Composition containing emamectin benzoate and chlorfenapyr and application thereof

By adding specific wetting and dispersants to the pesticide composition, the prevention and treatment effect of American white moth and diamondback moth is improved, and the problems of insufficient synergistic efficiency and environmental pollution in the prior art are solved, and efficient, low-cost and safe pesticide applications are achieved.

CN119699342APending Publication Date: 2025-03-28AIGEFU CROP TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411797002.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-09
Publication Date
2025-03-28

AI Technical Summary

Technical Problem

In the prevention and control of American white moth and rhododendron, the combined agents have insufficient synergistic efficiency, poor control effect, high cost, and potential harm to crops and the environment.

Method used

A composition containing methylvitamin and nitrile is used to form a dense interface mask by adding adipicyl-α,ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2 hydroxypropane)propylene diacetate as a wetting dispersant, thereby forming a dense interface mask, improving the wetting ability and deposition of the active ingredients, reducing agent loss and reducing environmental pollution.

Benefits of technology

It significantly improves the wetting ability and deposition amount of pesticide composition on target plants, enhances the prevention and treatment effect of American white moth and diamondback moth, reduces the environmental pollution of pesticides, and is low in cost, safe and reliable.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a composition containing emamectin benzoate and chlorfenapyr. The pesticide composition comprises the following components: chlorfenapyr, emamectin benzoate, a wetting dispersant, a thickening agent, an anti-freezing agent, a preservative, a pH regulator, a defoaming agent, an antioxidant and water. The wetting dispersant is a mixture of hexanediyl-alpha, omega-bis (dimethyldodecyl) ammonium bromide and N, N-bis (3-chloro-2-hydroxypropane) propylene diamine sodium diacetate, and the wetting dispersant can be well adsorbed on a water-oil interface to form a compact interfacial film, so that the surface tension of a pesticide liquid is effectively reduced, the contact angle between the pesticide liquid and a target is reduced, and the stability of the target is improved. The wetting capacity and deposition amount of active ingredients on target plants are effectively improved, pesticide loss is reduced, and the prevention and treatment effect of pesticide liquid is improved. The pesticide composition prepared by the invention can be used for efficiently preventing and treating American white moth of poplar and plutella xylostella of cabbage, and is high in suspension rate and small in environmental pollution.
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Description

Technical Field

[0001] The invention relates to the technical field of pesticide compositions, and in particular to a composition containing emamectin benzoate and chlorfenapyr and an application thereof. Background Art

[0002] The gypsy moth is an insect of the genus Gypsophila, family Lygustris, order Lepidoptera, and is a worldwide quarantine pest. It mainly harms broad-leaved trees and is a leaf-eating pest of trees such as poplars, willows, and elms.

[0003] The diamondback moth (Plutella xylostella), belonging to the family Plutella xylostella of the order Lepidoptera, commonly known as the little green caterpillar or the two-headed moth, is an important vegetable pest distributed worldwide.

[0004] CN113875761A discloses an insecticidal composition, which contains active ingredients Compound I and Compound II, wherein Compound II is selected from at least one of spinosad, ethyl spinosad, bromofenac, thiobencarb, sulfoxaflor, emamectin benzoate, cypermethrin, ethoxyfen, and bifenthrin. The present invention also relates to the use of the insecticidal composition for preventing or controlling pests of the families of Plutella xylostella, Cibotia, Noctuidae, Delphacidae, Aleyrodidae, Tetranychus, Thripidae, Aphididae, and Cypripedium. However, it only studies the combination of various raw materials, and does not optimize its actual application effect. Summary of the invention

[0005] In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is to provide a pesticide composition with reasonable components, significant synergistic effect, good effect in controlling the gypsy moth and the diamondback moth, low cost, safety to crops, and environmental friendliness.

[0006] In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical solutions: A composition containing emamectin benzoate and chlorfenapyr comprises the following components: chlorfenapyr, emamectin benzoate, a wetting dispersant, a thickener, an antifreeze agent, a preservative, a pH regulator, a defoamer, an antioxidant and water.

[0007] Preferably, a composition containing emamectin benzoate and chlorfenapyr comprises the following components in weight percentage: 9-10% chlorfenapyr, 0.1-0.9% emamectin benzoate, 10-40% wetting and dispersing agent, 0.1-5% thickener, 1-8% antifreeze agent, 0.1-1% preservative, 0.1-1% pH regulator, 1-5% defoaming agent, 0.1-1% antioxidant, and the balance is water.

[0008] Further preferably, the composition containing emamectin benzoate and chlorfenapyr comprises the following components in weight percentage: 5% chlorfenapyr, 2% emamectin benzoate, 35% wetting and dispersing agent, 3% thickener, 5% antifreeze agent, 0.5% preservative, 2% defoaming agent, 0.3% pH adjuster, 0.5% antioxidant, and 46.7% water.

[0009] Chlorfenapyr, a white solid, is a new type of pyrrole compound. It acts on the mitochondria of cells in insects and works through the multifunctional oxidase in insects, mainly inhibiting the conversion of adenosine diphosphate to adenosine triphosphate. Adenosine triphosphate stores the energy necessary for cells to maintain their life functions. The drug has stomach poison and contact killing effects. It has strong permeability on the leaf surface, has a certain systemic effect, and has the characteristics of a wide insecticide spectrum, high prevention effect, long-lasting effect, and safety.

[0010] Emamectin benzoate, also known as spinosad in English, is a highly effective, low-toxic, safe, and non-polluting biopesticide with stomach poison and contact killing effects. Its mechanism of action is to enhance the conductivity of chloride ions through glutamate-gated chloride ion channels, thereby stimulating the release of a large amount of GABA, causing paralysis and death of poisoned insects. It has high activity, a wide insecticide spectrum, and is not prone to drug resistance. It is widely used in the prevention and control of various pests on economic crops such as vegetables, fruit trees, and cotton.

[0011] Since the solubility of chlorfenapyr and avermectin benzoate in water is extremely low, they can only be prepared as suspensions before application. The stability of the suspension will directly affect the effect of the medication. At the same time, the use of a single agent is prone to drug resistance; arbitrary mixing is prone to antagonism. The inventors found that due to the low solid content of the active ingredient, it is easy to have problems such as stratification, water precipitation and low suspension rate. The inventors added a wetting dispersant prepared by mixing hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium in a specific mass ratio. The wetting dispersant can be well adsorbed at the water / oil phase interface to form a dense interface film, effectively reduce the surface tension of the pesticide solution, reduce the contact angle between the solution and the target, effectively improve the wetting ability and deposition amount of the active ingredient on the target plant, reduce the loss of the agent, and reduce the pollution of the pesticide to the environment. At the same time, the wetting dispersant helps to maintain the stability of the oil-water interface, can better disperse the thickener in the solution, and better regulate the fluidity and suspension stability of the solution.

[0012] Preferably, the wetting and dispersing agent is at least one of hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium.

[0013] Further preferably, the wetting and dispersing agent is hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide; the preparation method of the hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide is as follows: 45-60g of lauryldimethylamine, 20-30g of 1,6-dibromo-hexane and 100-160mL of 70-99wt% ethanol aqueous solution are mixed and heated to 70-80℃ for reflux reaction for 20-24h. After the reaction is completed, the solvent is evaporated under reduced pressure and the obtained solid is washed with ethyl acetate 2-3 times, then recrystallized with 300-500mL of ethyl acetate, and finally dried at 60-80℃ for 6-8h to obtain hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide.

[0014] Further preferably, the wetting and dispersing agent is a mixture of hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine sodium diacetate in a mass ratio of 1-2:2-3; the preparation method of the N,N-bis(3-chloro-2-hydroxypropane)propylenediamine sodium diacetate is as follows: (1) At 20-40°C, 2-4 g of 1,3-propylenediamine, 23-33 g of sodium chloroacetate and 40-60 mL of water were mixed and reacted for 20-24 h, then the temperature was raised to 50-70°C and the reaction was continued for 2-3 h. The solvent was then evaporated under reduced pressure. The obtained solid was mixed with 50-80 mL of 10-20 wt% hydrochloric acid solution and stirred for 20-30 min, filtered, and the filter cake was washed with water until the filtrate was neutral, and dried at 60-80°C for 6-8 h to obtain sodium N,N-propylenediamine diacetate; (2) Add 5-8 g of sodium N,N-propylenediamine diacetate to 20-30 mL of 1-3 wt% sodium hydroxide aqueous solution, stir to dissolve, adjust the pH of the solution to 6.5-7.5 with 3-5 wt% formic acid aqueous solution, then drop 11-17 g of epichlorohydrin into the solution at a rate of 1-2 drops / second, react for 3-5 hours after the dropwise addition is complete, and evaporate the solvent to obtain sodium N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate; (3) Mix 2-4 g of N,N-bis(3-chloro-2-hydroxypropane)propylenediamine sodium diacetate with 30-50 mL of water, stir until completely dissolved, and heat to 80-100°C. Add 4-8 g of cetylamine to the solution, react for 10-15 h, add 50-100 mL of anhydrous ethanol, stir for 10-20 min, filter, collect the residue, and dry at 60-80°C for 6-8 h to obtain N,N-bis(3-chloro-2-hydroxypropane-N-hexadecyl secondary amine)propylenediamine sodium diacetate.

[0015] Preferably, the thickener is one or a combination of two or more of xanthan gum, carrageenan, gellan gum, gum arabic, sodium carboxymethyl cellulose, magnesium aluminum silicate, and bentonite.

[0016] Preferably, the antifreeze agent is one or a mixture of two or more of glycerol, propylene glycol, ethylene glycol, sodium chloride, urea, and glycerol.

[0017] Preferably, the preservative is one or a mixture of two or more of sorbic acid, sodium benzoate, and propyl polyhydroxybenzoate.

[0018] Preferably, the defoaming agent is one or a mixture of two or more of polyoxyethylene polyoxypropanolamine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether, and polydimethylsiloxane.

[0019] Preferably, the pH adjuster is one of citric acid and glacial acetic acid.

[0020] Preferably, the antioxidant is one of tea polyphenols and tocopherol.

[0021] The present invention also discloses a method for preparing the composition containing emamectin benzoate and chlorfenapyr, comprising the following steps: S1. Weigh the raw materials according to the formula, mix chlorfenapyr, emamectin benzoate, a wetting and dispersing agent, a defoaming agent, an antifreeze agent, and water to obtain a base material; S2 sand-grinds the base material to obtain fine material; S3: mixing a thickener, a preservative, a pH adjuster, an antioxidant, and water to obtain an emulsion; S4: mixing the fine material with the emulsion to obtain the composition containing emamectin benzoate and chlorfenapyr.

[0022] Preferably, the particle size of the fine material in step S2 is 1 μm-5 μm.

[0023] The invention also discloses the application of the pesticide composition containing emamectin benzoate and chlorfenapyr in preventing and controlling cabbage diamondback moth and poplar gypsy moth.

[0024] Compared with the prior art, the present invention has the following beneficial effects: The pesticide composition prepared by the invention is a suspension agent, and the dispersion medium is environmentally friendly water, which can avoid the problems of being flammable, explosive, poisoning, etc., and will not generate dust pollution, is safe for operators and the environment, has no dust drift, has good dispersibility in water, and is prepared by adding a wetting dispersant mixed with hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium, which can be well adsorbed at the water-oil interface to form a dense interface film, effectively reduce the surface tension of the pesticide solution, reduce the contact angle between the solution and the target, effectively improve the wetting ability and deposition amount of the active ingredient on the target plant, reduce the loss of the agent, improve the prevention and control effect of the solution, reduce the pollution of the pesticide to the environment, and have a high suspension rate. DETAILED DESCRIPTION

[0025] The present invention is further described in detail with reference to the following specific embodiments. The process, conditions, experimental methods, etc. for implementing the invention, except for the contents specifically mentioned below, are all common knowledge and common common sense in the art, and the present invention has no special restrictions.

[0026] To avoid redundancy, the items used in the following examples are all commercially available products unless otherwise specified, and the methods used are all conventional methods unless otherwise specified.

[0027] Example 1 A method for preparing a composition containing emamectin benzoate and chlorfenapyr comprises the following steps: S1: 475 g of chlorfenapyr, 25 g of avermectin benzoate, 3500 g of a wetting and dispersing agent, 200 g of polyoxyethylene polyoxypropanolamine ether, 200 g of polyoxyethylene polyoxypropanolamine ether, and 2000 g of water are mixed to obtain a base material; S2: sand-grinding the base material to obtain fine material with a particle size of 1 μm-5 μm; S3: 300 g of xanthan gum, 50 g of propyl polyhydroxybenzoate, 30 g of citric acid, 50 g of tea polyphenols, and 2670 g of water are mixed to obtain an emulsion; S4: mixing the fine material with the emulsion and stirring at a rotation speed of 700 rpm for 30 minutes to obtain the composition containing emamectin benzoate and chlorfenapyr.

[0028] The wetting and dispersing agent is a mixture of hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium in a mass ratio of 2:3; The preparation method of the hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide is as follows: 50 g of lauryl dimethylamine, 22 g of 1,6-dibromo-hexane and 130 mL of 99 wt% ethanol aqueous solution were mixed and heated to 78 ° C for reflux reaction for 24 h. After the reaction, the solvent was evaporated under reduced pressure and the obtained solid was washed 3 times with ethyl acetate, then recrystallized with 350 mL of ethyl acetate and finally dried at 70 ° C for 8 h to obtain hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide.

[0029] The preparation method of the N,N-bis(3-chloro-2-hydroxypropane)propylenediaminediacetate sodium comprises the following steps: (1) At 30°C, 2.8 g of 1,3-propylenediamine was mixed with 25.6 g of sodium chloroacetate and 50 mL of water and reacted for 24 h. The mixture was then heated to 60°C and reacted for 3 h. The solvent was then evaporated under reduced pressure. The obtained solid was mixed with 60 mL of 10 wt% hydrochloric acid solution and stirred for 30 min. The solid was filtered and the filter cake was washed with water until the filtrate was neutral. The filter cake was dried at 80°C for 8 h to obtain sodium N,N-propylenediamine diacetate. (2) Add 6.8 g of sodium N,N-diamine diacetate to 30 mL of 1 wt% sodium hydroxide aqueous solution, stir to dissolve, adjust the pH of the solution to 7 with 3 wt% formic acid aqueous solution, then add 13.5 g of epichlorohydrin to the solution at a rate of 2 drops / second, react for 4 hours after the addition is complete, and evaporate the solvent to obtain sodium N,N-bis(3-chloro-2-hydroxypropane)diamine diacetate; (3) Mix 3.5 g of N,N-bis(3-chloro-2-hydroxypropane)propylenediamine sodium diacetate with 40 mL of water, stir until completely dissolved, and heat to 80-10°C. Add 7.1 g of cetylamine to the solution, react for 12 h, add 100 mL of anhydrous ethanol, stir for 20 min, filter, collect the filter residue, and dry it at 60-80°C for 8 h to obtain N,N-bis(3-chloro-2-hydroxypropane-N-hexadecyl secondary amine)propylenediamine sodium diacetate.

[0030] Example 2 A method for preparing a composition containing emamectin benzoate and chlorfenapyr comprises the following steps: S1: 475 g of chlorfenapyr, 25 g of avermectin benzoate, 3500 g of a wetting and dispersing agent, 200 g of polyoxyethylene polyoxypropanolamine ether, 200 g of polyoxyethylene polyoxypropanolamine ether, and 2000 g of water are mixed to obtain a base material; S2: sand-grinding the base material to obtain fine material with a particle size of 1 μm-5 μm; S3: 300 g of xanthan gum, 50 g of propyl polyhydroxybenzoate, 30 g of citric acid, 50 g of tea polyphenols, and 2670 g of water are mixed to obtain an emulsion; S4: mixing the fine material with the emulsion and stirring at a rotation speed of 700 rpm for 30 minutes to obtain the composition containing emamectin benzoate and chlorfenapyr.

[0031] The wetting and dispersing agent is hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide; The preparation method of the hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide is as follows: 50 g of lauryl dimethylamine, 22 g of 1,6-dibromo-hexane and 130 mL of 99 wt% ethanol aqueous solution were mixed and heated to 78 ° C for reflux reaction for 24 h. After the reaction, the solvent was evaporated under reduced pressure and the obtained solid was washed 3 times with ethyl acetate, then recrystallized with 350 mL of ethyl acetate and finally dried at 70 ° C for 8 h to obtain hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide.

[0032] Example 3 A method for preparing a composition containing emamectin benzoate and chlorfenapyr comprises the following steps: S1: 475 g of chlorfenapyr, 25 g of avermectin benzoate, 3500 g of a wetting and dispersing agent, 200 g of polyoxyethylene polyoxypropanolamine ether, 200 g of polyoxyethylene polyoxypropanolamine ether, and 2000 g of water are mixed to obtain a base material; S2: sand-grinding the base material to obtain fine material with a particle size of 1 μm-5 μm; S3: 300 g of xanthan gum, 50 g of propyl polyhydroxybenzoate, 30 g of citric acid, 50 g of tea polyphenols, and 2670 g of water are mixed to obtain an emulsion; S4: mixing the fine material with the emulsion and stirring at a rotation speed of 700 rpm for 30 minutes to obtain the composition containing emamectin benzoate and chlorfenapyr.

[0033] The wetting and dispersing agent is sodium N,N-bis(3-chloro-2-hydroxypropane)propylenediaminediacetate; The preparation method of the N,N-bis(3-chloro-2-hydroxypropane)propylenediaminediacetate sodium comprises the following steps: (1) At 30°C, 2.8 g of 1,3-propylenediamine was mixed with 25.6 g of sodium chloroacetate and 50 mL of water and reacted for 24 h. The mixture was then heated to 60°C and reacted for 3 h. The solvent was then evaporated under reduced pressure. The obtained solid was mixed with 60 mL of 10 wt% hydrochloric acid solution and stirred for 30 min. The mixture was filtered and the filter cake was washed with water until the filtrate was neutral. The filter cake was dried at 80°C for 8 h to obtain sodium N,N-propylenediamine diacetate. (2) Add 6.8 g of sodium N,N-diamine diacetate to 30 mL of 1 wt% sodium hydroxide aqueous solution, stir to dissolve, adjust the pH of the solution to 7 with 3 wt% formic acid aqueous solution, then add 13.5 g of epichlorohydrin to the solution at a rate of 2 drops / second, react for 4 hours after the addition is complete, and evaporate the solvent to obtain sodium N,N-bis(3-chloro-2-hydroxypropane)diamine diacetate; (3) Mix 3.5 g of N,N-bis(3-chloro-2-hydroxypropane)propylenediamine sodium diacetate with 40 mL of water, stir until completely dissolved, and heat to 80-10°C. Add 7.1 g of cetylamine to the solution, react for 12 h, add 100 mL of anhydrous ethanol, stir for 20 min, filter, collect the filter residue, and dry it at 60-80°C for 8 h to obtain N,N-bis(3-chloro-2-hydroxypropane-N-hexadecyl secondary amine)propylenediamine sodium diacetate.

[0034] Comparative Example 1 A method for preparing a composition containing emamectin benzoate and chlorfenapyr comprises the following steps: S1: 475 g of chlorfenapyr, 25 g of avermectin benzoate, 3500 g of a wetting and dispersing agent, 200 g of polyoxyethylene polyoxypropanolamine ether, 200 g of polyoxyethylene polyoxypropanolamine ether, and 2000 g of water are mixed to obtain a base material; S2: sand-grinding the base material to obtain fine material with a particle size of 1 μm-5 μm; S3: 300 g of xanthan gum, 50 g of propyl polyhydroxybenzoate, 30 g of citric acid, 50 g of tea polyphenols, and 2670 g of water are mixed to obtain an emulsion; S4: mixing the fine material with the emulsion and stirring at a rotation speed of 700 rpm for 30 minutes to obtain the composition containing emamectin benzoate and chlorfenapyr.

[0035] The wetting and dispersing agent is commercially available sodium lignin sulfonate.

[0036] Test Example 1 Suspension rate determination: With reference to GB / T14825-2006 "Determination of Suspension Rate of Pesticides", the pesticide compositions obtained in Examples 1-3 and Comparative Example 1 were stored at room temperature for 14 days and at 54°C for 14 days, respectively. The suspension rates of the samples after room temperature storage and high temperature storage were measured, and each sample was tested 3 times, and the test results were averaged.

[0037] Determination of water separation rate: The water separation rate is the percentage of the water layer precipitated from the suspension product after storage. The determination method is to store 100 mL of the product in a graduated storage container and then directly read the volume of the precipitated water portion after the storage time is up.

[0038] The test results are shown in Table 1: Table 1: Suspension rate and water separation rate test results of pesticide compositions

[0039] Generally, the suspension rate of a suspending agent is qualified if it is greater than 90%, and the water separation rate is qualified if it is less than 5%. It can be seen from the experimental data in Table 1 that the suspension rate and water separation rate of the pesticide composition prepared by the present invention are both within the qualified range. In addition, the suspension effect of the pesticide composition prepared in Example 1 is significantly better than that of other embodiments and comparative examples. The possible reason is that a wetting and dispersing agent mixed with hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium is added. The wetting and dispersing agent can be well adsorbed at the water / oil phase interface to form a dense interface film, effectively reduce the surface tension of the pesticide solution, help to maintain the stability of the oil-water interface, enable the thickener to be better dispersed in the solution, and better adjust the fluidity and suspension stability of the solution.

[0040] Test Example 2 Contact angle measurement: The test object is the pesticide composition obtained in Examples 1-3 and Comparative Example 1. The test method is to place a glass slide carrying cowpea leaves horizontally on the stage of the SL200KB contact angle measuring instrument at 25°C, and use a micro-syringe to add 1.5 μL of deionized water and a 200-fold dilution of the pesticide composition to the front of the leaf, respectively. The contact angle formed when the droplet contacts the leaf surface is photographed by a CCD camera, and the contact angle is calculated by a fitting analysis method. The test results are shown in Table 2: Table 2: Contact angle measurement results of pesticide compositions

[0041] The smaller the contact angle, the better the adhesion between the pesticide solution and the target. From the experimental data in Table 2, it can be seen that the contact angle of the pesticide composition obtained in Example 1 is the smallest. The possible reason is that the wetting and dispersing agent mixed with a specific mass ratio of hexanediyl-α, ω-bis(dimethyldodecyl) ammonium bromide and N, N-bis(3-chloro-2-hydroxypropane) propylenediamine diacetate sodium is well adsorbed at the water / oil phase interface to form a dense interface film, which effectively reduces the surface tension of the pesticide solution and the contact angle between the solution and the target, and can effectively improve the wetting ability and deposition amount of the active ingredient on the target plant.

[0042] Test Example 3 Field efficacy test: (1) Test method The tested cabbage variety was Zhonggan No. 15. The pesticide composition prepared in each embodiment and control example was diluted 1000 times, and clean water was used as a blank control (CK). Each plot had an area of ​​6.67 m 2 , repeated 3 times. Set up isolated rows in each plot and arrange them in random blocks. Apply pesticides once during the period of occurrence of cabbage moth. Use a 2.5L small sprayer to apply pesticides. Spray evenly until the droplets just flow down.

[0043] (2) Survey methods The number of diamondback moths in 10 cabbages was counted in each plot, which were the number of diamondback moths one day before the drug application and the number of diamondback moths one day after the drug application. The insect population reduction rate and control effect were calculated according to the following formula. The Duncan's new multiple range method in SPSS22.0 software was used to perform variance analysis on the control effect among the treatments.

[0044] Pest reduction rate (%) = [(Pest number before application - Pest number after application) ÷ Pest number before application] × 100 Control effect (%) = (insecticidal reduction rate in treated area - insecticidal reduction rate in control area) ÷ (1 - insecticidal reduction rate in control area) × 100 Table 3: Field efficacy test results

[0045] (Note: Each group of comparative example 1 has significant differences from each example) It can be seen from the experimental data in Table 3 that the pesticide composition obtained in Example 1 of the present invention has the best field efficacy, indicating that it has the strongest toxicity to the diamondback moth. The possible reason is that the wetting and dispersing agent can be well adsorbed at the water / oil phase interface to form a dense interface film, which effectively reduces the surface tension of the pesticide solution, reduces the contact angle between the solution and the target, effectively improves the wetting ability and deposition amount of the active ingredient on the target plant, reduces the loss of the agent, and still has a good control effect after 7 days. At the same time, by comparing the experimental results of Example 1 with Comparative Examples 2 and 3, it can be seen that chlorfenapyr and avermectin benzoate have a good synergistic effect, which is more conducive to the control of the cabbage diamondback moth.

Claims

1. A composition containing emamectin benzoate and chlorfenapyr, characterized in that: The invention comprises the following components in weight percentage: 9-10% of chlorfenapyr, 0.1-0.9% of emamectin benzoate, 10-40% of a wetting and dispersing agent, 0.1-5% of a thickener, 1-8% of an antifreeze agent, 0.1-1% of a preservative, 0.1-1% of a pH regulator, 1-5% of a defoaming agent, and the balance is water; The wetting and dispersing agent is at least one of hexanediyl-α, ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium.

2. The pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in claim 1, characterized in that: The wetting and dispersing agent is hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide.

3. The pesticide composition according to claim 2, characterized in that The preparation method of the hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide is as follows: 45-60g of lauryldimethylamine, 20-30g of 1,6-dibromo-hexane and 100-160mL of 70-99wt% ethanol aqueous solution are mixed, heated to 70-80°C for reflux reaction for 20-24h, and after the reaction is completed, the solvent is evaporated under reduced pressure to obtain a solid, which is washed with ethyl acetate for 2-3 times, then recrystallized with 300-500mL of ethyl acetate, and finally dried at 60-80°C for 6-8h to obtain hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide.

4. The pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in claim 1, characterized in that: The wetting and dispersing agent is a mixture of hexanediyl-α,ω-bis(dimethyldodecyl)ammonium bromide and N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate sodium in a mass ratio of 1-2:2-3.

5. The pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in claim 4, characterized in that: The preparation method of the N,N-bis(3-chloro-2-hydroxypropane)propylenediaminediacetate sodium is as follows: (1) At 20-40°C, 2-4 g of 1,3-propylenediamine, 23-33 g of sodium chloroacetate and 40-60 mL of water were mixed and reacted for 20-24 h, then the temperature was raised to 50-70°C and the reaction was continued for 2-3 h. The solvent was then evaporated under reduced pressure. The obtained solid was mixed with 50-80 mL of 10-20 wt% hydrochloric acid solution and stirred for 20-30 min, filtered, and the filter cake was washed with water until the filtrate was neutral, and dried at 60-80°C for 6-8 h to obtain sodium N,N-propylenediamine diacetate; (2) Add 5-8 g of sodium N,N-propylenediamine diacetate to 20-30 mL of 1-3 wt% sodium hydroxide aqueous solution, stir to dissolve, adjust the pH of the solution to 6.5-7.5 with 3-5 wt% formic acid aqueous solution, then drop 11-17 g of epichlorohydrin into the solution at a rate of 1-2 drops / second, react for 3-5 hours after the dropwise addition is complete, and evaporate the solvent to obtain sodium N,N-bis(3-chloro-2-hydroxypropane)propylenediamine diacetate; (3) Mix 2-4 g of N,N-bis(3-chloro-2-hydroxypropane)propylenediamine sodium diacetate with 30-50 mL of water, stir until completely dissolved, and heat to 80-100°C. Add 4-8 g of cetylamine to the solution, react for 10-15 h, add 50-100 mL of anhydrous ethanol, stir for 10-20 min, filter, collect the residue, and dry at 60-80°C for 6-8 h to obtain N,N-bis(3-chloro-2-hydroxypropane-N-hexadecyl secondary amine)propylenediamine sodium diacetate.

6. The pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in claim 1, characterized in that: The thickener is one or a combination of two or more of xanthan gum, carrageenan, gellan gum, gum arabic, sodium carboxymethyl cellulose, magnesium aluminum silicate, and bentonite.

7. The pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in claim 1, characterized in that: The antifreeze agent is one or a mixture of two or more of glycerol, propylene glycol, ethylene glycol, sodium chloride, urea and glycerol.

8. A method for preparing a pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in any one of claims 1 to 7, characterized in that: The steps include: S1. Weigh the raw materials according to the formula, mix chlorfenapyr, emamectin benzoate, a wetting and dispersing agent, a defoaming agent, an antifreeze agent, and water to obtain a base material; S2 sand-grinds the base material to obtain fine material; S3: mixing a thickener, a preservative, a pH adjuster, an antioxidant, and water to obtain an emulsion; S4: mixing the fine material with the emulsion to obtain the composition containing emamectin benzoate and chlorfenapyr.

9. The method for preparing the pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in claim 8, characterized in that: The particle size of the fine material in step S2 is 1 μm-5 μm.

10. Use of the pesticide composition containing emamectin benzoate and chlorfenapyr as claimed in any one of claims 1 to 7 for controlling Plutella xylostella and Hyphantria cunea.

Citation Information

Patent Citations

  • Insecticidal composition

    CN113875761A