients, and XL-50 and XL-90 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 alkyl glycosides, 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 pesticide composition formula containing glufosinate and fluazifop-butyl, and significantly improve the efficacy.

[0021] Preferably, the method for preparing the organic thickener comprises the following steps:

[0022] S61. Dissolve 5 parts of N-isopropylacrylamide and 14 parts of acrylamide in 10 parts of water according to their weight, adjust the pH to 9, and obtain a polymerization monomer solution for later use; mix 6 parts of sorbitan oleate and 18 parts of petroleum ether to obtain a dispersion for later use;

[0023] S62, mixing the polymerization monomer solution and the dispersion according to the mass fractions, and then homogenizing them, the homogenization speed is 3500 rpm, the processing time is 15 minutes, and a polymerization reaction liquid is obtained; 0.003 parts of ammonium persulfate are added to the polymerization reaction liquid, and the polymerization reaction is carried out at 55° C. under anaerobic conditions for 5 hours to obtain a polymer emulsion, which is reserved;

[0024] S63. Dissolve 1.6 parts of dicyclohexylmethane-4,4'-diisocyanate and 6.4 parts of polyethylene glycol in 9 parts of petroleum ether according to their mass fractions to obtain a prepolymerization solution. After mixing the prepolymerization solution and the polymer emulsion, add 0.005 parts of dibutyltin dilaurate and 0.6 parts of diethylene glycol, increase the temperature and carry out polymerization reaction at 50°C under anaerobic conditions for 4 hours. The reaction product is filtered to obtain a filter cake, which is washed with petroleum ether and dried to obtain an organic thickener.

[0025] By adopting the above technical scheme, the prepared organic thickener increases the viscosity of the mixed system by forming a three-dimensional network structure, so that the original drug particles in the pesticide composition are not easy to settle, thereby improving the stability of the pesticide composition. At the same time, this network structure helps the attachment and penetration of the active ingredients of the pesticide on the surface of the plant, thereby improving the utilization rate and efficacy of the pesticide. The network structure formed by the organic thickener in the water dispersion system enables the pesticide composition to have better spreadability on the surface of the plant, so that the agent can contact the crop more fully, thereby improving the effect of the pesticide. The polyurethane film in the organic thickener is formed by the reaction of dicyclohexylmethane-4,4'-diisocyanate and polyethylene glycol, and has good biodegradability. This makes the pesticide composition more easily decomposed by microorganisms after use, reducing pollution to the environment. The organic thickener cooperates with other components such as composite surfactants, alkyl glycosides, silicone emulsions, etc., and utilizes the synergistic effect between them to conduct well in the plant body, thereby improving the utilization rate of the pesticide composition and the efficacy of the unit pesticide active ingredient. This synergistic effect makes the pesticide composition have higher selectivity and lower toxicity, and has less impact on non-target organisms. In summary, the organic thickener plays a multi-faceted role in the pesticide composition in this application, such as increasing viscosity and stability, enhancing spreadability, improving biodegradability, and exerting synergistic effects, which comprehensively improves the comprehensive performance of the pesticide composition.

[0026] Preferably, the dispersant is aromatic phenol polyoxyethylene succinate sulfonate.

[0027] Preferably, the preservative is sodium benzoate; and the defoaming agent is an organosilicon defoaming agent.

[0028] In a second aspect, the present application provides a method for preparing a pesticide composition containing glufosinate-ammonium and fluazifop-butyl, using the following technical solution:

[0029] As a general technical concept, the present application also provides a method for preparing the above-mentioned pesticide composition containing glufosinate-ammonium and fluazifop-butyl, comprising the following steps:

[0030] S91. Mix the active ingredient, glycerol, composite synergist, composite surfactant and water according to their weight proportions, and stir for 15-20 minutes to obtain solution A;

[0031] S92. Mix an organic thickener, a defoamer, a dispersant and a preservative according to their weight proportions, add solution A, mix and stir for 8-10 minutes to obtain a pesticide composition containing glufosinate-ammonium and fluazifop-butyl.

[0032] Preferably, in step S91, the stirring speed is 200-300 r / min, and in step S92, the stirring speed is 150-200 r / min.

[0033] In summary, the beneficial technical effects of this application are:

[0034] 1. Synergistic effect: The synergistic effect of the pesticide composition is achieved through the scientific ratio of glufosinate-ammonium and fluazifop-butyl, as well as the addition of composite surfactants and composite synergists. This synergistic effect not only improves the control effect of pesticides on weeds, but also reduces the amount of pesticides used, thereby saving costs.

[0035] 2. High selectivity: The pesticide composition is highly selective and can effectively control specific types of weeds without causing damage to crops. This helps reduce pesticide residues on crops and improve the safety of agricultural products.

[0036] 3. Environmental compatibility: Due to the use of raw materials with good biodegradability, such as alkyl glycosides and silicone emulsions, the pesticide composition can be degraded quickly in the environment, reducing environmental pollution. At the same time, its low toxicity also reduces the impact on non-target organisms.

[0037] 4. Improve the utilization rate and efficacy: The addition of composite surfactants and composite synergists effectively reduces the surface tension of the pesticide composition, the contact angle of the liquid on the plant surface and the penetration time, allowing the pesticide to penetrate into the plant leaf tissue faster and kill weeds. This not only improves the utilization rate of the pesticide composition, but also enhances the efficacy of the unit pesticide active ingredient.

[0038] 5. Optimize anti-settling performance: The use of organic thickeners forms a polyurethane film on the surface of the thickening polymer, which expands and ruptures in water to release thickening components and form a three-dimensional network structure in the water dispersion system, increasing the viscosity of the mixed system. This feature effectively improves the anti-settling performance of the original drug in the pesticide composition, ensures the stability of the pesticide during storage and use, and comprehensively improves the comprehensive performance of the pesticide composition.

[0039] 6. Good spreading property: Alkyl polyglycoside and organosilicon emulsion are used in a specific ratio, and the synergistic effect between them is utilized to significantly improve the utilization rate of the pesticide composition and the efficacy of the active ingredient per unit of pesticide. At the same time, the organosilicon microemulsion has a good spreading effect in the formulation of the pesticide composition containing glufosinate-ammonium and fluazifop-butyl, significantly improving the efficacy. DETAILED DESCRIPTION

[0040] 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-50 and XL-90 are isomeric alcohol ether products of BASF.

[0041] In the following examples and preparation examples, 1 part means 50 g.

[0042] Preparation Example 1 Preparation of methylvalerynol polyoxyethylene ether

[0043] The preparation method of methylpentynol polyoxyethylene ether is as follows: according to the mass fraction, under nitrogen protection, 98 parts of methylpentynol are slowly heated to 120°C, dehydrated and cooled by 30°C, 2 parts of sodium hydroxide are added, the temperature is again raised to 120°C and 484 parts of ethylene oxide are added, reacted at 120°C and 0.01MPa for 2 hours, cooled and discharged to obtain methylpentynol polyoxyethylene ether.

[0044] Preparation Example 2 Preparation of composite surfactant

[0045] The composite surfactant comprises the following raw materials by weight: 10 parts of lauramide propyl hydroxysulfobetaine, 8 parts of sodium polyoxyethylene fatty alcohol ether sulfate, 12 parts of coconut acid diethanolamide, 25 parts of methylpentyl alcohol polyoxyethylene ether, 10 parts of trihydroxyethylamine, and 10 parts of deionized water, wherein the methylpentyl alcohol polyoxyethylene ether is prepared in Preparation Example 1; the preparation method of the composite surfactant comprises the following steps:

[0046] S31, according to the mass parts, the fatty alcohol polyoxyethylene ether sodium sulfate and trihydroxyethylamine are mixed, stirred evenly, and then coconut acid diethanolamide is added and stirred evenly to obtain a mixed solution;

[0047] S32. Add lauramide propyl hydroxysulfobetaine, methylpentyl alcohol polyoxyethylene ether and deionized water to the mixed solution according to their mass fractions, stir and heat to 40°C, stir for 60 minutes, and cool to room temperature to obtain a composite surfactant.

[0048] Preparation Example 3 Preparation of silicone emulsion

[0049] 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 20 minutes, 4 parts of XL-50 and 3 parts of XL-90 are added, the temperature is raised to 47°C, and the mixture is fully stirred for 8 minutes. 1 part of acetic acid is added, and after stirring for 15 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 a silicone defoamer is added, and the mixture is stirred for 5 minutes to obtain a silicone emulsion.

[0050] Preparation Example 4 Preparation of organic thickener

[0051] The preparation method of the organic thickener comprises the following steps:

[0052] S61. Dissolve 5 parts of N-isopropylacrylamide and 14 parts of acrylamide in 10 parts of water according to their weight, adjust the pH to 9, and obtain a polymerization monomer solution for later use; mix 6 parts of sorbitan oleate and 18 parts of petroleum ether to obtain a dispersion for later use;

[0053] S62, mixing the polymerization monomer solution and the dispersion according to the mass fractions, and then homogenizing them, the homogenization speed is 3500 rpm, the processing time is 15 minutes, and a polymerization reaction liquid is obtained; 0.003 parts of ammonium persulfate are added to the polymerization reaction liquid, and the polymerization reaction is carried out at 55° C. under anaerobic conditions for 5 hours to obtain a polymer emulsion, which is reserved;

[0054] S63. Dissolve 1.6 parts of dicyclohexylmethane-4,4'-diisocyanate and 6.4 parts of polyethylene glycol in 9 parts of petroleum ether according to their mass fractions to obtain a prepolymerization solution. After mixing the prepolymerization solution and the polymer emulsion, add 0.005 parts of dibutyltin dilaurate and 0.6 parts of diethylene glycol, increase the temperature and carry out polymerization reaction at 50°C under anaerobic conditions for 4 hours. The reaction product is filtered to obtain a filter cake, which is washed with petroleum ether and dried to obtain an organic thickener. Example 1

[0055] A pesticide composition containing glufosinate ammonium and fluazifop-butyl, comprising the following raw materials by weight: 25 parts of active ingredients, 5 parts of composite surfactants, 1 part of glycerol, 2 parts of organic thickeners, 0.2 parts of organosilicon defoamers, 4 parts of composite synergists, 1 part of arylphenol polyoxyethylene succinate sulfonate, 0.3 parts of sodium benzoate, and 160 parts of water, wherein the active ingredient is prepared by mixing glufosinate ammonium and fluazifop-butyl in a weight ratio of 5:1, and the composite synergist is prepared by mixing an alkyl glycoside and an organosilicon emulsion in a weight ratio of 2:3.

[0056] The preparation method of the above-mentioned pesticide composition containing glufosinate-ammonium and fluazifop-butyl comprises the following steps:

[0057] S91. According to the mass fractions, the active ingredient, glycerol, composite synergist, composite surfactant and water were mixed and stirred at a speed of 200 r / min for 20 minutes to obtain solution A;

[0058] S92. Mix an organic thickener, a silicone defoamer, arylphenol polyoxyethylene succinate sulfonate and sodium benzoate in parts by mass, add solution A, mix and stir at a speed of 150 r / min for 10 minutes to obtain a pesticide composition containing glufosinate ammonium and fluazifop-butyl. Example 2

[0059] A pesticide composition containing glufosinate ammonium and fluazifop-butyl, comprising the following raw materials by weight: 30 parts of active ingredients, 6 parts of composite surfactants, 2 parts of glycerol, 3 parts of organic thickeners, 0.3 parts of organosilicon defoamers, 5 parts of composite synergists, 1.3 parts of arylphenol polyoxyethylene succinate sulfonates, 0.5 parts of sodium benzoate, and 170 parts of water, wherein the active ingredient is prepared by mixing glufosinate ammonium and fluazifop-butyl in a weight ratio of 5:1, and the composite synergist is prepared by mixing an alkyl glycoside and an organosilicon emulsion in a weight ratio of 2:3.

[0060] The preparation method of the above-mentioned pesticide composition containing glufosinate-ammonium and fluazifop-butyl comprises the following steps:

[0061] S91. According to the mass fractions, the active ingredient, glycerol, composite synergist, composite surfactant and water were mixed and stirred at a speed of 300 r / min for 15 minutes to obtain solution A;

[0062] S92. Mix an organic thickener, a silicone defoamer, arylphenol polyoxyethylene succinate sulfonate and sodium benzoate according to their mass fractions, add solution A, mix and stir at a speed of 200 r / min for 8 minutes to obtain a pesticide composition containing glufosinate ammonium and fluazifop-butyl. Example 3

[0063] A pesticide composition containing glufosinate ammonium and fluazifop-butyl, comprising the following raw materials by weight: 28 parts of active ingredients, 5.5 parts of composite surfactants, 1.5 parts of glycerol, 2.5 parts of organic thickeners, 0.25 parts of organosilicon defoamers, 4.5 parts of composite synergists, 1.2 parts of arylphenol polyoxyethylene succinate sulfonates, 0.4 parts of sodium benzoate, and 165 parts of water, wherein the active ingredient is prepared by mixing glufosinate ammonium and fluazifop-butyl in a weight ratio of 5:1, and the composite synergist is prepared by mixing an alkyl glycoside and an organosilicon emulsion in a weight ratio of 2:3.

[0064] The preparation method of the above-mentioned pesticide composition containing glufosinate-ammonium and fluazifop-butyl comprises the following steps:

[0065] S91. According to the mass fractions, the active ingredient, glycerol, composite synergist, composite surfactant and water were mixed and stirred at a speed of 250 r / min for 18 minutes to obtain solution A;

[0066] S92. Mix an organic thickener, a silicone defoamer, aromatic phenol polyoxyethylene succinate sulfonate and sodium benzoate in parts by mass, add solution A, mix and stir at a speed of 180 r / min for 9 minutes to obtain a pesticide composition containing glufosinate ammonium and fluazifop-butyl.

[0067] Comparative Example 1

[0068] The same as Example 3, except that an equal amount of lauramide propyl hydroxysulfobetaine is used instead of the complex surfactant.

[0069] Comparative Example 2

[0070] The same as Example 3, except that an equal amount of fatty alcohol polyoxyethylene ether sodium sulfate is used instead of the composite surfactant.

[0071] Comparative Example 3

[0072] The same as Example 3, except that an equal amount of coconut oil diethanolamide is used instead of the complex surfactant.

[0073] Comparative Example 4

[0074] The same as Example 3, except that an equal amount of methylvaleryl alcohol polyoxyethylene ether is used instead of the complex surfactant.

[0075] Comparative Example 5

[0076] The same as Example 3, except that an equal amount of water is used to replace the organic thickener.

[0077] Comparative Example 6

[0078] The same as Example 3, except that the composite synergist is an alkyl glycoside.

[0079] Comparative Example 7

[0080] The same as Example 3, except that the composite synergist is an organosilicon emulsion.

[0081] 1. Performance testing

[0082] The pesticide compositions containing glufosinate-ammonium and fluazifop-butyl prepared in Examples 1 to 3 and Comparative Examples 1 to 7 were tested. The test results are shown in Table 1.

[0083] Surface tension measurement: The maximum bubble pressure method was used on a BP-100 dynamic surface tension meter, the temperature was (25±1)℃, and the range of the liquid dynamic surface tension was 5-200000ms. The pesticide composition was diluted 1333 times. After the sample measurement was completed, the data was processed using KRüSS LabDesk software. Repeat 3 times and take the average value.

[0084] Contact angle measurement: Select fresh and clean Erigeron candidum leaves at the 6-leaf stage. Use the syringe provided by the OCA-50 contact angle meter to inject 3 μL of sample, adjust the workbench so that the leaf surface receives the droplet and start timing. Take an image after 30 seconds, and automatically integrate the image to measure the contact angle of the droplet on the plant surface. The whole process is controlled by the workstation. Repeat at least 3 times and calculate the average contact angle.

[0085] Permeability test: At 20°C, add 999.25g of distilled water + 0.75g of the pesticide composition into a 1000mL beaker, stir evenly, and put in a cotton disc after the foam disappears. Record the time from when the disc is put in to when it completely sinks to the bottom. Repeat 3 times and take the average value. The shorter the penetration time, the better the effect of the pesticide composition.

[0086] Table 1 Performance test

[0087]

[0088] 2. Efficacy test on weeds in non-cultivated land

[0089] The test site was selected in Xitaiping Village, Shankou Town, Daiyue District, Tai'an City, Shandong Province. No herbicides had been used in the test area for one year before the test, and the weed population was stable and evenly distributed. The main weeds in the test field were Leptochloa chinensis, Digitaria sanguinalis, Setaria viridis, and Portulaca oleracea, and there were also sporadic occurrences of Amaranthus retroflexus, Cyperus rotundus, and Teff. The test site was brown loam, with a relatively flat terrain and uniform soil fertility, an organic matter content of 10.25 mg / kg, and a pH of 6.7.

[0090] The experimental design is as follows: 11 treatments, corresponding to the pesticide compositions of Examples 1 to 3 and Comparative Examples 1 to 7 and the water control CK, each treatment is repeated 4 times, and the dosage is 400 g / hm 2 , sampling 30m in each plot 2 , arranged in random blocks, with protection rows set up between cells and around the experimental field.

[0091] Application time: Manual spraying was performed using a Linong HD-400 pressure storage sprayer. Stem and leaf spraying was used for 1 spray. Most monocotyledonous weeds had 6-8 leaves, and broadleaf weeds had 10-12 leaves (7-10 cm). The day of application was cloudy, with a northerly wind of 3-4, an average temperature of 23.48°C, a maximum temperature of 31.0°C, a minimum temperature of 21.3°C, and a relative humidity of 77.6%. During the test, there was no adverse weather factor.

[0092] The weeds investigated were Leptochloa chinensis, Digitaria sanguinalis, Setaria viridis, and Portulaca oleracea. The weed control efficacy was investigated 5 and 30 days after application.

[0093] Control effect = [number of weeds in the control area (or fresh weight) - number of weeds in the treatment area (or fresh weight)] / number of weeds in the control area (or fresh weight) × 100%.

[0094] The results are shown in Table 2.

[0095] Table 2 Herbal efficacy test

[0096]

[0097] Analyzing the data in Tables 1 and 2, we can see that:

[0098] 1) The pesticide composition containing glufosinate-ammonium and fluazifop-butyl prepared in Examples 1 to 3 has the advantages of synergistic effect, high selectivity, environmental compatibility, reduced environmental pollution, cost saving, etc. At the same time, the added composite surfactant can effectively reduce the surface tension of the pesticide composition, the contact angle and penetration time of the liquid on the plant surface, penetrate into the plant leaf tissue, kill weeds, and improve the utilization rate of the pesticide composition and the efficacy of the unit pesticide component.

[0099] 2) The performance comparison analysis of the pesticide composition containing glufosinate and fluazifop-butyl prepared in combination with Example 3 and Comparative Examples 1-4 shows that the components in the prepared composite surfactant can effectively reduce the surface tension of the pesticide composition and the contact angle of the liquid on the plant surface. This helps the liquid to penetrate more easily into the plant leaf tissue, thereby improving the utilization rate and efficacy of the pesticide. By reducing the surface tension, the composite surfactant makes it easier for the liquid to penetrate into the internal structure of the plant leaf, which helps to kill weeds more effectively and improve the effect of the pesticide. The different components in the composite surfactant cooperate with each other to improve the stability of the pesticide composition and the spreadability on the plant surface. This helps the agent to be evenly distributed on the crop, increases the contact area between the agent and the crop, and thus improves the efficacy. There is a synergistic effect between the different components in the composite surfactant, which can enhance the effect of the pesticide, so that a lower dose of the pesticide can achieve the expected weeding effect, thereby saving costs and reducing environmental pollution. The use of the composite surfactant helps to improve the environmental compatibility of the pesticide and reduce pollution to the environment. This is because they can help pesticides act more effectively on target weeds while reducing the impact on non-target organisms. In summary, the role of the composite surfactant in this application is to effectively reduce the surface tension and contact angle of the pesticide composition, enhance permeability, improve stability and spreadability through the synergistic effect between its components, thereby achieving the advantages of synergistic enhancement, high selectivity, environmental compatibility, reduced environmental pollution, and cost savings.

[0100] 3) The performance comparison analysis of the pesticide composition containing refined glufosinate and fluazifop-butyl prepared in combination with Example 3 and Comparative Example 5 shows that the organic thickener prepared in the present application increases the viscosity of the mixed system by forming a three-dimensional network structure, so that the original drug particles in the pesticide composition are not easy to settle, thereby improving the stability of the pesticide composition. At the same time, this network structure helps the attachment and penetration of the pesticide active ingredient on the plant surface, thereby improving the utilization rate and efficacy of the pesticide. The network structure formed by the organic thickener in the water dispersion system enables the pesticide composition to have better spreadability on the plant surface, so that the agent can be more fully contacted with the crop, thereby improving the effect of the pesticide. The organic thickener cooperates with other components such as composite surfactants, alkyl glycosides, and organosilicon emulsions, and utilizes the synergistic effect between them, which can be well conducted in the plant body, thereby improving the utilization rate of the pesticide composition and the efficacy of the unit pesticide active ingredient. This synergistic effect enables the pesticide composition to have higher selectivity and lower toxicity, and has less impact on non-target organisms. In summary, the organic thickener plays a multi-faceted role in the pesticide composition of the present application, such as improving viscosity and stability, enhancing spreadability, improving biodegradability, and exerting a synergistic effect, thereby comprehensively improving the comprehensive performance of the pesticide composition.

[0101] 4) The performance comparison analysis of the pesticide composition containing refined glufosinate and fluazifop-butyl prepared in combination with Example 3 and Comparative Examples 6-7 shows that the composite synergist is prepared by mixing alkyl glycoside and silicone emulsion in a mass ratio of 2:3, and its role in the present application is to improve the utilization efficiency of the pesticide composition and the efficacy of the unit pesticide active ingredient. Alkyl glycoside is a surfactant with good biodegradability, which can reduce the surface tension of the product, enable the agent to be fully spread on the crop, make the contact area between the agent and the crop larger, enhance the residence time of the liquid on the plant surface, reduce the loss of active ingredients, and make the efficacy more significant. At the same time, alkyl glycoside can also improve the effect and biodegradability of pesticides. XL-50 and XL-90 in the silicone emulsion are isomeric alcohol ether products of BASF, and the specific ratio of the two is compounded and used in the silicone emulsion, so that the silicone emulsion has a microemulsion effect and good stability. Hydroxyl silicone oil and amino polyether block silicone oil are compounded, and the pH value is adjusted with acetic acid, and water is slowly added to form a good water-in-oil type silicone microemulsion. This microemulsion has a good spreading effect in the formulation of the pesticide composition containing glufosinate and fluazifop-butyl, and significantly improves the efficacy. Alkyl glycosides and silicone emulsions are compounded in a specific ratio. By utilizing the synergistic effect between them, they can be well conducted in the plant body, improve the utilization rate of the pesticide composition and the efficacy of the unit pesticide active ingredient. This synergistic effect is mainly reflected in the following aspects: Alkyl glycosides can reduce the surface tension of the product, so that the agent can be fully spread on the crop, so that the contact area between the agent and the crop is larger, and the residence time of the liquid on the plant surface can be enhanced, the loss of active ingredients is reduced, and the efficacy is more significant. The silicone emulsion can provide good spreading and stability, so that the pesticide composition forms a uniform film on the surface of the plant, which is conducive to the absorption and conduction of the agent. There are interactions between alkyl glycoside and silicone emulsion, such as hydrogen bonds and van der Waals forces, which help improve the stability and adhesion of the pesticide composition, thereby improving the utilization rate and efficacy of the pesticide. The molecular structures of alkyl glycoside and silicone emulsion are complementary. The hydrophilic groups in the alkyl glycoside molecules can interact with the hydrophobic groups in the silicone emulsion to form a stable complex, which is beneficial to the stability and conduction of the pesticide composition.

[0102] 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 methods of the present application 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 protection scope of the present application.

Claims

1. A pesticide composition containing glufosinate-ammonium and fluazifop-butyl, characterized in that: The preparation method comprises the following raw materials by weight: 25-30 parts of active ingredient, 5-6 parts of composite surfactant, 1-2 parts of glycerol, 2-3 parts of organic thickener, 0.2-0.3 parts of defoamer, 4-5 parts of composite synergist, 1-1.3 parts of dispersant, 0.3-0.5 parts of preservative, and 160-170 parts of water, wherein the active ingredient is prepared by mixing refined glufosinate ammonium and fluazifop-butyl in a weight ratio of 5:1; the composite synergist is prepared by mixing alkyl glycoside and silicone emulsion in a weight ratio of 2:3; The preparation method of the silicone emulsion is as follows: according to the mass fractions, 23 parts of hydroxy silicone oil and 18 parts of amino polyether block silicone oil are mixed, stirred for 20 minutes, and then 4 parts of XL-50 and 3 parts of XL-90 are added, the temperature is raised to 47°C, and the mixture is fully stirred for 8 minutes, and then 1 part of acetic acid is added, and after stirring for 15 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 a silicone defoamer is added, and the mixture is stirred for 5 minutes to obtain the silicone emulsion; The composite surfactant is composed of the following raw materials by weight: 10 parts of lauramide propyl hydroxysulfobetaine, 8 parts of sodium polyoxyethylene fatty alcohol ether sulfate, 12 parts of coconut acid diethanolamide, 25 parts of methylpentyl alcohol polyoxyethylene ether, 10 parts of trihydroxyethylamine, and 10 parts of deionized water; The preparation method of the organic thickener comprises the following steps: S61. Dissolve 5 parts of N-isopropylacrylamide and 14 parts of acrylamide in 10 parts of water according to their mass fractions, adjust the pH to 9, and obtain a polymerization monomer solution for later use; mix 6 parts of sorbitan oleate and 18 parts of petroleum ether to obtain a dispersion for later use; S62, mixing the polymerization monomer solution and the dispersion according to the mass fractions, and then homogenizing them, the homogenization speed is 3500 rpm, the processing time is 15 minutes, and a polymerization reaction liquid is obtained; 0.003 parts of ammonium persulfate are added to the polymerization reaction liquid, and the polymerization reaction is carried out at 55° C. under anaerobic conditions for 5 hours to obtain a polymer emulsion, which is reserved; S63. Dissolve 1.6 parts of dicyclohexylmethane-4,4'-diisocyanate and 6.4 parts of polyethylene glycol in 9 parts of petroleum ether according to their mass fractions to obtain a prepolymerization solution; after mixing the prepolymerization solution and the polymer emulsion, add 0.005 parts of dibutyltin dilaurate and 0.6 parts of diethylene glycol, raise the temperature and carry out polymerization reaction at 50°C under anaerobic conditions for 4 hours, filter the reaction product to obtain a filter cake, wash with petroleum ether, and dry to obtain an organic thickener; The dispersant is arylphenol polyoxyethylene succinate sulfonate.

2. A pesticide composition containing glufosinate-ammonium and fluazifop-butyl according to claim 1, characterized in that: The preparation method of the composite surfactant comprises the following steps: S31, according to the mass parts, the fatty alcohol polyoxyethylene ether sodium sulfate and trihydroxyethylamine are mixed, stirred evenly, and then coconut acid diethanolamide is added and stirred evenly to obtain a mixed solution; S32. Add lauramide propyl hydroxysulfobetaine, methylpentyl alcohol polyoxyethylene ether and deionized water to the mixed solution according to their mass fractions, stir and heat to 40°C, stir for 60 minutes, and cool to room temperature to obtain a composite surfactant.

3. A pesticide composition containing glufosinate-ammonium and fluazifop-butyl according to claim 1, characterized in that: The preparation method of the methylvalernoyl alcohol polyoxyethylene ether is as follows: according to the mass fraction, under the protection of nitrogen, 98 parts of methylvalernoyl alcohol are slowly heated to 120° C., dehydrated and cooled by 30° C., 2 parts of sodium hydroxide are added, the temperature is again raised to 120° C., 484 parts of ethylene oxide are added, the reaction is carried out at 120° C. and 0.01 MPa for 2 hours, the temperature is lowered and the material is discharged, and the methylvalernoyl alcohol polyoxyethylene ether is obtained.

4. The pesticide composition containing glufosinate-ammonium and fluazifop-butyl according to claim 1, characterized in that: The preservative is sodium benzoate; the defoaming agent is an organosilicon defoaming agent.

5. A method for preparing a pesticide composition containing glufosinate-ammonium and fluazifop-butyl according to any one of claims 1 to 4, comprising the following steps: S91. Mix the active ingredient, glycerol, composite synergist, composite surfactant and water according to their weight proportions, and stir for 15-20 minutes to obtain solution A; S92. Mix an organic thickener, a defoamer, a dispersant and a preservative according to their weight proportions, add solution A, mix and stir for 8-10 minutes to obtain a pesticide composition containing glufosinate-ammonium and fluazifop-butyl.

6. The method for preparing a pesticide composition containing glufosinate-ammonium and fluazifop-butyl according to claim 5, characterized in that: In step S91, the stirring speed is 200-300 r / min, and in step S92, the stirring speed is 150-200 r / min.

Images