WO2020103646A1 - Method for preparing micro-capsule suspension-suspension agent containing lambda-cyhalothrin and lufenuron and micro-capsule suspension-suspension agent thereof - Google Patents

Abstract

The present disclosure relates to a method for preparing a micro-capsule suspension-suspension agent containing lambda-cyhalothrin and lufenuron and the micro-capsule suspension-suspension agent thereof, the method comprising: a. mixing amino resin prepolymer aqueous solution and lambda-cyhalothrin emulsifiable concentrate according to a weight ratio of (1-5):1 to obtain a first material; b. mixing the first material and buffer solution to obtain a second material having a pH value of 4-7; c. mixing the second material and an acid solution to obtain a third material having a pH value of 3-4; d. stirring the third material at 40-70°C for 2-5 hours to obtain a fourth material; and e. mixing the fourth material, a lufenuron suspension agent and an emulsifying and dispersing agent according to a weight ratio of 1:(0.1-1):(0.01-2). The micro-capsule suspension-suspension agent containing lambda-cyhalothrin and lufenuron that is prepared by using the method according to the present disclosure has good storage stability, may prevent injurious insects in crops effectively over the long term, reduces the frequency of pesticide use and the amount of pesticide use, saves costs, and reduces environmental pollution.

Description

Method for preparing microcapsule suspension-suspending agent containing high-efficiency cyhalothrin and lufenuron and microcapsule suspension-suspending agent

cross reference

The present invention requires that the application number is 201811378078.1, and the invention title is "a method for preparing microcapsule suspension-suspending agent containing lambda cyhalothrin and lufenuron and its microcapsule suspension-suspending agent. "Chinese patent application priority, the entire content of the application is incorporated by reference in the present invention.

Technical field

The present disclosure relates to the field of pesticides, and in particular, to a method for preparing a microcapsule suspension-suspending agent containing lambda-cyhalothrin and lufenuron and a microcapsule suspension-suspending agent.

Background technique

Lambda-cyhalothrin is a broad-spectrum insecticide. It can inhibit the conduction of insect axons and has the effects of avoiding, knocking down and poisoning insects. It can also be used with most fungicides and insecticides. And herbicides have good control effect. In traditional pesticide formulations, the active ingredients are easy to fail under the influence of the external environment, such as sunshine, soil pH, etc., and the shelf life is short, thereby reducing the prevention effect of pesticides. Existing formulations containing lambda-cyhalothrin on the market contain a large amount of organic solvents, which pollute the environment. In addition, the high-efficiency cyfluthrin single agent has certain limitations. Its compounding with chlorfenapyr can not only effectively improve the actual control effect, reduce the dosage, reduce the cost, delay the emergence of drug resistance, but also extend the pesticide varieties. Service life, reduce pollution to the environment.

The microcapsule suspension agent uses natural or synthetic polymer materials to form a core-shell structure tiny container, which can coat pesticides and suspend in water. It is a long-lasting period, less organic solvent, and less harmful to the operator New pesticide formulations. The high-efficiency cyhalothrin microcapsule suspension agent obtained by the traditional preparation method is prone to agglomeration and solidification, which makes it difficult to store, and has a poor effect on crop pest control, and it is difficult to meet the preparation requirements of pesticide pest control.

Summary of the invention

The purpose of the present disclosure is to provide a method for preparing a microcapsule suspension-suspension of high-efficiency cyfluthrin and lufenuron which is easy to store and has high efficacy, and a high-efficiency cyfluthrin and lufenuron prepared by the method Microcapsule suspension-suspending agent.

In order to achieve the above object, the first aspect of the present disclosure: to provide a method for preparing a high-efficiency cyhalothrin and fenprofen microcapsule suspension-suspending agent, the method includes the following steps: a. The amino resin prepolymer aqueous solution and The high-efficiency cyhalothrin emulsifiable concentrate is mixed in a weight ratio of (1-5): 1 to obtain a first material; b. The first material obtained in step a is mixed with a buffer solution to obtain a second material. The pH value of the second material is 4-7; c. The second material obtained in step b is mixed with an acidic solution to obtain a third material. The pH value of the third material is 3-4; d. The third material obtained in step c is treated for 2-5 hours under the condition of a temperature of 40-70 ° C to obtain a fourth material; e. The fourth material obtained in step d and the mitoxamide suspension agent It is mixed with the emulsifying and dispersing agent in a weight ratio of 1: (0.1-1): (0.01-2) to obtain a microcapsule suspension-suspending agent containing lambda-cyhalothrin and lufenuron.

Preferably, the aqueous solution of the amino resin prepolymer in step a is obtained by prepolymerizing an amino-containing compound, formaldehyde and water; the molar ratio of the amino-containing compound to formaldehyde is (0.1-2): 1 , The weight ratio of water to formaldehyde is (2-6): 1; the amino-containing compound includes one or more of urea, melamine and benzomelamine; the conditions of the pre-polymerization include: pH 8-10, temperature 60-80 ° C, time 0.5-3 hours.

Preferably, the lambda cyhalothrin emulsifiable concentrate in step a contains lambda cyhalothrin, an organic solvent and an emulsifier; the organic solvent includes petroleum ether, ethyl acetate, methyl oleate, xylene and One or more of mineral spirits, the emulsifier includes sodium lignosulfonate, sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, styrene-maleic anhydride copolymer, fatty alcohol polyoxygen One of vinyl ether, sorbitan polyoxyethylene polyoxypropylene ether, sorbitan monostearate polyoxyethylene ether, sodium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate One or more; the weight ratio of the lambda-cyhalothrin, the organic solvent and the emulsifier is 1: (0.1-5): (0.01-0.2).

Preferably, the buffer solution in step b contains a buffer pair including one or more of citric acid-sodium citrate, citric acid-disodium hydrogen phosphate and acetic acid-sodium acetate.

Preferably, the acidic solution in step c includes one or more of hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid and ammonium chloride.

Preferably, the mixing in step a is performed under stirring conditions, and the stirring speed is 1500-3000 rpm; the mixing in step b is performed under stirring conditions, and the stirring speed is 1000-1200 rpm; the mixing in step c is performed under stirring conditions, and the stirring speed is 1200-1500 rpm.

Preferably, in step e, the fourth material is mixed with the first dispersant, thickener and antifreeze, and then mixed with the emulsified dispersant; the first dispersant includes dodecylbenzenesulfonate Sodium, methylene bisnaphthalene sulfonate, sodium 1-methylnaphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, desugared sodium lignosulfonate, desugared condensation One or more of sodium lignin sulfonate, sodium succinate sulfonate, split powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether; the thickener includes aluminum magnesium silicate , Xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon one or more; the antifreeze includes ethylene glycol, 1,2-propanediol, propylene trioxide One or more of alcohol and urea; the weight ratio of the fourth material to the first dispersant, the thickener and the antifreeze is 1: (0.01-0.2): (0.001-0.02) : (0.02-0.15).

Preferably, in step e, the fourth material is mixed with the lufenuron suspension agent and the emulsifying and dispersing agent in a weight ratio of 1: (0.2-0.5): (0.02-0.05).

Preferably, the lufenuron suspension in step e is obtained by mixing lufenuron with a second dispersant and water, and the weight ratio of the lufenuron to the second dispersant and water is 1: (0.2-0.5): (1.5-3), the second dispersant includes sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate, benzyl Naphthalenesulfonic acid formaldehyde condensate, sodium lignosulfonate, desugared lignosulfonate sodium, desugared condensed sodium lignosulfonate, sodium succinate sulfonate, split powder, nonylphenol polyoxyethylene ether And one or more of fatty alcohol polyoxyethylene ether, the emulsifying and dispersing agent includes sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate , Benzyl naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, desugared lignin sulfonate, desugared condensed sodium lignin sulfonate, sodium succinate sulfonate, opened powder, nonylphenol polyoxygen One or more of vinyl ether and fatty alcohol polyoxyethylene ether.

The second aspect of the present disclosure: providing a high-efficiency cyhalothrin and microcarbosulfan microcapsule suspension-suspending agent prepared by the method of the first aspect of the present disclosure.

Through the above technical solutions, the present invention adjusts the specific pH value in multiple steps, and the prepared microcapsule suspension-suspending agent providing cyfluthrin and lufenuron has good storage stability and is not prone to agglomeration and solidification. It can slow-release and long-term control of crop pests, reduce the number and amount of medicines used, save costs and reduce environmental pollution.

Other features and advantages of the present disclosure will be described in detail in the detailed description section that follows.

detailed description

The specific embodiments of the present disclosure will be described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present disclosure, and are not intended to limit the present disclosure.

The first aspect of the present disclosure: to provide a method for preparing a microcapsule suspension-suspending agent containing high-efficiency cyhalothrin and lufenuron. The method includes the following steps: a. An amino resin prepolymer aqueous solution and high-efficiency chlorofluorocarbon Cypermethrin emulsifiable concentrate is mixed in a weight ratio of (1-5): 1 to obtain a first material; b. Mix the first material obtained in step a with a buffer solution to obtain a second material, the second material The pH value is 4-7; c, the second material obtained in step b is mixed with an acidic solution to obtain a third material, the pH value of the third material is 3-4; d, the temperature is 40 Treating the third material obtained in step c for 2-6 hours at -70 ° C to obtain a fourth material; e. Dispersing the fourth material obtained in step d with fenprofen and emulsifying and dispersing The agent is mixed in a weight ratio of 1: (0.1-1): (0.01-2) to obtain a microcapsule suspension-suspension agent containing lambda-cyhalothrin and lufenuron.

In the present disclosure, lambda-cyhalothrin is the compound [1α (S *), 3α (Z)]-(RS) -3- (2-chloro-3,3,3-trifluoro-1-propenyl) The trade name of -2,2-dimethylcyclopropanecarboxylic acid-cyano- (3-phenoxyphenyl) methyl ester, the English name is λ-Cyhalothrin, and the molecular formula is C ₂₃ H ₁₉ ClF ₃ NO ₃ , The relative molecular weight is 449.9, the CAS number is 91465-08-6, and the structural formulas are shown in formula (1) and formula (2).

In the present disclosure, lufenuron is compound RS) -1- [2,5-dichloro-4- (1,1,2,3,3,3-hexafluoropropoxy) phenyl] -3- ( The trade name of 2,6-difluorobenzoyl) urea, English name is Lufenuron, molecular formula is C ₁₇ H ₈ Cl ₂ F ₈ N ₂ O ₃ , relative molecular weight is 511.2, CAS number is 103055-07-8, structural formula As shown in formula (3).

According to the first aspect of the present disclosure, the preparation method of the aqueous solution of the amino resin prepolymer in step a may be a preparation method well known to those skilled in the art, and the disclosure does not particularly limit it. Preferably, the aqueous solution of the amino resin prepolymer may be obtained by prepolymerizing an amino group-containing compound, formaldehyde and water, and the molar ratio of the amino group-containing compound to formaldehyde may be (0.1-2): 1, The mass ratio of water to formaldehyde may be (2-6): 1. The amino group-containing compound may include one or more of urea, melamine, and benzomelamine. The pre-polymerization conditions may include: a pH of 8-10, a temperature of 60-80 ° C, and a time of 0.5- 3 hours.

According to the first aspect of the present disclosure, the preparation method of the lambda cyhalothrin emulsifiable concentrate in step a may be a preparation method well-known to those skilled in the art, and the disclosure does not particularly limit it. Preferably, the lambda cyhalothrin emulsifiable concentrate may contain lambda cyhalothrin, an organic solvent and an emulsifier, and the lambda cyhalothrin, organic solvent and emulsifier can be mixed to obtain the lambda cyhalothrin Cypermethrin emulsifiable concentrate. Wherein, the organic solvent may be various substances capable of dissolving and diluting lambda cyhalothrin, preferably, the organic solvent may include petroleum ether, ethyl acetate, methyl oleate, xylene and solvent oil One or more. The emulsifier may be various substances having an emulsifying effect. Preferably, the emulsifier may include sodium lignosulfonate, sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, styrene-maleic Anhydride copolymer, fatty alcohol polyoxyethylene ether, sorbitan polyoxyethylene polyoxypropylene ether, sorbitan monostearate polyoxyethylene ether, sodium lauryl sulfate, polyvinyl alcohol, polycarboxylate And one or more of naphthalene sulfonate. In order to further improve the particle size distribution and coating rate of the microcapsules in the microcapsule suspension agent, thereby further improving the storage stability of the microcapsule suspension agent, preferably, the high-efficiency cyhalothrin, organic solvent and emulsifier The weight ratio may be 1: (0.1-5): (0.01-0.2), the organic solvent content of the ratio is appropriate, and the pollution to the environment can be reduced.

According to the first aspect of the present disclosure, in order to improve the coating rate, uniformity and capsule tightness of the microcapsules, thereby further improving the storage stability of the high-efficiency cyhalothrin and fenprofen microcapsule suspension-suspending agent, It is not easy to cause agglomeration and solidification, and has a good crop pest control effect. After the first material is obtained, the pH can be adjusted by using a buffer solution and an acid solution, respectively. For example, in one embodiment, the first material may be mixed with a buffer solution to obtain a second material with a pH of 4-7; then the second material may be mixed with an acidic solution to obtain a pH of 3 -4 The third material.

According to the first aspect of the present disclosure, the meaning of the buffer solution in step b is well known to those skilled in the art, and is a solution containing a buffer pair. Preferably, the buffer pair may include one or more of citric acid-sodium citrate, citric acid-sodium hydrogen phosphate and acetic acid-sodium acetate. In order to adjust the pH of the second material to 5-7, the pH of the buffer solution may be 3-5.5. The total concentration of the buffer pair in the buffer solution may be 1-5% by weight.

According to the first aspect of the present disclosure, the acidic solution in step c may be an acidic substance conventional in the art. Preferably, the acidic solution may include one or more of hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid, and ammonium chloride. The concentration of acid in the acidic solution may be 0.5-8% by weight.

According to the first aspect of the present invention, appropriate reaction conditions can increase the coverage of the microcapsules, improve the particle size distribution and the thickness of the capsule shell, and thereby improve the storage stability of the microcapsule suspension agent. Preferably, the mixing in step a may be performed under stirring conditions, and the stirring speed may be 1500-3000 rpm. The mixing in step b may be performed under stirring conditions, and the stirring speed may be 1000-1200 rpm. The mixing in step c may also be performed under stirring conditions, and the stirring speed may be 1200-1500 rpm.

According to the first aspect of the present disclosure, those skilled in the art should know that when an insecticide is acidic or alkaline, it not only hinders the growth of plants, but also causes environmental pollution. Therefore, before mixing the fourth material with the lufenuron suspension agent and the emulsifying and dispersing agent, the acidity and alkalinity of the fourth material is preferably neutral. Therefore, the method of the first aspect of the present disclosure further includes the step of adjusting the pH of the fourth material to neutral. The method of adjusting the pH may be a conventional method in the art, which will not be repeated here.

According to the first aspect of the present disclosure, in order to avoid microcapsule aggregation, precipitation, compaction, etc., the method may further include that, in step e, the fourth material may be firstly combined with the first dispersant, thickener and antifreeze After the agent is mixed, it is mixed with the emulsifying and dispersing agent again to obtain a microcapsule suspension-suspension agent containing lambda cyhalothrin and lufenuron. The first dispersant may include sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate, benzylnaphthalenesulfonate formaldehyde condensate, ligninsulfonate One of sodium, desugared sodium lignosulfonate, desugared condensed sodium lignosulfonate, sodium succinate sulfonate, pulverized powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether Or more. The thickener may include one or more of aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite, and white carbon black. The antifreeze agent may include one or more of ethylene glycol, 1,2-propanediol, glycerin, and urea. The weight ratio of the fourth material to the first dispersant, thickener and antifreeze may be 1: (0.01-0.2): (0.001-0.02): (0.02-0.15).

Further, in order to improve the storage performance of the microcapsules, in step e, the weight ratio of the fourth material to the lufenuron suspension agent and the emulsifying and dispersing agent is preferably 1: (0.2-0.5): (0.02- 0.05) Mixed.

According to the first aspect of the present disclosure, the preparation method of the lufenuron suspension in step e may be a preparation method well-known to those skilled in the art, and the disclosure does not particularly limit it. For example, you can fully mix and disperse lumbenzuron with the second dispersant and water, so that lumbenzuron is present in the aqueous solution in the form of suspended particles, and then sand it so that the average particle size of lumbenzuron particles is 1-5 microns. A lufenuron suspension was obtained. The second dispersant may include sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate, benzylnaphthalenesulfonate formaldehyde condensate, ligninsulfonate One of sodium, desugared sodium lignosulfonate, desugared condensed sodium lignosulfonate, sodium succinate sulfonate, pulverized powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether Or more. The weight ratio of the lufenuron to the second dispersant and water may be 1: (0.2-0.5): (1.5-3). In addition, the lufenuron suspension agent may further include one or more of defoamers, thickeners, antifreeze agents, and preservatives. The defoaming agent may be a polyether defoaming agent and / or a silicone defoaming agent. The thickener may include one or more of aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite, silica, and the like. The antifreeze agent may include one or more of ethylene glycol, 1,2-propanediol, glycerin, and urea.

According to the first aspect of the present disclosure, in order to further improve the storage stability of the microcapsule suspension-suspending agent containing lambda-cyhalothrin and lufenuron, the emulsifying and dispersing agent in step e may include dodecylbenzene Sodium sulfonate, sodium methylenebisnaphthalene sulfonate, sodium 1-methylnaphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonate formaldehyde condensate, sodium lignosulfonate, desugared sodium lignosulfonate, desugared One or more of condensed sodium lignin sulfonate, sodium succinate sulfonate, split powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether.

The second aspect of the present disclosure: to provide a microcapsule suspension-suspending agent containing lambda cyhalothrin and loxifen prepared by the method of the first aspect of the present disclosure.

The disclosure is further described in detail below by examples, and is not intended to limit the disclosure.

In the examples and comparative examples, lambda-cyhalothrin was purchased from Jiangsu Huifeng Agrochemical Co., Ltd., lodicarb (content 98%) was purchased from Jiangsu Zhongqi Technology Co., Ltd., and melamine was purchased from Beijing Chemical Factory. Urea was purchased from Beijing Chemical Plant, benzomelamine was purchased from Beijing Chemical Plant, formaldehyde was purchased from Beijing Chemical Plant, sorbitan monostearate polyoxyethylene ether was purchased from Nanjing Taihua Chemical Co., Ltd., dodecyl sulfate Sodium was purchased from Beijing Zhongchuang Hongda Technology Co., Ltd., sodium lignosulfonate was purchased from Beijing Zhongchuang Hongda Technology Co., Ltd., and sodium dodecylbenzenesulfonate was purchased from Beijing Zhongchuang Hongda Technology Co., Ltd .; polyvinyl alcohol Purchased from Zhengzhou Aocai Chemical Materials Co., Ltd., fatty alcohol polyoxyethylene ether from Xingtai Lanxing Auxiliary Factory, aluminum magnesium silicate from Hunan Pengtai High-tech Materials Co., Ltd., bentonite from Zhejiang Anji Tianlong Organic Bentonite Co., Ltd., Silicone defoamer was purchased from Shanghai Maitu High-tech Materials Group, ethylene glycol, glycerin, 1,2-propanediol were purchased from Beijing Chemical Plant, xanthan gum was purchased from Shandong Zhongxuan Co., Ltd., and sodium benzoate was purchased from Beijing Huamei Zhibo Technology Co., Ltd., 200 # solvent oil was purchased from Jiangsu Hualun Chemical Co., Ltd., 150 # solvent oil was purchased from Jiangsu Hualun Chemical Co., Ltd., petroleum ether was purchased from Xilong Chemical Co., Ltd., ethyl acetate was purchased from Xilong Chemical Co., Ltd.

Example 1

Mix melamine, formaldehyde and water, and react at pH 8 at a temperature of 70 ° C for 1.5 hours to obtain an aqueous solution of melamine-formaldehyde resin prepolymer. The molar ratio of formaldehyde to melamine is 1: 0.5. Water and formaldehyde The weight ratio is 2.5: 1.

Mix lambda cyhalothrin, 200 # solvent oil and sorbitan monostearate polyoxyethylene ether uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 200 #The weight ratio of solvent oil and sorbitan monostearate polyoxyethylene ether is 1: 2: 0.05.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 4: 1 at a stirring speed of 2000 rpm to obtain the first material; then at room temperature, adjust the pH to 4.3. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the above first material at a uniform speed within 1 hour, and mixed evenly at a stirring speed of 1000 rpm to obtain a pH value adjusted to The second material of 6.2; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform speed within 1.5 hours, and mix evenly at a stirring speed of 1200 rpm to obtain a pH value adjusted to 3.2 The third material; at 60 ℃, the third material is treated for 2 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; lignin sulfonate is added to the fourth material Sodium, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol is 1: 0.01: 0.005: 0.05.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, the lambda cyhalothrin microcapsule suspension agent and the lufenuron suspension agent are mixed, and then sodium lignosulfonate and water are added, and the mixture is stirred evenly to obtain the lambda cyhalothrin and lofenuron containing this example Microcapsule suspension-suspending agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.3: 0.05.

Example 2

Mix melamine, formaldehyde and water, and react at pH 8 and temperature of 70 ° C for 1.5h to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 1, water and formaldehyde The weight ratio is 4: 1.

Mixing lambda cyhalothrin, 150 # solvent oil and sodium lignosulfonate uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 150 # solvent oil and lignin sulfonic acid The weight ratio of sodium is 1: 0.5: 0.1.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 2: 1 at a stirring speed of 1500 rpm to obtain the first material; then at room temperature, set the pH value 3. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the first material evenly within 1 hour, mixed evenly at a stirring speed of 1100 rpm, and the pH value is adjusted to The second material of 6; at room temperature, add hydrochloric acid with a concentration of 6% by weight to the above second material at a uniform rate within 1 hour, and mix evenly at a stirring speed of 1300 rpm to obtain a pH value adjusted to The third material of 3; under the condition of 50 ℃, the third material is processed for 4 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; dodecane is added to the fourth material Sodium benzene sulfonate, xanthan gum and glycerin are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, in which the fourth material is combined with sodium dodecylbenzene sulfonate, xanthan gum and glycerin The weight ratio of alcohol is 1: 0.05: 0.01: 0.1.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, the lambda cyhalothrin microcapsule suspension agent and the lufenuron suspension agent are mixed, and then sodium lignosulfonate and water are added, and the mixture is stirred evenly to obtain the lambda cyhalothrin and lofenuron containing this example Microcapsule suspension-suspending agent. Among them, the weight ratio of the cyfluthrin microcapsule suspension agent, the lufenuron suspension agent, and the sodium lignosulfonate is 1: 0.5: 0.1.

Example 3

Mix melamine, formaldehyde and water, and react at pH 8 at a temperature of 72 ° C for 1.5 hours to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 1.5, water and formaldehyde The weight ratio is 5: 1.

Mix lambda cyhalothrin, 200 # solvent oil and sorbitan monostearate polyoxyethylene ether uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 200 #The weight ratio of solvent oil and sorbitan monostearate polyoxyethylene ether is 1: 3: 0.15.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 3: 1 at a stirring speed of 2500 rpm to obtain the first material; then at room temperature, adjust the pH to 3.6. The total concentration of the buffer pair is 0.55% by weight of acetic acid-sodium acetate buffer solution, which is added to the above first material at a uniform speed within 1.5 hours, mixed evenly at a stirring speed of 1200 rpm, and the pH value is adjusted to 4.5 The second material; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform rate within 1 hour, and mix evenly at a stirring speed of 1400 rpm to obtain a pH value adjusted to 3.5 The third material; at 45 ℃, the third material is treated for 5 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; lignin sulfonate is added to the fourth material Sodium, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol is 1: 0.2: 0.015: 0.2.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, the lambda cyhalothrin microcapsule suspension agent and the lufenuron suspension agent are mixed, and then sodium lignosulfonate and water are added, and the mixture is stirred evenly to obtain the lambda cyhalothrin and lofenuron containing this example Microcapsule suspension-suspending agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.8: 1.

Example 4

Mix melamine, formaldehyde and water, and react at pH 8 and temperature of 70 ° C for 1.5h to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 2, water and formaldehyde The weight ratio is 6: 1.

Mixing lambda-cyhalothrin, petroleum ether and sodium lauryl sulfate uniformly to obtain lambda-cyhalothrin emulsifiable concentrate, wherein the lambda-cyhalothrin, petroleum ether and sodium lauryl sulfate The weight ratio is 1: 5: 0.2.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 5: 1 at 3000 rpm to obtain the first material; then at room temperature, set the pH value 4.5. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the first material at a uniform speed within 1 hour, and mixed evenly at a stirring speed of 1200 rpm to obtain a pH value adjusted to The second material of 6.5; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform rate within 1.5 hours, and mix evenly at a stirring speed of 1500 rpm to obtain a pH value adjusted to 3.7 The third material; at 60 ° C, process the third material for 2 hours to obtain a fourth material and adjust the pH of the fourth material to 7; add fatty alcohol to the fourth material Oxyethylene ether, bentonite and 1,2-propylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to fatty alcohol polyoxyethylene ether, bentonite and 1,2-propylene glycol is 1: 0.2: 0.02: 0.15.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, the lambda cyhalothrin microcapsule suspension agent and the lufenuron suspension agent are mixed, and then sodium lignosulfonate and water are added, and the mixture is stirred evenly to obtain the lambda cyhalothrin and lofenuron containing this example Microcapsule suspension-suspending agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 1: 2.

Example 5

Mix melamine, formaldehyde and water, and react at pH 7.5 and temperature of 70 ℃ for 1.5h to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 0.1, water and formaldehyde The weight ratio is 2: 1.

Mix lambda cyhalothrin, 200 # solvent oil and sorbitan monostearate polyoxyethylene ether uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 200 #The weight ratio of solvent oil and sorbitan monostearate polyoxyethylene ether is 1: 0.1: 0.01.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 1: 1 with a stirring speed of 2000 rpm to obtain the first material; then at room temperature, set the pH value 4.5. The total concentration of the buffer pair is 2% by weight of the citric acid-disodium hydrogen phosphate buffer solution, which is added to the first material at a uniform rate within 1 hour, and mixed evenly at a stirring speed of 1100 rpm to obtain a pH value The second material adjusted to 7; at room temperature, hydrochloric acid with a concentration of 5% by weight is added to the above second material at a uniform rate within 1.5 hours, and mixed evenly at a stirring speed of 1300 rpm to obtain a pH value The third material adjusted to 3.5; at 60 ℃, the third material is treated for 2 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; add to the fourth material Sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, in which the fourth material is combined with sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol The weight ratio is 1: 0.02: 0.001: 0.02.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns The suspension of chlorpyrifos was obtained.

Finally, the lambda cyhalothrin microcapsule suspension agent and the lufenuron suspension agent are mixed, and then sodium lignosulfonate and water are added, and the mixture is stirred evenly to obtain the lambda cyhalothrin and lofenuron containing this example Microcapsule suspension-suspending agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.2: 0.5.

Example 6

Mix melamine, formaldehyde and water, and react at pH 8 at a temperature of 70 ° C for 1.5 hours to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 0.2, water and formaldehyde The weight ratio is 2.5: 1.

Mix lambda cyhalothrin, ethyl acetate and polyvinyl alcohol uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the weight ratio of lambda cyhalothrin, ethyl acetate and polyvinyl alcohol is 1 : 1.5: 0.02.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 4: 1 at a stirring speed of 2000 rpm to obtain the first material; then at room temperature, adjust the pH to 4.5. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the above first material at a uniform speed within 0.5 hours, and mixed evenly at a stirring speed of 1000 rpm to obtain a pH value adjusted to The second material of 6.2; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform speed within 1.5 hours, and mix evenly at a stirring speed of 1200 rpm to obtain a pH value adjusted to 3.2 The third material; at 60 ℃, the third material is treated for 2 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; lignin sulfonate is added to the fourth material Sodium, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol is 1: 0.15: 0.002: 0.04.

20% by weight of fenprofen (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, the lambda cyhalothrin microcapsule suspension agent and the lufenuron suspension agent are mixed, and then sodium lignosulfonate and water are added, and the mixture is stirred evenly to obtain the lambda cyhalothrin and lofenuron containing this example Microcapsule suspension-suspending agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.1: 0.01.

Example 7

Mix melamine, formaldehyde and water, and react at pH 8 at a temperature of 70 ° C for 1.5 hours to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 0.2, water and formaldehyde The weight ratio is 2.5: 1.

Mix lambda cyhalothrin, ethyl acetate and polyvinyl alcohol uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the weight ratio of lambda cyhalothrin, ethyl acetate and polyvinyl alcohol is 1 : 1.5: 0.02.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 4: 1 at a stirring speed of 2000 rpm to obtain the first material; then at room temperature, adjust the pH to 4.5. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the above first material at a uniform speed within 0.5 hours, and mixed evenly at a stirring speed of 1000 rpm to obtain a pH value adjusted to The second material of 6.2; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform speed within 1.5 hours, and mix evenly at a stirring speed of 1200 rpm to obtain a pH value adjusted to 3.2 The third material; at 60 ℃, the third material is treated for 2 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; lignin sulfonate is added to the fourth material Sodium, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol is 1: 0.15: 0.002: 0.04.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, mix the lambda cyhalothrin microcapsule suspension agent with lufenuron suspension agent, and then add sodium lignin sulfonate and water, and stir well to obtain the suspension and suspension of lambda cyhalothrin and lufenuron microcapsules. Agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.3: 0.03.

Example 8

Mix melamine, formaldehyde and water, and react at pH 8 at a temperature of 70 ° C for 1.5 hours to obtain a melamine-formaldehyde resin prepolymer aqueous solution, in which the molar ratio of formaldehyde to melamine is 1: 0.2, water and formaldehyde The weight ratio is 2.5: 1.

Mix lambda cyhalothrin, ethyl acetate and polyvinyl alcohol uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the weight ratio of lambda cyhalothrin, ethyl acetate and polyvinyl alcohol is 1 : 1.5: 0.02.

Mix the melamine-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 4: 1 at a stirring speed of 2000 rpm to obtain the first material; then at room temperature, adjust the pH to 4.5. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the above first material at a uniform speed within 0.5 hours, and mixed evenly at a stirring speed of 1000 rpm to obtain a pH value adjusted to The second material of 6.2; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform speed within 1.5 hours, and mix evenly at a stirring speed of 1200 rpm to obtain a pH value adjusted to 3.2 The third material; at 60 ℃, the third material is treated for 2 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; lignin sulfonate is added to the fourth material Sodium, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol is 1: 0.04: 0.03: 0.2.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, mix the lambda cyhalothrin microcapsule suspension agent with lufenuron suspension agent, and then add sodium lignin sulfonate and water, and stir well to obtain the suspension and suspension of lambda cyhalothrin and lufenuron microcapsules. Agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.1: 0.01.

Example 9

Mix urea, formaldehyde and water, and react at pH 7.5 and temperature of 70 ° C for 1.5h to obtain an aqueous solution of urea-formaldehyde resin prepolymer. The molar ratio of formaldehyde to urea is 1: 2. Water and formaldehyde The weight ratio is 2.6: 1.

Mix lambda cyhalothrin, 200 # solvent oil and sorbitan monostearate polyoxyethylene ether uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 200 #The weight ratio of solvent oil and sorbitan monostearate polyoxyethylene ether is 1: 2.5: 0.05.

Mix the urea-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 4: 1 at a stirring speed of 2000 rpm to obtain the first material; then at room temperature, set the pH value 4.5. The total concentration of the buffer pair is 2% by weight of acetic acid-sodium acetate buffer solution, which is added to the above first material at a uniform speed within 1.5 hours, mixed evenly at a stirring speed of 1000 rpm, and the pH value is adjusted to The second material of 6.2; at room temperature, add hydrochloric acid with a concentration of 5% by weight to the above second material at a uniform speed within 1.5 hours, and mix evenly at a stirring speed of 1200 rpm to obtain a pH value adjusted to 3.2 The third material; at 60 ℃, the third material is treated for 2 hours to obtain a fourth material and the pH value of the fourth material is adjusted to 7; lignin sulfonate is added to the fourth material Sodium, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight ratio of the fourth material to sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol is 1: 0.01: 0.004: 0.05.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, mix the lambda cyhalothrin microcapsule suspension agent with lufenuron suspension agent, and then add sodium lignin sulfonate and water, and stir well to obtain the suspension and suspension of lambda cyhalothrin and lufenuron microencapsulation Agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 1: 0.05.

Example 10

Mix urea, formaldehyde and water, and react at pH 8 at a temperature of 70 ° C for 1.5 hours to obtain an aqueous solution of urea-formaldehyde resin prepolymer. The molar ratio of formaldehyde to urea is 1: 1. Water and formaldehyde The weight ratio is 2.8: 1.

Mix lambda cyhalothrin, 200 # solvent oil and sorbitan monostearate polyoxyethylene ether uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 200 #The weight ratio of solvent oil and sorbitan monostearate polyoxyethylene ether is 1: 1.5: 0.06.

Mix the urea-formaldehyde resin prepolymer aqueous solution and lambda cyhalothrin emulsifiable concentrate at a weight ratio of 3: 1 with a stirring speed of 2000 rpm to obtain the first material; then at room temperature, set the pH value 3.6. The citric acid-sodium citrate buffer solution with a total concentration of 4% by weight of the buffer pair is added to the above first material at a uniform speed within 1 hour, and mixed evenly at a stirring speed of 1000 rpm to obtain the pH value. The second material adjusted to 6.2; at room temperature, add phosphoric acid with a concentration of 4% by weight to the above second material at a uniform speed within 1.5 hours, and mix evenly at a stirring speed of 1200 rpm to obtain the pH value. The third material adjusted to 3.2; at 60 ° C, the third material is treated for 2 hours to obtain a fourth material and the pH of the fourth material is adjusted to 7; wood is added to the fourth material Sodium sulfonate, aluminum magnesium silicate and ethylene glycol are mixed evenly to obtain a high-efficiency cyhalothrin microcapsule suspension agent, wherein the weight of the fourth material and sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol The ratio is 1: 0.02: 0.005: 0.05.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, mix the lambda cyhalothrin microcapsule suspension agent with lufenuron suspension agent, and then add sodium lignin sulfonate and water, and stir well to obtain the suspension and suspension of lambda cyhalothrin and lufenuron microcapsules. Agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.3: 0.03.

Example 11

Mix benzomelamine, formaldehyde and water, and react at pH 8 and temperature 70 ° C for 2 hours to obtain an aqueous solution of benzomelamine-formaldehyde resin prepolymer. The molar ratio of formaldehyde to melamine is 1: 0.5, the weight ratio of water and formaldehyde is 2.8: 1.

Mix lambda cyhalothrin, 200 # solvent oil and sorbitan monostearate polyoxyethylene ether uniformly to obtain lambda cyhalothrin emulsifiable concentrate, wherein the lambda cyhalothrin, 200 #The weight ratio of solvent oil and sorbitan monostearate polyoxyethylene ether is 1: 2: 0.06.

The benzomelamine-formaldehyde resin prepolymer aqueous solution and the high-efficiency cyhalothrin emulsifiable concentrate are mixed at a weight ratio of 3: 1 at a stirring speed of 2000 rpm to obtain the first material; then at room temperature, the pH A citric acid-sodium citrate buffer solution with a value of 4 and a total buffer pair concentration of 4% by weight is added to the above-mentioned first material at a uniform rate within 1 hour, and mixed uniformly at a stirring speed of 1000 rpm to obtain a pH The second material whose value is adjusted to 6.2; at room temperature, sulfuric acid with a concentration of 5% by weight is added to the above second material at a uniform speed within 1.5 hours, and mixed evenly at a stirring speed of 1200 rpm to obtain a pH The third material whose value is adjusted to 3.2; at 60 ° C, process the third material for 2 hours to obtain a fourth material and adjust the pH of the fourth material to 7; to the fourth material Add sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol and mix well to obtain a high-efficiency cyhalothrin microcapsule suspension agent, in which the fourth material is combined with sodium lignosulfonate, aluminum magnesium silicate and ethylene glycol The weight ratio is 1: 0.03: 0.005: 0.05.

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Finally, mix the lambda cyhalothrin microcapsule suspension agent with lufenuron suspension agent, and then add sodium lignin sulfonate and water, and stir well to obtain the suspension and suspension of lambda cyhalothrin and lufenuron microcapsules. Agent. Among them, the weight ratio of lambda cyhalothrin microcapsule suspension agent, lufenuron suspension agent, and sodium lignosulfonate is 1: 0.15: 0.05.

Comparative Example 1

The difference from Example 1 is that after the first material is obtained, the pH value of the material is directly adjusted to 3.2 by using hydrochloric acid with a concentration of 5% by weight without adjusting the pH value of the acetic acid-sodium acetate buffer solution.

Comparative Example 2

The difference from Example 1 is that after the first material is obtained, the pH of the material is adjusted to 4.4 with an acetic acid-sodium acetate buffer solution having a pH of 4.4 and a total concentration of 2% by weight of the buffer pair. Steps to adjust the pH.

Comparative Example 3

The difference from Example 1 is that the pH value of the third material is adjusted to 2 using hydrochloric acid with a concentration of 5 wt%.

Comparative Example 4

Mix high-efficiency cyhalothrin, 200 # solvent oil, sorbitan monostearate polyoxyethylene ether and water in a weight ratio of 1: 0.6: 0.1: 2 to uniformly obtain high-efficiency cyhalothrin water Emulsion, the same method as in Example 1 was used to prepare fenprofen suspension, the high-efficiency cyfluthrin aqueous emulsion and the fenprofen suspension were mixed in a weight ratio of 1: 0.5, to obtain high-efficiency cyfluthrin and fenprofen micro Suspending emulsion.

Comparative Example 5

Mix high-efficiency cyhalothrin, 200 # solvent oil, sorbitan monostearate polyoxyethylene ether and water in a weight ratio of 1: 0.5: 0.1: 5 and mix evenly to obtain high-efficiency cyhalothrin water Emulsion.

Comparative Example 6

20% by weight of fenpyrifos (content 95%), 2% by weight of sodium lauryl sulfate, 6% by weight of sodium lignosulfonate, 0.2% by weight of silicone defoamer, 5% by weight Ethylene glycol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 60% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand milling, and the average particle size is less than 5 microns. The suspension of chlorpyrifos was obtained.

Test Example 1

This test example is used to test the high-efficiency cyfluthrin and microcarbosulfan suspensions obtained in Examples 1-11 and Comparative Examples 1-3 and the high-efficiency cyfluthrin obtained in Comparative Example 4. The heat storage stability and low temperature stability of the fenfluramide microsuspension, the high-efficiency cyhalothrin aqueous emulsion of Comparative Example 5, and the fenpyramide suspension of Comparative Example 6.

Thermal storage stability test: the micro-capsule suspension-suspending agent of lambda-cyhalothrin and lufenuron obtained in Examples 1-11 and Comparative Examples 1-3 and the lambda-cyhalothrin obtained in Comparative Example 4 The microsuspension of lufenuron, the high-efficiency cyhalothrin aqueous emulsion of Comparative Example 5, and the lufenuron suspension of Comparative Example 6 were put into a container, sealed and placed in a constant temperature oven at (54 ± 2) ℃, Take it out after standing for 14 days. According to the GB / T14825-2006 standard, determine the suspension rate. The results are shown in Table 1.

Low-temperature stability measurement: the micro-capsule suspension-suspending agent of lambda-cyhalothrin and lufenuron obtained in Examples 1-11 and Comparative Examples 1-3 and the lambda-cyhalothrin obtained in Comparative Example 4 and Lufenuron microsuspension, the high-efficiency cyhalothrin aqueous emulsion of Comparative Example 5 and the lufenuron suspension of Comparative Example 6 were put into a container, sealed and placed in a refrigerator at (0 ± 2) ℃ for 1h , Stir once every 15min, 15s each time, observe whether there is any change in appearance, continue to stand at (0 ± 2) ℃ for 7 days, then take it out and leave it at room temperature to recover, according to GB / T14825-2006 standard, determine The suspension rate, the results are shown in Table 1.

Table 1

A	Thermal storage stability	Low temperature stability
Example 1	Good fluidity, no layering and agglomeration, suspension rate is 96.2%	Good fluidity, no layering and agglomeration, suspension rate is 96.4%
Example 2	Good fluidity, no layering and agglomeration, suspension rate is 96.3%	Good fluidity, no layering and agglomeration, suspension rate is 98.1%
Example 3	Good fluidity, no layering and agglomeration, suspension rate is 93.4%	Good fluidity, no layering and agglomeration, suspension rate is 95.2%
Example 4	Good fluidity, no layering and agglomeration, suspension rate is 96.7%	Good fluidity, no layering and agglomeration, suspension rate is 96.7%
Example 5	Good fluidity, no layering and agglomeration, suspension rate is 94.6%	Good fluidity, no layering and agglomeration, suspension rate is 96.1%
Example 6	Good fluidity, no layering and agglomeration, suspension rate is 97.1%	Good fluidity, no layering and agglomeration, suspension rate is 96.5%
Example 7	Good fluidity, no layering and agglomeration, suspension rate is 98.3%	Good fluidity, no layering and agglomeration, suspension rate is 99.5%
Example 8	Good fluidity, no layering and agglomeration, suspension rate is 94.5%	Good fluidity, no layering and agglomeration, suspension rate is 95.3%
Example 9	Good fluidity, no layering and agglomeration, suspension rate is 95.9%	Good fluidity, no layering and agglomeration, suspension rate is 96.9%
Example 10	Good fluidity, no layering and agglomeration, suspension rate is 96.2%	Good fluidity, no layering and agglomeration, suspension rate is 93.2%
Example 11	Good fluidity, no layering and agglomeration, suspension rate is 95.2%	Good fluidity, no layering and agglomeration, suspension rate is 95.8%

Comparative Example 1	Increased viscosity, slightly poorer fluidity, suspension rate is 81.4%	The fluidity is slightly worse, the suspension rate is 83.6%
Comparative Example 2	Increased viscosity, poor fluidity, suspension rate is 82.9%	Liquidity is slightly worse, suspension rate is 86.9%
Comparative Example 3	solidification	solidification
Comparative Example 4	Increased viscosity, poor fluidity, suspension rate is 75.9%	Increased viscosity, poor fluidity, suspension rate is 73.9%
Comparative Example 5	Layered	Layered
Comparative Example 6	Increased viscosity, poor fluidity, suspension rate is 85.9%	Increased viscosity, poor fluidity, suspension rate is 83.4%

It can be seen from Table 1 that the high-efficiency cyfluthrin and microcarbosulfan microcapsule suspension-suspending agent obtained by the preparation method provided by the present invention has good thermal storage stability and low-temperature storage stability.

Test Example 2

This test example compares the high-efficiency cyfluthrin and microcarbosulfan microcapsule suspension-suspending agents obtained in Examples 1-11, Comparative Examples 1-3, and the high-efficiency cyfluthrin and lice obtained in Comparative Example 4. The control effect of mite-urea microsuspension, high-efficiency cyhalothrin aqueous emulsion of Comparative Example 5 and the mite-urea suspension of Comparative Example 6 on Plutella xylostella on cabbage was tested. Before the test, add a certain amount of distilled water, stir well, and adjust the high-efficiency cyfluthrin and microcarbosulfan microcapsule suspension-suspending agent obtained in Examples 1-11, Comparative Examples 1-3, and Comparative Example 4 respectively. The active ingredient concentration in the lambda-cyhalothrin and fenfenuron micro-suspension, Comparative Example 5 lambda-cyhalothrin aqueous emulsion and Comparative Example 6 fenprofen suspension was 10% by weight.

Test location: Weifang City, Shandong Province. The test field is a cabbage planting base for many years. The test field has flat terrain, medium fertility, and medium texture. Cabbage in each treatment area after application is routinely managed.

The specific steps include using a knapsack sprayer to suspend and suspend the high-efficiency cyfluthrin and microcarbosulfan microcapsules obtained in Examples 1-11 and Comparative Examples 1-3 according to the application rate of 30 kg / mu. The lambda-cyhalothrin and fenprofen micro-suspension obtained in Comparative Example 4, the lambda-cyhalothrin aqueous emulsion in Comparative Example 5, and the fenprofen suspension solution in Comparative Example 6 were applied to the respective planting areas. Cabbage plants were page sprayed, and the blank control group used the same amount of water to spray the cabbage plants in the planting area.

The control effect of Plutella xylostella was investigated 10 days, 20 days, 30 days and 50 days after application. The specific test method was carried out in accordance with the Guidelines for Pesticide Field Efficacy Test. Random 5-point sampling was used in each treatment area. 25 bushes of cabbage were investigated in each treatment area. The control effect of Plutella xylostella in each treatment area was investigated. The mortality was calculated according to formula (1) and the corrected mortality was calculated according to formula (2). Table 2 shows.

The specific results are shown in Table 2.

Table 2

Test Example 3

This test example compares the high-efficiency cyfluthrin and microcarbosulfan microcapsule suspension-suspending agents obtained in Examples 1-11, Comparative Examples 1-3, and the high-efficiency cyfluthrin and lice obtained in Comparative Example 4. The control effects of fencarbazone microsuspension emulsion, high-efficiency cyhalothrin aqueous emulsion of Comparative Example 5 and chlorfenapyr suspension of Comparative Example 6 on cabbage whitefly and aphids were tested. Before the test, add a certain amount of distilled water, stir evenly, adjust the high-efficiency cyfluthrin and fenprofen microcapsule suspension-suspending agent obtained in Examples 1-11, Comparative Examples 1-3, and the high efficiency obtained in Comparative Example 4. The concentration of the active ingredient in the cyfluthrin and microfenuron microsuspension, the high-efficiency cyhalothrin aqueous emulsion of Comparative Example 5, and the fenflufenuron suspension of Comparative Example 6 was 10% by weight.

Test location: Dingzhou City, Hebei Province. The land is flat and has good fertility. The Chinese cabbage in each treatment area after the application of the pesticide is produced and managed according to the routine.

The specific steps include, using a knapsack sprayer, according to the spray volume of 30 kg / mu, suspending and suspending the high-efficiency cyfluthrin and microcarbosulfan microcapsules obtained in Examples 1-11 and Comparative Examples 1-3, The microfluidic cyfluthrin and fenprofen microsuspension obtained in Comparative Example 4, the cypermethrin aqueous emulsion of Comparative Example 5 and the fenprofen suspending agent liquid of Comparative Example 6 were sprayed uniformly on each On the cabbage plants in the planting area, the blank control group sprayed the cabbage plants in the planting area with the same amount of clean water. When applying the pesticides, the adjacent cells were covered with plastic film to prevent the interference of the drugs.

The control effect of whitefly and aphids was investigated 10 days, 20 days, 30 days and 50 days after application. The specific test method was carried out in accordance with the "Pesticide Field Efficacy Test Guidelines". Each treatment area adopts random 5-point sampling. Each treatment area investigates 25 cabbage plants, investigates the control effect of whitefly and aphids in each treatment area, calculates the mortality rate according to formula (1) and calculates the corrected mortality rate according to formula (2). The results are shown in Table 3:

table 3

It can be seen from Tables 2 and 3 that the preparation method provided by the present disclosure adjusts the pH value in two steps and prepares the high-efficiency cyfluthrin and loprofen under the reaction conditions of specific stirring speed, emulsifier and solvent. Capsule suspension-suspending agent can achieve the effect of slow-release and long-term control of crop pests. Moreover, the effect of the high-efficiency cyfluthrin and microcarbosulfan microcapsule suspension-suspending agent prepared by the method is much better than that of the high-efficiency cyfluthrin aqueous emulsion single dose and the single fenprofen suspension. Compared with other dosage forms of lambda-cyhalothrin and lufenuron microcapsule suspension-suspending agent, the lambda-cyhalothrin and lufenuron microcapsules of the present invention have the characteristics of long lasting period, which can reduce the number of medications and medication Quantity, cost savings, which contains less organic solvents, which can reduce environmental pollution.

The preferred embodiments of the present disclosure have been described in detail above. However, the present disclosure is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present disclosure, various simple modifications can be made to the technical solutions of the present disclosure. These simple modifications All belong to the protection scope of the present disclosure.

In addition, it should be noted that the specific technical features described in the above specific embodiments can be combined in any suitable manner without contradictions. In order to avoid unnecessary repetition, the present disclosure The combination method will not be explained separately.

In addition, various combinations of various embodiments of the present disclosure can also be arbitrarily combined, as long as it does not violate the idea of the present disclosure, it should also be regarded as what is disclosed in the present disclosure.

Industrial applicability

A method for preparing a microcapsule suspension-suspension agent containing high-efficiency cyhalothrin and lufenuron and a microcapsule suspension-suspension agent provided in the embodiments of the present disclosure include: a. Prepolymerizing the amino resin The aqueous solution and lambda cyhalothrin emulsifiable concentrate are mixed in a weight ratio of (1-5): 1 to obtain the first material; b. The first material is mixed with the buffer solution to obtain a second material with a pH of 4-7; c. Mix the second material with the acid solution to obtain a third material with a pH of 3-4; d. Stir the third material for 2-5 hours at a temperature of 40-70 ° C to obtain a fourth material; e. Mix the fourth material with fenprofen suspending agent and emulsifying and dispersing agent in a weight ratio of 1: (0.1-1): (0.01-2); prepared by the method containing lambda cyhalothrin and lice The microcapsule suspension-suspending agent of teburea has good storage stability, can slowly release long-term control of crop pests, reduce the number and amount of medication, save costs, and reduce environmental pollution.

Claims (10)

1. A method for preparing microcapsule suspension-suspending agent containing high-efficiency cyhalothrin and lufenuron, characterized in that the method comprises the following steps:

   a. Mix the aqueous solution of amino resin prepolymer and high-efficiency cyhalothrin emulsifiable concentrate at a weight ratio of (1-5): 1, to obtain the first material;

   b. Mix the first material obtained in step a with the buffer solution to obtain a second material, and the pH of the second material is 4-7;

   c. Mix the second material obtained in step b with an acid solution to obtain a third material, and the pH of the third material is 3-4;

   d. The third material obtained in step c is stirred for 2-5 hours under the condition of a temperature of 40-70 ° C to obtain a fourth material;

   e. Mix the fourth material obtained in step d with the fenprofen suspending agent and emulsifying and dispersing agent in a weight ratio of 1: (0.1-1): (0.01-2) to obtain a high-efficiency cyhalothrin And microcapsule suspension-suspensions of lufenuron.
2. The method according to claim 1, wherein the aqueous solution of the amino resin prepolymer in step a is obtained by prepolymerizing an amino group-containing compound, formaldehyde and water;

   Optionally, the molar ratio of the amino-containing compound to formaldehyde is (0.1-2): 1, and the weight ratio of water to formaldehyde is (2-6): 1;

   Optionally, the amino-containing compound includes one or more of urea, melamine and benzomelamine;

   Optionally, the pre-polymerization conditions include: a pH value of 8-10, a temperature of 60-80 ° C, and a time of 0.5-3 hours.
3. The method according to claim 1 or 2, wherein the lambda cyhalothrin in step a contains lambda cyhalothrin, an organic solvent and an emulsifier;

   Optionally, the organic solvent includes one or more of petroleum ether, ethyl acetate, methyl oleate, xylene and solvent oil;

   Optionally, the emulsifier includes sodium lignosulfonate, sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, styrene-maleic anhydride copolymer, fatty alcohol polyoxyethylene ether, sorbitan One or more of alcohol polyoxyethylene polyoxypropylene ether, sorbitan monostearate polyoxyethylene ether, sodium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate;

   Optionally, the weight ratio of the lambda-cyhalothrin, the organic solvent and the emulsifier is 1: (0.1-5): (0.01-0.2).
4. The method according to claim 1, wherein the buffer solution in step b contains a buffer pair;

   Optionally, the buffer pair includes one or more of citric acid-sodium citrate, citric acid-disodium hydrogen phosphate, and acetic acid-sodium acetate.
5. The method according to claim 1, wherein the acidic solution in step c includes one or more of hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid, and ammonium chloride.
6. The method according to any one of claims 1, 2, 4 and 5, wherein the method comprises one or more of the following features:

   The mixing in step a is performed under stirring conditions, and the stirring speed is 1500-3000 rpm;

   The mixing in step b is performed under stirring conditions, and the stirring speed is 1000-1200 rpm;

   The mixing in step c is performed under stirring conditions, and the stirring speed is 1200-1500 rpm.
7. The method according to claim 1, further comprising, in step e, mixing the fourth material with the first dispersant, thickener and antifreeze, and then with the emulsifying dispersant mixing;

   Optionally, the first dispersant includes sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate, benzylnaphthalenesulfonate formaldehyde condensate, Sodium lignosulfonate, desugared sodium lignosulfonate, desugared condensed sodium lignosulfonate, sodium succinate sulfonate, pulverized powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether One or more of

   Optionally, the thickener includes one or more of aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite, and white carbon black;

   Optionally, the antifreeze includes one or more of ethylene glycol, 1,2-propanediol, glycerin, and urea;

   Optionally, the weight ratio of the fourth material to the first dispersant, the thickener and the antifreeze is 1: (0.01-0.2): (0.001-0.02): (0.02-0.15) .
8. The method according to claim 1 or 7, characterized in that in step e, the weight ratio of the fourth material to the lufenuron suspension agent and the emulsifying and dispersing agent is 1: (0.2-0.5): (0.02-0.05) mixed.
9. The method according to claim 8, characterized in that the louse mite suspension in step e is obtained by mixing loprofen with a second dispersant and water;

   Optionally, the weight ratio of the lufenuron to the second dispersant and water is 1: (0.2-0.5): (1.5-3);

   Optionally, the second dispersant includes sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate, benzylnaphthalenesulfonate formaldehyde condensate, Sodium lignosulfonate, desugared sodium lignosulfonate, desugared condensed sodium lignosulfonate, sodium succinate sulfonate, pulverized powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether One or more of

   Optionally, the emulsifying and dispersing agent includes sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde condensate, benzylnaphthalenesulfonate formaldehyde condensate, wood Sodium sulfonate, desugared lignin sulfonate, desugared condensed lignin sulfonate, sodium succinate sulfonate, split powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether One or more.
10. The microcapsule suspension-suspending agent containing lambda cyhalothrin and loxifen prepared by the method of any one of claims 1-9.