WO2020108197A1 - 一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂及其制备方法 - Google Patents

一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂及其制备方法 Download PDF

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WO2020108197A1
WO2020108197A1 PCT/CN2019/113602 CN2019113602W WO2020108197A1 WO 2020108197 A1 WO2020108197 A1 WO 2020108197A1 CN 2019113602 W CN2019113602 W CN 2019113602W WO 2020108197 A1 WO2020108197 A1 WO 2020108197A1
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atrazine
suspension
weight
metolachlor
sodium
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PCT/CN2019/113602
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English (en)
French (fr)
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刘润峰
潘静
高敬雨
李蕾
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上海明德立达生物科技有限公司
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Publication of WO2020108197A1 publication Critical patent/WO2020108197A1/zh

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • A01N25/28—Microcapsules or nanocapsules
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/22—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom

Definitions

  • the present invention requires a Chinese patent application filed in the China Patent Office with the application number 201811446732.8 and the invention titled "A microcapsule suspension-suspending agent containing atrazine and mesochlor and its preparation method" Priority, the entire content of this application is incorporated by reference into the present invention.
  • the invention relates to the technical field of pesticides, in particular, to a microcapsule suspension-suspending agent containing atrazine and mesochlor and its preparation method.
  • Mesochlor is a selective herbicide of acetamide developed by Syngenta. It is based on metolachlor and uses advanced technology to successfully remove inactive R-body, and the resulting refined active S -body. In addition to the advantages of metolachlor, refined metolachlor is superior to metolachlor in safety and control effect. At the same time, according to the results of toxicological studies, its toxicity is better than that of metolachlor The amine is low, and even only one-tenth of the latter's toxicity. Fine metolachlor is suitable for a broad spectrum of crops and is the main herbicide for corn and soybean, an important food crop in the world.
  • refined metolachlor is mainly based on emulsifiable concentrate.
  • the use and release of a large amount of organic solvents are not only harmful to the ecological environment and users, but also prone to chemical damage, affecting the healthy growth of crops and the guarantee of yield.
  • the present disclosure provides a method for preparing a microcapsule suspension-suspending agent containing atrazine and mesoprofen, and the atrazine and mesoprofen containing the method
  • the microcapsule suspension-suspending agent is both fast-acting and effective, and can effectively control various weeds in crops.
  • the first aspect of the present disclosure to provide a method for preparing microcapsule suspension-suspending agent containing atrazine and mesochlor, wherein the method includes the following steps: a. The aqueous solution of formaldehyde resin prepolymer and refined metolachlor emulsifiable concentrate are mixed in a weight ratio of 1: (0.5-2) to obtain the first material; b. The first material obtained in step a and the buffer solution are mixed evenly, Adjust the pH value of the first material to 5.0-6.5 to obtain a second material; c. Mix the second material obtained in step b with an acidic pH regulator uniformly to adjust the pH of the second material The third material is obtained from 2.5-4.5; d.
  • the third material obtained in step c is subjected to curing polycondensation to obtain the material after curing polycondensation, and then the pH value of the material after curing polycondensation is adjusted to neutral After mixing with the first dispersant, thickener and antifreeze uniformly to obtain a fourth material; e, the fourth material obtained in step d is mixed with the atrazine suspension agent and then added a second dispersant and mixed Evenly.
  • the method further includes: the aqueous solution of the urea-formaldehyde resin prepolymer in step a is obtained by prepolymerizing urea, formaldehyde and water; the conditions of the prepolymerization include: a pH value of 8-9 , The temperature is 65-75 °C, the time is 1-2h.
  • the method further includes: the refined metolachlor emulsifiable concentrate in step a contains refined metolachlor, an organic solvent, and an emulsifier;
  • the organic solvent includes petroleum ether, ethyl acetate, and dichloromethane One or more of methane, chloroform, xylene, solvent oil S-150 and solvent oil S-200
  • the emulsifier includes sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, benzene One of ethylene-maleic anhydride copolymer, alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitan ester, sodium lauryl sulfate, polyvinyl alcohol and castor oil polyoxyethylene ether One or more kinds;
  • the weight ratio of the sinomethon, the organic solvent and the emulsifier is 1: (0.1-1): (0.05-0.2).
  • the buffer solution in step b contains a buffer pair, and the buffer pair includes one or more of citric acid-sodium citrate, citric acid-disodium hydrogen phosphate, and acetic acid-sodium acetate.
  • the total concentration of the buffer pair in the buffer solution is 1-5% by weight, and the pH value of the buffer solution is 3-5.
  • the acidic pH adjusting agent in step c includes one or more of hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid, and ammonium chloride solution, and the concentration of the acidic pH adjusting agent is 1-10% by weight.
  • the temperature of the curing polycondensation is 40-65° C. and the time is 2-4h; the method includes: adjusting the pH value of the material after curing polycondensation to an intermediate level through an alkaline pH adjusting agent
  • the alkaline pH adjusting agent includes one or more of triethylamine, triethanolamine, sodium hydroxide, potassium hydroxide solution; the fourth material, the first dispersant, the first The weight ratio of the thickener and the first antifreeze is 1: (0.01-0.2): (0.001-0.02): (0.02-0.15).
  • step e the weight ratio of the fourth material, the atrazine suspending agent and the second dispersing agent is 1: (0.5-5): (0.01-0.2).
  • the method further includes: before step e, mixing, dispersing, and scrubbing the atrazine original drug, the third dispersant, the third thickener, the third antifreeze, and water to obtain the results in step e
  • the atrazine suspending agent, the atrazine suspending agent is suspended particles with an average particle size of 1-5 ⁇ m.
  • the mixing conditions in step a include: the stirring speed is 200-400r/min, and the stirring time is 30-60min; step b includes, at 25-35°C, within 0.5-1h The buffer solution is added to the first material at a uniform speed, and the mixture is stirred and mixed at a speed of 200-500r/min; step c includes, at 25-35°C, the acidic pH adjusting agent is added to the In the second material, stir and mix at 200-500r/min; the mixing conditions in step d include: stirring speed 200-300r/min, stirring time 1-3h; step e The mixing conditions include: the stirring speed is 200-400r/min, and the stirring time is 30-60 minutes.
  • the second aspect of the present disclosure to provide a microcapsule suspension-suspending agent containing atrazine and mesochlor which is prepared by the method of the first aspect of the present disclosure.
  • the preparation method of the present disclosure significantly improves the storage stability of microcapsule suspension-suspending agent containing atrazine and mesochlor and the control effect on farmland weeds.
  • the microcapsule suspension-suspending agent containing atrazine and mesochlor can be both fast-acting and sustained, and can effectively control various weeds in crops.
  • the first aspect of the present disclosure to provide a method for preparing a microcapsule suspension-suspending agent containing atrazine and mesochlor, wherein the method includes the following steps: a.
  • the weight ratio is 1: (0.5 -2) Mix the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate uniformly to obtain the first material; b. Add the buffer solution to the first material obtained in step a and mix well to adjust the first The pH value of the material is 5.0-6.5 to obtain the second material; c.
  • step b By adding an acidic pH adjuster to the second material obtained in step b and mixing it uniformly, adjust the pH value of the second material to 2.5-4.5 to obtain the second material Three materials; d.
  • the third material obtained in step c is subjected to curing and polycondensation to obtain the material after curing and polycondensation, and then the pH value of the material after curing and polycondensation is adjusted to neutrality with the first dispersant, thickener and antifreeze Mix the agent uniformly to obtain the fourth material; e. Mix the fourth material obtained in step d with the atrazine suspension agent, add the second dispersant and mix evenly.
  • mesochlor is an acetamide herbicide, has a chloroacetamide structure, is a cell division inhibitor, and affects cell growth by inhibiting the synthesis of long-chain fatty acids.
  • Atrazine is also known as atrazine, and its chemical name is 6-chloro-N-ethyl-N′-(1-methylethyl)-1,3,5-triazabenzene-2,4 diamine, English name Atrazine, English chemical name is 6-chloro-N-ethyl-N′-(1-methylethyl)-1,3,5-Triazine-2,4-diamine, molecular formula C 8 H 14 ClN 5 , CAS NO. 1912-24-9, its structural formula is shown in formula (2).
  • the method may further include: the urea-formaldehyde resin prepolymer aqueous solution in step a is obtained by prepolymerizing urea, formaldehyde and water; the conditions of prepolymerization include: a pH value of 8-9 and a temperature of 65-75°C, time is 1-2h.
  • the preparation method of the urea-formaldehyde resin prepolymer aqueous solution may be a preparation method well known to those skilled in the art, and the invention is not particularly limited thereto;
  • the urea-formaldehyde resin prepolymer aqueous solution may be composed of a raw material liquid containing urea, formaldehyde and water It is obtained by prepolymerization;
  • the urea-formaldehyde resin prepolymer aqueous solution can be obtained by prepolymerization of urea, a formaldehyde aqueous solution with a concentration of 35-45% by weight, and water.
  • the molar ratio of formaldehyde to urea can be 1: (0.5-1), water and
  • the volume ratio of the aqueous formaldehyde solution may be 1: (0.5-2).
  • the refined metolachlor emulsifiable concentrate in step a may contain refined Alachlor, organic solvents and emulsifiers; organic solvents may include one or more of petroleum ether, ethyl acetate, methylene chloride, chloroform, xylene, solvent oil S-150 and solvent oil S-200
  • the emulsifier may include sodium dodecyl sulfate, sodium dodecylbenzenesulfonate, styrene-maleic anhydride copolymer, alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene loss One or more of sorbitan esters, sodium lauryl sulfate, polyvinyl alcohol, and castor oil polyoxyethylene ether; the weight ratio of refined metolachlor, organic solvent
  • the buffer solution in step b may be a buffer solution known to those skilled in the art
  • the buffer pair of the buffer solution may include a citric acid-sodium citrate buffer pair, a citric acid-disodium hydrogen phosphate buffer pair, and an acetic acid-sodium acetate buffer pair
  • the total concentration of the buffer pair in the buffer solution may be 1-5% by weight
  • the pH value of the buffer solution may be 3-5.
  • the acidic pH adjusting agent may include one or more of hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid, and ammonium chloride solution, and the concentration of the acidic pH adjusting agent may be 1-10% by weight.
  • the principle of in-situ polymerization to prepare microcapsule suspension agent encapsulating pesticide active ingredients is to deposit the encapsulating material on the surface of the active ingredient capsule core by changing the conditions, and finally form the microcapsules encapsulating the active ingredient. Under the adjustment of additives, a stable suspension of microcapsules is formed. Therefore, in the preparation process of the microcapsule suspension agent, the type of alkaline regulator, the adjustment time and the final pH value of the system can be selected, which can improve the coating rate, uniformity and capsule tightness of the microcapsule, thereby Further improve the storage stability of microcapsule suspension.
  • the temperature of curing polycondensation may be 40-65°C, and the time of curing polycondensation may be 2-4h; further, the pH of the cured polycondensation product may be adjusted by an alkaline pH adjuster The value is adjusted to neutral; the alkaline pH adjusting agent may be an alkaline pH adjusting agent known to those skilled in the art, preferably, the alkaline pH adjusting agent may be triethylamine, triethanolamine, sodium hydroxide and potassium hydroxide One or more of the solutions, the concentration of the alkaline pH adjuster may be 1-10% by weight; the weight ratio of the fourth material to the first dispersant, the first thickener and the first antifreeze may be 1: ( 0.01-0.2): (0.001-0.02): (0.02-0.15).
  • the fourth material is fine acetolachlor microcapsule suspension agent
  • the first thickener can be a conventional type in the art, such as one or more of xanthan gum, magnesium aluminum silicate, and white carbon black
  • An antifreeze may be a conventional type in the art, for example, one or more of ethylene glycol, propylene glycol, glycerin and urea.
  • the material after curing polycondensation with pH adjusted to neutral and the appropriate amount of auxiliary agent are mixed evenly, which can improve the stability of the suspending agent.
  • the adjuvant may be an adjuvant well known to those skilled in the art that can improve the stability of the suspending agent.
  • the auxiliaries may be the first dispersant, the suspension of fine metolachlor microcapsule suspension, that is, the fourth material and the first The ratio of the weight of the dispersant may be 1: (0.01-2).
  • step e the fourth material obtained in step d is mixed with the atrazine suspending agent, and then a second dispersant is added and mixed uniformly, and the resulting agent can be used as atrazine and refined isoprofen
  • the amine microcapsule suspension-suspending agent is used.
  • an appropriate amount of water can be added to the obtained agent.
  • the weight ratio of the fourth material, atrazine suspension agent and the second dispersant can be 1: (0.5-5) : (0.01-2).
  • the method may further include: before step e, mixing, dispersing, and scrubbing the atrazine original drug, third dispersant, third thickener, third antifreeze, and water in sequence to obtain step e
  • Atrazine suspension agent can exist in the form of suspended particles, the average particle size of suspended particles can be 1-5 ⁇ m;
  • the third thickener can be a conventional type in the art, such as xanthan gum , One or more of magnesium aluminum silicate and white carbon;
  • the first antifreeze may be a conventional type in the art, for example, one or more of ethylene glycol, propylene glycol, glycerin and urea.
  • the first dispersant, the second dispersant, and the third dispersant may each independently include sodium dodecylbenzenesulfonate, sodium methylenebisnaphthalenesulfonate, sodium 1-methylnaphthalenesulfonate formaldehyde Condensate, benzyl naphthalene sulfonate formaldehyde condensate, sodium lignin sulfonate, desugared sodium lignosulfonate, desugared condensed sodium lignin sulfonate, sodium succinate sulfonate, pulverized powder, polycarboxylic acid One or more of salt, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether; the thickener in step d may include aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, One or more of carboxymethyl cellulose, bentonite, and silica, and the antifreeze agent
  • the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate can be stirred uniformly by stirring at a speed of 200-400 rpm, and the stirring time is preferably 30-60 min;
  • the buffer solution can be added to the first material at a speed of 0.5-1h at 25-35°C, and then it can be stirred at a speed of 200-500r/min to achieve uniform stirring;
  • step c it can be -35°C, add the acidic pH adjuster to the second material evenly within 0.5-1h, and then stir at 200-500r/min to achieve uniform stirring; in step d, it can be 200-300r/ Stirring at a speed of min achieves uniform
  • the second aspect of the present disclosure to provide a microcapsule suspension-suspending agent containing atrazine and mesochlor which is prepared by the method of the first aspect of the present disclosure.
  • the microcapsule suspension-suspension agent containing atrazine and mesoprofen provided by the present disclosure can be applied to the control of grasses and broad-leaved weeds before crop seedlings.
  • refined metolachlor was purchased from Zhejiang Heben Technology Co., Ltd.
  • solvent oil S-200 was purchased from Jiangsu Hualun Chemical Co., Ltd.
  • polyoxyethylene sorbitan monohydrate Stearic acid ester was purchased from Nanjing Taihua Chemical Co., Ltd.
  • sorbitan monostearate polyoxyethylene ether was purchased from Nanjing Taihua Chemical Co., Ltd.
  • acetic acid-sodium acetate buffer solution was purchased from Beijing Chemical Reagent Company
  • polycarboxyl The acid salt was purchased from Heda Chemicals (Shanghai) Co., Ltd.
  • the aluminum magnesium silicate was purchased from Zhejiang Fenghong New Material Co., Ltd.
  • the ethylene glycol was purchased from Beijing Chemical Reagent Company
  • Atrazine was purchased from Zhejiang Zhongshan Chemical Group Co., Ltd.
  • sodium lauryl sulfate was purchased from Beijing Chemical Reagent Company
  • sodium methylenebisnaphthalene sulfonate was purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.
  • silicone defoamer was purchased from Meitu High-tech Materials Group
  • Xanthan Gum It was purchased from Zhejiang Fenghong New Materials Co., Ltd.
  • sodium benzoate was purchased from Beijing Chemical Reagent Company
  • fatty alcohol polyoxyethylene ether was purchased from Nanjing Taihua Chemical Co., Ltd., and the rest were commercial reagents.
  • urea with a 40% by weight formaldehyde aqueous solution uniformly, and react at pH 8 and a temperature of 70°C for 1.5 hours; add water to dilute it to obtain an aqueous solution of urea-formaldehyde resin prepolymer.
  • the molar ratio is 1:0.5, and the volume ratio of water and formaldehyde aqueous solution is 1:1.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:1.5
  • adding an acetic acid-sodium acetate buffer solution with a pH value of 4.5 and a total buffer pair concentration of 1.5% by weight to the above first material evenly within 1 hour, stirring at 300 rpm Mix well at a speed to adjust the pH to 5.5 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 3% by weight to the above second material at a uniform rate within 1 hour, stirring at 300 rpm Mix the speed uniformly to adjust the pH value to 4 to obtain the third material; under the condition of 45 °C, the third material is cured and polycondensed for 3 hours to obtain the material after cu
  • Atrazine 50% by weight of atrazine, 0.5% by weight of sodium lauryl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 39% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand grinding, and the sand is ground to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • the resulting agent can be used as atrazine and refined propofol Microcapsule suspension of amines-suspending agent.
  • the weight ratio of fine metolachlor microcapsule suspension agent to atrazine suspension agent and fatty alcohol polyoxyethylene ether is 1:1:0.05.
  • urea with a 40% by weight formaldehyde aqueous solution uniformly, and react at pH 8 and a temperature of 70°C for 1.5 hours; add water to dilute it to obtain an aqueous solution of urea-formaldehyde resin prepolymer.
  • the molar ratio is 1:0.5, and the volume ratio of water and formaldehyde aqueous solution is 1:1.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:1.5
  • adding an acetic acid-sodium acetate buffer solution with a pH value of 4.5 and a total buffer pair concentration of 1.5% by weight to the above first material evenly within 1 hour, stirring at 300 rpm Mix well at a speed to adjust the pH to 5.5 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 3% by weight to the above second material at a uniform rate within 1 hour, stirring at 300 rpm Mix the speed uniformly to adjust the pH value to 4 to obtain the third material; under the condition of 45 °C, the third material is cured and polycondensed for 3 hours to obtain the material after cu
  • Atrazine 50% by weight of atrazine, 0.5% by weight of sodium lauryl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 39% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand grinding, and the sand is ground to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • the resulting agent can be used as atrazine and refined propofol Microcapsule suspension of amines-suspending agent.
  • the weight ratio of the fine metolachlor microcapsule suspension agent to the atrazine suspension agent and fatty alcohol polyoxyethylene ether is 1:3:0.03.
  • urea with a 40% by weight formaldehyde aqueous solution uniformly, and react at pH 8 and a temperature of 70°C for 1.5 hours; add water to dilute it to obtain an aqueous solution of urea-formaldehyde resin prepolymer.
  • the molar ratio is 1:0.5, and the volume ratio of water and formaldehyde aqueous solution is 1:1.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:1.5
  • adding an acetic acid-sodium acetate buffer solution with a pH value of 4.5 and a total buffer pair concentration of 1.5% by weight to the above first material evenly within 1 hour, stirring at 300 rpm Mix well at a speed to adjust the pH to 5.5 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 3% by weight to the above second material at a uniform rate within 1 hour, stirring at 300 rpm Mix the speed uniformly to adjust the pH value to 4 to obtain the third material; under the condition of 45 °C, the third material is cured and polycondensed for 3 hours to obtain the material after cu
  • Atrazine 50% by weight of atrazine, 0.5% by weight of sodium lauryl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 39% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand grinding, and the sand is ground to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • the resulting agent can be used as atrazine and refined propofol Microcapsule suspension of amines-suspending agent.
  • the weight ratio of fine metolachlor microcapsule suspension agent to atrazine suspension agent and fatty alcohol polyoxyethylene ether is 1:1:0.05.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:1 ;
  • a first material wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:1 ;
  • Add an acetic acid-sodium acetate buffer solution with a pH value of 3.0 and a total buffer pair concentration of 2% by weight and add it to the above first material at a uniform rate within 0.5 hours, stirring at 500 rpm Mix at a uniform speed to adjust the pH to 6.5 to obtain a second material;
  • hydrochloric acid with a concentration of 5 wt% to the second material at a uniform rate within
  • Atrazine 50% by weight of atrazine, 0.5% by weight of sodium lauryl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 39% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand grinding, and the sand is ground to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • microcapsule suspension of acetolachlor and atrazine suspension are mixed, and then the polycarboxylate is added, and the mixture is stirred evenly.
  • the resulting agent can be used as a solution containing atrazine and acetolachlor.
  • Microcapsule suspension-use of suspending agent wherein, the weight ratio of the fine metolachlor microcapsule suspension agent, the atrazine suspension agent, and the polycarboxylate is 1:0.5:0.1.
  • the refined metolachlor, solvent oil S-150 and castor oil polyoxyethylene ether are mixed uniformly to obtain refined metolachlor emulsifiable concentrate, in which refined metolachlor is combined with solvent oil S-150 and castor oil
  • the weight ratio of oxyethylene ether is 1:1:0.05.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are uniformly mixed to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:2
  • the pH value is 5.0
  • the total concentration of the buffer pair is 1% by weight of acetic acid-sodium acetate buffer solution, which is added to the first material evenly within 1 hour, and stirred at 400 rpm Mix at a uniform speed to adjust the pH to 5.5 to obtain a second material; at room temperature, add hydrochloric acid with a concentration of 8% by weight to the second material at a uniform rate within 0.5 hours, stirring at 500 rpm Mix the speed uniformly to adjust the pH value to 2.5 to obtain the third material; under the condition of 50 °C, the third material is cured and polycondensed for 4 hours to obtain the material
  • Atrazine 50% by weight of atrazine, 1% by weight of sodium lauryl sulfate, 2% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylene dioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 39.5% by weight of water are thoroughly mixed and dispersed, and after uniform dispersion, they are passed into a sand mill for sand grinding, and the sand is ground to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • the obtained medicine can be used as atrazine and refined isopropyl
  • the microcapsule suspension-suspending agent of alachlor the weight ratio of fine metolachlor microcapsule suspension agent, atrazine suspension agent, and sodium methylenebisnaphthalene sulfonate is 1:2:0.05.
  • acetolachlor, ethyl acetate and sodium dodecylbenzene sulfonate uniformly to obtain acetolachlor emulsifiable concentrate.
  • acetolachlor and ethyl acetate and dodecylbenzene The weight ratio of sodium sulfonate is 1:0.5:0.05.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:0.5 ;
  • At room temperature add an acetic acid-sodium acetate buffer solution with a pH of 4.5 and a total concentration of 2% by weight to the first material within 1 hour, stirring at 200 rpm Mix uniformly at a rate to adjust the pH to 6.2 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 5% by weight to the second material at a uniform rate within 0.5 hours, stirring at 400 rpm Mix the speed uniformly to adjust the pH value to 3.2 to obtain the third material; at 60 °C, the third material is cured and polycondensed for 2 hours to obtain the material after curing
  • Atrazine suspension 50% by weight of atrazine, 0.5% by weight of powder, 3% by weight of sodium methylenebisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylene glycol, 0.3 Xanthan gum by weight, 0.2% by weight sodium benzoate and 39% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, it is passed into a sand mill for sand milling, and the sand is milled to a suspension with an average particle size of less than 5 microns to obtain Atrazine suspension.
  • the obtained agent can be used as atrazine and Microcapsule suspension-suspending agent of acetolachlor.
  • the weight ratio of fine metolachlor microcapsule suspension agent to atrazine suspension agent and 1-methylnaphthalene sulfonate sodium formaldehyde condensate is 1:3:0.15.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:2 ;
  • adding an acetic acid-sodium acetate buffer solution with a pH of 4.5 and a total concentration of 2% by weight to the first material within 1 hour, stirring at 300 rpm Mix uniformly at a speed to adjust the pH to 5.5 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 5% by weight to the second material at a uniform rate within 0.5 hours, stirring at 200 rpm Mix the speed uniformly to adjust the pH value to 4.0 to obtain the third material; under the condition of 45 °C, the third material is cured and polycondensed for 2 hours to obtain the material after curing polycon
  • Atrazine 50% by weight of atrazine, 0.5% by weight of sodium lauryl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 39% by weight of water are thoroughly mixed and dispersed. After being evenly dispersed, they are passed into a sand mill for sand grinding, and the sand is ground to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • the obtained medicine can be used as atrazine and refined isopropyl methyl Microcapsule suspension of glufosinate-suspending agent.
  • the weight ratio of fine metolachlor microcapsule suspension agent, atrazine suspension agent, and desugared lignosulfonate sodium is 1:5:0.05.
  • urea with a 35 wt% formaldehyde aqueous solution uniformly, and react at pH 8 and temperature 70°C for 1.5h; add water to dilute to obtain an aqueous solution of urea-formaldehyde resin prepolymer.
  • the molar ratio is 1:0.5, and the volume ratio of water to formaldehyde aqueous solution is 1:2.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:1
  • adding an acetic acid-sodium acetate buffer solution with a pH of 4.5 and a total buffer pair concentration of 2% by weight to the first material in 0.5 hours, stirring at 300 rpm Mix uniformly at a rate to adjust the pH to 6.2 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 5% by weight to the second material evenly within 1.5 hours, stirring at 500 rpm Mix the speed uniformly to adjust the pH value to 3.2 to obtain the third material; at 60 °C, the third material is cured and polycondensed for 2 hours to obtain the material after curing and polycondensation; and the
  • Atrazine 0.5% by weight of sodium dodecyl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 57% by weight of water are fully mixed and dispersed. After being evenly dispersed, pass into a sand mill for sand milling. The sand is milled to a suspension with an average particle size of less than 5 microns. Liquid to obtain atrazine suspension.
  • the obtained agent can be used as atrazine and refined isopropyl methyl Microcapsule suspension of glufosinate-suspending agent.
  • the weight ratio of the fine metolachlor microcapsule suspension agent, the atrazine suspension agent, and the sodium succinate sulfonate is 1:4:0.01.
  • urea with 40% by weight formaldehyde aqueous solution uniformly, react at pH 9 and temperature 65°C for 1 hour; dilute with water to obtain urea-formaldehyde resin prepolymer aqueous solution, in which the mole of formaldehyde and urea The ratio is 1:0.5, and the volume ratio of water and formaldehyde aqueous solution is 1:2.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:2 ;
  • adding an acetic acid-sodium acetate buffer solution with a pH of 4.5 and a total concentration of 2% by weight to the first material within 1 hour, stirring at 200 rpm Mix at a uniform speed to adjust the pH to 6.2 to obtain a second material;
  • at room temperature add hydrochloric acid with a concentration of 5% by weight to the second material evenly within 1 hour, stirring at 500 rpm Mix the speed uniformly to adjust the pH value to 3.2 to obtain the third material;
  • the third material is subjected to curing and polycondensation for 2 hours to obtain the material after curing and polycondensation
  • Atrazine 0.5% by weight of sodium dodecyl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 57% by weight of water are fully mixed and dispersed. After being evenly dispersed, pass into a sand mill for sand milling. The sand is milled to a suspension with an average particle size of less than 5 microns Liquid to obtain atrazine suspension.
  • the obtained medicament can be used as micro-containing atrazine and refined metolachlor Capsule suspension-suspending agent used.
  • the weight ratio of fine metolachlor microcapsule suspension, atrazine suspension, and split powder is 1:0.8:0.02.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:2 ;
  • a citric acid-sodium citrate buffer solution with a pH of 3.6 and a total buffer pair concentration of 4% by weight to the above first material at a uniform rate within 0.5 hours at 400 rpm
  • the mixing speed is evenly mixed to adjust the pH to 6.2 to obtain a second material; under room temperature conditions, phosphoric acid with a concentration of 4% by weight is added to the above second material at a uniform speed within 0.5 hours at 200 rpm
  • the mixing speed is evenly mixed to adjust the pH value to 2.5 to obtain the third material; at 60 °C, the third material is cured and polycondensed for 4 hours to obtain the material after
  • Atrazine 0.5% by weight of sodium dodecyl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 57% by weight of water are fully mixed and dispersed. After being evenly dispersed, pass into a sand mill for sand milling. The sand is milled to a suspension with an average particle size of less than 5 microns. Liquid to obtain atrazine suspension.
  • the resulting agent can be used as atrazine and refined isopropyl methyl Microcapsule suspension of glufosinate-suspending agent.
  • the weight ratio of fine metolachlor microcapsule suspension agent, atrazine suspension agent and nonylphenol polyoxyethylene ether is 1:1.2:0.05.
  • urea with a 35 wt% formaldehyde aqueous solution uniformly, and react at pH 8 and temperature 70°C for 1.5h; add water to dilute to obtain an aqueous solution of urea-formaldehyde resin prepolymer.
  • the molar ratio is 1:0.5, and the volume ratio of water to formaldehyde aqueous solution is 1:2.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:0.5
  • a buffer solution of citric acid-dibasic sodium phosphate with a pH of 4.0 and a total buffer pair concentration of 4% by weight to the first material at a constant speed within 1 hour at 400 rpm.
  • Atrazine 0.5% by weight of sodium dodecyl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 57% by weight of water are fully mixed and dispersed. After being evenly dispersed, pass into a sand mill for sand milling. The sand is milled to a suspension with an average particle size of less than 5 microns Liquid to obtain atrazine suspension.
  • the obtained medicine can be used as atrazine and refined metolachlor
  • the microcapsule suspension-suspending agent is used. Among them, the weight ratio of fine metolachlor microcapsule suspension agent, atrazine suspension agent, and sodium lignosulfonate is 1:1.5:0.04.
  • Example 1 According to the preparation method in Example 1, an aqueous solution of urea-formaldehyde resin prepolymer and refined metolachlor emulsifiable concentrate were prepared.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:4 ;
  • the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:4 ;
  • Add phosphoric acid with a concentration of 5% by weight to the first material at a uniform rate within 2 hours, mix evenly at a stirring speed of 500 rpm to adjust the pH to 3.2, and obtain a second material ;
  • the second material is cured by polycondensation for 2 hours to obtain a cured polycondensation product, and the pH value of the cured polycondensation product is adjusted to 7;
  • Atrazine 0.5% by weight of sodium dodecyl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 57% by weight of water are fully mixed and dispersed. After being evenly dispersed, pass into a sand mill for sand milling. The sand is milled to a suspension with an average particle size of less than 5 microns. Liquid to obtain atrazine suspension.
  • the suspension of refined metolachlor microcapsules with atrazine suspension, then add sodium lignin sulfonate, and mix well.
  • the obtained medicine can be used as atrazine and refined metolachlor
  • the microcapsule suspension-suspending agent is used. Among them, the weight ratio of the fine metolachlor microcapsule suspension agent to the atrazine suspension agent and sodium lignosulfonate is 1:0.3:0.05.
  • Example 1 According to the preparation method in Example 1, an aqueous solution of urea-formaldehyde resin prepolymer and refined metolachlor emulsifiable concentrate were prepared.
  • the obtained urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate are mixed uniformly to obtain a first material, wherein the weight ratio of the urea-formaldehyde resin prepolymer aqueous solution and refined metolachlor emulsifiable concentrate is 1:4 ;
  • an acetic acid-sodium acetate buffer solution with a pH value of 4.5 and a total concentration of 2% by weight to the first material within 1 hour, stirring at 500 rpm Mix uniformly at a speed to adjust the pH to 6.5 to obtain a second material; at 60°C, cure the second material for 2.5 hours to obtain a cured polycondensation product, and adjust the pH of the cured polycondensation product To 7; add sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol and mix well to obtain a suspension of refined metolachlor microcapsules, in which the
  • Atrazine 0.5% by weight of sodium dodecyl sulfate, 3% by weight of sodium methylene bisnaphthalene sulfonate, 2% by weight of silicone defoamer, 5% by weight of ethylenedioxide Alcohol, 0.3% by weight of xanthan gum, 0.2% by weight of sodium benzoate and 57% by weight of water are fully mixed and dispersed. After being evenly dispersed, pass into a sand mill for sand milling. The sand is milled to an average particle size of less than 5 microns in suspension Liquid to obtain atrazine suspension.
  • the obtained medicine can be used as atrazine and refined metolachlor
  • the microcapsule suspension-suspending agent is used. Among them, the weight ratio of fine metolachlor microcapsule suspension agent, atrazine suspension agent, and sodium lignosulfonate is 1:0.5:0.05.
  • Example 1 an agent that can be used as a microcapsule suspension-suspension agent containing atrazine and mesochlor is prepared, except that the pH of the third material is 2.0.
  • Example 1 an agent that can be used as a microcapsule suspension-suspending agent containing atrazine and mesochlor is prepared, except that the pH of the third material is 9.
  • Example 1 The raw materials in Example 1 are used, except that refined metolachlor, solvent oil S-200, and sorbitan monostearate polyoxyethylene ether and water are mixed uniformly to obtain refined metolachlor water Emulsion, mixed with atrazine suspending agent to form a suspoemulsion, in which the weight ratio of acetolachlor, solvent oil S-200, sorbitan monostearate polyoxyethylene ether, water is 1: 4:0.06:6, the weight ratio of refined metolachlor aqueous emulsion to atrazine suspension is 1:1.
  • Example 1 The raw materials and preparation method of Example 1 are used, with the difference that no atrazine suspending agent is added.
  • Example 1 The raw materials and preparation method of Example 1 were used, with the difference that no spermethram suspension was added.
  • This test example is used to test the heat storage stability and thermal stability of the microcapsule suspension-suspending agent containing atrazine and mesoprofen obtained in Example 1-11 and the corresponding agent obtained in Comparative Example 1-7. Low temperature stability.
  • Example 1 Good fluidity, no layering and agglomeration, suspension rate is 97.3% Good fluidity, no layering and agglomeration, suspension rate is 97.9%
  • Example 2 Good fluidity, 5% water analysis, no agglomeration, 92.5% suspension rate Good fluidity, no layering and agglomeration, suspension rate is 93.4%
  • Example 3 Good fluidity, 3% water separation, no lumps, 94.6% suspension rate Good fluidity, no layering and agglomeration, suspension rate is 94.7%
  • Example 4 Good fluidity, no layering and agglomeration, suspension rate is 96.9% Good fluidity, no layering and agglomeration, suspension rate is 97.0%
  • Example 5 Good fluidity, no layering and agglomeration, suspension rate is 96.4% Good fluidity, no layering and agglomeration, suspension rate is 96.2%
  • Example 6 Good fluidity, no layering and agglomeration, suspension rate is 96.6% Good fluid
  • microcapsule suspension-suspending agent containing atrazine and mesochlor obtained by the preparation method provided by the present invention has good thermal storage stability and low-temperature storage stability.
  • the microcapsule suspension-suspending agent containing atrazine and mesochlor obtained in Examples 1-11 and the corresponding agents obtained in Comparative Examples 1-7 were Test the control effect.
  • a second dilution was performed, and the medicaments of Examples 1-11 and Comparative Examples 1-7 were prepared as medicinal solutions according to the concentration of mesochlor-atrazine at 10% by weight, respectively.
  • Test location Nanning City, Guangxi province. The land is flat and has good fertility. The corn in each treatment area after application is managed according to conventional production.
  • the specific steps include using a knapsack sprayer and suspending and suspending the fine metolachlor-atrazine microcapsules obtained in Examples 1-11 and Comparative Examples 1-7 according to the application liquid amount of 30 kg/mu.
  • the medicinal solution was sprayed evenly on the corn fields of each planting area before sowing after seedling, and a water control was set.
  • the preparation method provided by the present disclosure utilizes a specific combination of buffer solution and acidic pH adjuster, adjusts the acidity of the reaction system step by step, corresponding rotation speed, selects corresponding emulsifiers, solvents and other specific reaction conditions
  • the medicament can be used as a microcapsule suspension-suspending agent containing atrazine and mesochlor, which can achieve the effect of slow-release and long-term control of crop pests.
  • microcapsule suspension-suspension agent containing atrazine and mesochlor in the present disclosure has the characteristics of long duration of maintenance compared with other formulations of mesochlor and atrazine, which can be reduced
  • the number of medications and the amount of medications are used to save costs; there are few organic solvents in it, which can reduce the pollution to the environment.
  • the embodiment of the present invention provides a method for preparing a microcapsule suspension-suspending agent containing atrazine and mesochlor and its microcapsule suspension-suspending agent.
  • the method includes: a. The urea-formaldehyde The aqueous solution of resin prepolymer and refined metolachlor emulsifiable concentrate are mixed in a weight ratio of 1: (0.5-2) to obtain a first material; b. The pH value of the first material is adjusted to 5.0-6.5 to obtain a second Materials; c. Adjust the pH of the second material to 2.5-4.5 to obtain a third material; d.
  • the dispersant, thickener and antifreeze are mixed uniformly to obtain the fourth material; e, the fourth material is mixed with the atrazine suspending agent, and then the second dispersant is added and mixed evenly;
  • the microcapsule suspension-suspension of Jinhejing metolachlor significantly improved the storage stability and the control effect of weeds of the microcapsule suspension-suspension containing atrazine and mesochlor.

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Abstract

一种制备含有阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的方法及其微囊悬浮-悬浮剂，该方法包括：a、将尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油按照重量比为1：(0.5-2)混合，得到第一物料；b、调整所述第一物料的pH值为5.0-6.5，得到第二物料；c、调整所述第二物料的pH值为2.5-4.5，得到第三物料；d、第三物料进行固化缩聚，然后将固化缩聚后的物料的pH值调节至中性后与第一分散剂、增稠剂和防冻剂混合均匀，得到第四物料；e、第四物料与阿特拉津悬浮剂混合后加入第二分散剂并混合均匀。该制备方法显著提高了含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的贮存稳定性和对杂草的防治效果。

Description

一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂及其制备方法
交叉引用
本发明要求在中国专利局提交的、申请号为201811446732.8、发明名称为“一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂及其制备方法”的中国专利申请的优先权，该申请的全部内容通过引用结合在本发明中。
技术领域
本发明涉及农药技术领域，具体地，涉及一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂及其制备方法。
背景技术
精异丙甲草胺是先正达公司开发的乙酰胺类选择性除草剂，是在异丙甲草胺的基础上，利用先进工艺成功去除非活性R-体，而得到的精制的活性S-体。精异丙甲草胺除具有异丙甲草胺的优点外，在安全性和防治效果上比异丙甲草胺更胜一筹，同时，根据毒理学研究结果，其毒性要比异丙甲草胺低，甚至只有后者毒性的十分之一。精异丙甲草胺适用作物谱广，且是世界重要粮食作物玉米、大豆的主要除草剂。
目前市场上精异丙甲草胺以乳油为主，大量有机溶剂的使用及释放，不仅有害于生态环境及使用者，而且很容易发生药害，影响作物的健康生长及产量的保证。
发明内容
为了克服上述缺陷，本公开提供一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的制备方法，由该方法得到的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂既速效又持效且能够有效防治农作物多种杂草。
为了实现上述目的，本公开第一方面：提供一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的制备方法，其中，该方法包括以下步骤：a、将尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油按照重量比为1：(0.5-2)混合均匀，得到第一物料；b、将步骤a中得到的第一物料与缓冲溶液混合均匀，调整所述第一物料的pH值为5.0-6.5，得到第二物料； c、将步骤b中得到的所述第二物料与酸性pH值调节剂混合均匀，调整所述第二物料的pH值为2.5-4.5，得到第三物料；d、将步骤c中得到的所述第三物料进行固化缩聚，得到固化缩聚后的物料，然后将所述固化缩聚后的物料的pH值调节至中性后与第一分散剂、增稠剂和防冻剂混合均匀，得到第四物料；e、将步骤d中得到的所述第四物料与阿特拉津悬浮剂混合后加入第二分散剂并混合均匀。
可选地，该方法还包括：步骤a中的所述尿素-甲醛树脂预聚体水溶液为将尿素、甲醛和水进行预聚合得到的；所述预聚合的条件包括：pH值为8-9，温度为65-75℃，时间为1-2h。
可选地，该方法还包括：步骤a中的所述精异丙甲草胺乳油含有精异丙甲草胺、有机溶剂和乳化剂；所述有机溶剂包括石油醚、乙酸乙酯、二氯甲烷、三氯甲烷、二甲苯、溶剂油S-150和溶剂油S-200中的一种或多种，所述乳化剂包括十二烷基硫酸钠、十二烷基苯磺酸钠、苯乙烯-马来酸酐共聚物、烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、聚氧乙烯失水山梨醇酯类、月桂醇硫酸钠、聚乙烯醇和蓖麻油聚氧乙烯醚中的一种或多种；所述精异丙甲草胺、所述有机溶剂和所述乳化剂的重量比为1：(0.1-1)：(0.05-0.2)。
可选地，步骤b中的所述缓冲溶液含有缓冲对，所述缓冲对包括柠檬酸-柠檬酸钠、柠檬酸-磷酸氢二钠和乙酸-乙酸钠中的一种或多种，所述缓冲溶液中缓冲对的总浓度为1-5重量％，所述缓冲溶液的pH值为3-5。
可选地，步骤d中，步骤c中的所述酸性pH值调节剂包括盐酸、硫酸、磷酸、乙酸和氯化铵溶液中的一种或多种，所述酸性pH值调节剂的浓度为1-10重量％。
可选地，步骤d中，所述固化缩聚的温度为40-65℃、时间为2-4h；该方法包括：通过碱性pH调节剂将所述固化缩聚后的物料的pH值调节至中性，所述碱性pH调节剂包括三乙胺、三乙醇胺、氢氧化钠、氢氧化钾溶液中的一种或多种；所述第四物料、所述第一分散剂、所述第一增稠剂和所述第一防冻剂的重量比为1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15)。
可选地，步骤e中，所述第四物料、所述阿特拉津悬浮剂和所述第二分散剂的重量比为1：(0.5-5)：(0.01-0.2)。
可选地，该方法还包括：在步骤e之前，将阿特拉津原药、第三分散剂、第三增稠剂、第三防冻剂和水混合、分散和磨砂，得到步骤e中的所述阿特拉津悬浮剂，所述阿特拉津悬浮剂为平均粒径为1-5μm的悬浮微粒。
可选地，步骤a中的所述混合的条件包括：搅拌速度为200-400r/min，搅拌时间为30-60min；步骤b包括，在25-35℃下，在0.5-1h内将所述缓冲溶液匀速加入所述第一物料中，并以200-500r/min的转速搅拌混合均匀；步骤c包括，在25-35℃下，在0.5-1h内将所述酸性pH调节剂匀速加入所述第二物料中，并以200-500r/min的转速搅拌混合均匀；步骤d中的所述混合的条件包括：搅拌速度为200-300r/min，搅拌时间为1-3h；步骤e中的所述混合的条件包括：搅拌速度为200-400r/min，搅拌时间为30-60分钟。
本公开第二方面：提供本公开第一方面的方法制备的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂。
通过上述技术方案，本公开的制备方法显著提高了含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的贮存稳定性和对农田杂草的防治效果，采用该方法制备的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂能够既速效又持效且能够有效防治农作物多种杂草。
本公开的其他特征和优点将在随后的具体实施方式部分予以详细说明。
具体实施方式
以下对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本公开，并不用于限制本公开。
本公开第一方面：提供一种含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的制备方法，其中，该方法包括以下步骤：a、按照重量比为1：(0.5-2)将尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料；b、通过向步骤a得到的第一物料中加入缓冲溶液并混合均匀，调整第一物料的pH值为5.0-6.5，得到第二物料；c、通过向步骤b得到的第二物料中加入酸性pH值调节剂并混合均匀，调整第二物料的pH值为2.5-4.5，得到第三物料；d、将步骤c得到的第三物料进行固化缩聚，得到固化缩聚后的物料，然后将固化缩聚后的物料的pH值调节至中性后与第一分散剂、 增稠剂和防冻剂混合均匀，得到第四物料；e、将步骤d得到的第四物料与阿特拉津悬浮剂混合后加入第二分散剂并混合均匀。
本公开中，精异丙甲草胺为乙酰胺类除草剂，具有氯乙酰胺结构，为细胞分裂抑制剂，通过抑制长链脂肪酸的合成从而影响细胞生长。中文通用名称：精异丙甲草胺，英文通用名称：s-metolachlor，化学名称：(aRS,1S)-2-氯-6'-乙基-N-(2-甲氧基-1-甲基乙基)乙酰邻甲苯胺，分子式C 15H 22ClNO 2，相对分子量：283.8，CAS NO.178961-20-1，其结构式如式(1)所示。
Figure PCTCN2019113602-appb-000001
阿特拉津又名莠去津，化学名称为6-氯-N-乙基-N′-(1-甲基乙基)-1,3,5-三氮苯-2,4二胺,英文名Atrazine，英文化学名称为6-chloro-N-ethyl-N′-(1-methylethyl)-1,3,5-Triazine-2,4-diamine,分子式C 8H 14ClN 5,CAS NO.1912-24-9，其结构式如式(2)所示。
Figure PCTCN2019113602-appb-000002
根据本公开，该方法还可以包括：步骤a中的尿素-甲醛树脂预聚体水溶液为将尿素、甲醛和水进行预聚合得到的；预聚合的条件包括：pH值为8-9，温度为65-75℃，时间为1-2h。
尿素-甲醛树脂预聚体水溶液的制备方法可以为本领域技术人员公知的制备方法，本发明对其没有特别的限制；尿素-甲醛树脂预聚体水溶液可以由含有尿素、甲醛和水的原料液预聚合得到；尿素-甲醛树脂预聚体水溶液可以由尿素、浓度为35-45重量％的甲醛水溶液和水预聚合得到，甲醛和尿素的摩尔比可以为1：(0.5-1)，水和甲醛水溶液的体积比可以为1：(0.5-2)。
根据本公开，为进一步改善微胶囊悬浮剂中微胶囊的粒径分布以及包覆率，从而进一步提高微胶囊悬浮剂的贮存稳定性，步骤a中的精异丙甲草胺乳油可以含有精异丙甲草胺、有机溶剂和乳化剂；有机溶剂可以包括石油 醚、乙酸乙酯、二氯甲烷、三氯甲烷、二甲苯、溶剂油S-150和溶剂油S-200中的一种或多种，乳化剂可以包括十二烷基硫酸钠、十二烷基苯磺酸钠、苯乙烯-马来酸酐共聚物、烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、聚氧乙烯失水山梨醇酯类、月桂醇硫酸钠、聚乙烯醇和蓖麻油聚氧乙烯醚中的一种或多种；精异丙甲草胺、有机溶剂和乳化剂的重量比可以为1：(0.1-1)：(0.05-0.2)。精异丙甲草胺乳油的制备方法可以为本领域技术人员公知的制备方法，本发明对其没有特别的限制。
根据本公开，步骤b中缓冲溶液可以为本领域技术人员公知的缓冲溶液，缓冲溶液的缓冲对可包括柠檬酸-柠檬酸钠缓冲对、柠檬酸-磷酸氢二钠缓冲对和乙酸-乙酸钠缓冲对中的一种或多种，缓冲溶液中缓冲对的总浓度可为1-5重量％，缓冲溶液的pH值可以为3-5。
根据本公开，步骤c中，酸性pH值调节剂可以包括盐酸、硫酸、磷酸、乙酸和氯化铵溶液中的一种或多种，酸性pH值调节剂的浓度可以为1-10重量％。
根据本公开，原位聚合法制备包裹农药活性成分的微胶囊悬浮剂的原理是通过改变条件使成囊材料沉积在活性成分囊芯表面，最终形成包裹活性成分的微胶囊，并在适当适量的助剂调节下，形成稳定的微胶囊悬浮剂。因此，在微胶囊悬浮剂制备过程中，可以选择适当的碱性调节剂的种类、调节时间以及体系最终的pH值，能够提高微胶囊的包覆率、均匀度以及囊壳紧致性，从而进一步提高微胶囊悬浮剂的贮存稳定性。在一种优选的实施方式中，步骤d中，固化缩聚的温度可以为40-65℃、固化缩聚的时间可以为2-4h；进一步地，可以通过碱性pH调节剂将固化缩聚产物的pH值调节至中性；碱性pH调节剂可以为本领域技术人员公知的碱性pH调节剂，优选情况下，碱性pH调节剂可以为三乙胺、三乙醇胺、氢氧化钠和氢氧化钾溶液中一种或多种，碱性pH调节剂的浓度可以为1-10重量％；第四物料与第一分散剂、第一增稠剂和第一防冻剂的重量比可以为1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15)。第四物料即为精异丙甲草胺微胶囊悬浮剂；第一增稠剂可以为本领域常规种类，例如为黄原胶、硅酸镁铝和白炭黑的一种或多种；第一防冻剂可以为本领域常规种类，例如为乙二醇、丙二醇、丙三醇和尿素的一种或多种。
根据本公开，微胶囊成囊后，由于后续反应、重力、交联大分子树脂间的相互作用等因素，会出现微胶囊聚集、沉淀、板结等现象，为了进一步提 高微胶囊悬浮剂的稳定性，将pH调节至中性的固化缩聚后的物料和适当适量的助剂混合均匀，可以提高悬浮剂的稳定性。助剂可以为本领域技术人员熟知的能够提高悬浮剂稳定性的助剂，优选情况下，助剂可为第一分散剂，精异丙甲草胺微胶囊悬浮剂即第四物料与第一分散剂的重量的比值可以为1：(0.01-2)。
根据本公开，步骤e中，将步骤d得到的第四物料与阿特拉津悬浮剂混合后加入第二分散剂并混合均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用，使用时可以向得到的药剂中加入适量的水，第四物料、阿特拉津悬浮剂与第二分散剂的重量比可以为1：(0.5-5)：(0.01-2)。
根据本公开，该方法还可包括：在步骤e之前，将阿特拉津原药、第三分散剂、第三增稠剂、第三防冻剂和水依次混合、分散和磨砂，得到步骤e中的阿特拉津悬浮剂，阿特拉津悬浮剂可以以悬浮微粒形式存在，悬浮微粒的平均粒径可为1-5μm；第三增稠剂可以为本领域常规种类，例如为黄原胶、硅酸镁铝和白炭黑的一种或多种；第一防冻剂可以为本领域常规种类，例如为乙二醇、丙二醇、丙三醇和尿素的一种或多种。
根据本公开，第一分散剂、第二分散剂和第三分散剂可以各自独立地包括十二烷基苯磺酸钠、亚甲基双萘磺酸钠、1-甲基萘磺酸钠甲醛缩合物、苄基萘磺酸甲醛缩合物、木质素磺酸钠、脱糖木质素磺酸钠、脱糖缩合木质素磺酸钠、丁二酸酯磺酸钠、拉开粉、聚羧酸盐、壬基酚聚氧乙烯醚和脂肪醇聚氧乙烯醚中的一种或多种；步骤d中增稠剂可以包括硅酸铝镁、黄原胶、聚乙二醇、聚乙烯醇、羧甲基纤维素、膨润土和白炭黑中的一种或多种，防冻剂可以包括乙二醇、1,2-丙二醇、丙三醇和尿素中的一种或多种。
根据本公开，适当的反应条件能够提高精异丙甲草胺微胶囊的包覆率、改善粒径分布以及囊壳的厚度，进而提高微胶囊悬浮剂的贮存稳定性。优选地，步骤a中，尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油可通过在200-400转/分钟的速度下搅拌实现搅拌均匀，搅拌时间优选为30-60min；步骤b中，可在25-35℃下，在0.5-1h内将缓冲溶液匀速地加入至第一物料中，然后可以在200-500r/min的速度下搅拌实现搅拌均匀；步骤c中，可以在25-35℃，在0.5-1h内将酸性pH值调节剂匀速地加入至第二物料中，然后可以在200-500r/min的速度下搅拌实现搅拌均匀；步骤d中，可以在200-300r/min的速度下搅拌实现搅拌均匀，搅拌时间优选为1-3h；步骤e中，可 以在200-400r/min的速度下搅拌实现搅拌均匀，搅拌时间优选为30-60分钟。其中，匀速加入是指在加入的过程中，单位时间内的加入量基本相同。
本公开第二方面：提供本公开第一方面的方法制备的含有阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂。本公开提供的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂能够应用于作物苗前防治禾本科及阔叶杂草。
以下通过实施例进行进一步详细说明本公开，并不用于限制本公开。
在本公开的下述实施例和对比例中，精异丙甲草胺购自浙江禾本科技有限公司，溶剂油S-200购自江苏华伦化工有限公司，聚氧乙烯失水山梨醇单硬脂酸酯购自南京太化化工有限公司，失水山梨醇单硬脂酸酯聚氧乙烯醚购自南京太化化工有限公司，乙酸-乙酸钠缓冲溶液购自北京化学试剂公司，聚羧酸盐购自禾大化学品(上海)有限公司，硅酸铝镁购自浙江丰虹新材料股份有限公司，乙二醇购自北京化学试剂公司，阿特拉津购自浙江中山化工集团股份有限公司，十二烷基硫酸钠购自北京化学试剂公司，亚甲基双萘磺酸钠购自江苏擎宇化工科技有限公司，有机硅消泡剂购自迈图高新材料集团，黄原胶购自浙江丰虹新材料股份有限公司，苯甲酸钠购自北京化学试剂公司，脂肪醇聚氧乙烯醚购自南京太化化工有限公司，其余均为商购试剂。
实施例1
将尿素与浓度为40重量％的甲醛水溶液混合均匀，在pH值为8，温度为70℃条件下反应1.5h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:1。
将精异丙甲草胺、溶剂油S-200和聚氧乙烯失水山梨醇单硬脂酸酯混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与溶剂油S-200和失水山梨醇单硬脂酸酯聚氧乙烯醚的重量比为1:0.2:0.1。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:1.5；在室温条件下，将pH值为4.5、缓冲对的总浓度为1.5重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为5.5，得到第二物料；在室温条件下，将浓度为3重量％的盐酸在1小时内匀速地加入到上述第二物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为4，得到第三物料；在45℃的条件下，将第三物料进行固化缩聚3小时，得到固化缩聚后 的物料；并且通过三乙醇胺溶液将固化缩聚后的物料的pH值调节至7；加入聚羧酸盐、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂(第四物料)，其中，精异丙甲草胺微胶囊悬浮剂与聚羧酸盐、硅酸铝镁和乙二醇的重量比为1：0.02：0.005：0.05。
将50重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入脂肪醇聚氧乙烯醚，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、脂肪醇聚氧乙烯醚的重量比为1:1:0.05。
实施例2
将尿素与浓度为40重量％的甲醛水溶液混合均匀，在pH值为8，温度为70℃条件下反应1.5h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:1。
将精异丙甲草胺、溶剂油S-200和聚氧乙烯失水山梨醇单硬脂酸酯混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与溶剂油S-200和失水山梨醇单硬脂酸酯聚氧乙烯醚的重量比为1:0.2:0.1。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:1.5；在室温条件下，将pH值为4.5、缓冲对的总浓度为1.5重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为5.5，得到第二物料；在室温条件下，将浓度为3重量％的盐酸在1小时内匀速地加入到上述第二物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为4，得到第三物料；在45℃的条件下，将第三物料进行固化缩聚3小时，得到固化缩聚后的物料；并且通过三乙醇胺溶液将固化缩聚后的物料的pH值调节至7；加入聚羧酸盐、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂(第四物料)，其中，精异丙甲草胺微胶囊悬浮剂与聚羧酸盐、硅酸铝镁和乙二醇的重量比为1：0.02：0.005：0.05。
将50重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入脂肪醇聚氧乙烯醚，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、脂肪醇聚氧乙烯醚的重量比为1:3:0.03。
实施例3
将尿素与浓度为40重量％的甲醛水溶液混合均匀，在pH值为8，温度为70℃条件下反应1.5h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:1。
将精异丙甲草胺、溶剂油S-200和聚氧乙烯失水山梨醇单硬脂酸酯混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与溶剂油S-200和失水山梨醇单硬脂酸酯聚氧乙烯醚的重量比为1:0.2:0.1。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:1.5；在室温条件下，将pH值为4.5、缓冲对的总浓度为1.5重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为5.5，得到第二物料；在室温条件下，将浓度为3重量％的盐酸在1小时内匀速地加入到上述第二物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为4，得到第三物料；在45℃的条件下，将第三物料进行固化缩聚3小时，得到固化缩聚后的物料；并且通过三乙醇胺溶液将固化缩聚后的物料的pH值调节至7；加入聚羧酸盐、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂(第四物料)，其中，精异丙甲草胺微胶囊悬浮剂与聚羧酸盐、硅酸铝镁和乙二醇的重量比为1：0.01：0.001：0.02。
将50重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿 特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入脂肪醇聚氧乙烯醚，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、脂肪醇聚氧乙烯醚的重量比为1:1:0.05。
实施例4
将尿素与浓度为35重量％的甲醛水溶液混合均匀，在pH值为8，温度为70℃条件下进行反应2小时；加入蒸馏水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:1，水和甲醛水溶液的体积比为1:2。
将精异丙甲草胺、石油醚和木质素磺酸钠混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与石油醚和木质素磺酸钠的重量比为1:0.1:0.05。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:1；在室温条件下，将pH值为3.0、缓冲对的总浓度为2重量％的乙酸-乙酸钠缓冲溶液，在0.5小时内匀速地加入到上述第一物料中，以500转/分钟的搅拌速度混合均匀，以调节pH值为6.5，得到第二物料；在室温条件下，将浓度为5重量％的盐酸在0.5小时内匀速地加入到上述第二物料中，以200转/分钟的搅拌速度混合均匀，以调节pH值为4.5，得到第三物料；在50℃的条件下，将第三物料进行固化缩聚2小时，得到固化缩聚后的物料，并且通过硫酸溶液将固化缩聚后的物料的pH值调节至7；加入木质素磺酸钠、黄原胶和1,2-丙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂(第四物料)，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、黄原胶和1,2-丙二醇的重量比为1：0.05:0.005:0.05。
将50重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入聚羧酸盐，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、 聚羧酸盐的重量比为1:0.5:0.1。
实施例5
将尿素与浓度为35重量％的甲醛水溶液混合均匀，在pH值为9，温度为70℃条件下进行反应2小时；加入蒸馏水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:2。
将精异丙甲草胺、溶剂油S-150和蓖麻油聚氧乙烯醚混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与溶剂油S-150和蓖麻油聚氧乙烯醚的重量比为1:1:0.05。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1：2；在室温条件下，将pH值为5.0，缓冲对的总浓度为1重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以400转/分钟的搅拌速度混合均匀，以调节pH值为5.5，得到第二物料；在室温条件下，将浓度为8重量％的盐酸在0.5小时内匀速地加入到上述第二物料中，以500转/分钟的搅拌速度混合均匀，以调节pH值为2.5，得到第三物料；在50℃的条件下，将第三物料进行固化缩聚4小时，得到固化缩聚后的物料，并且通过磷酸溶液将固化缩聚后的物料的pH值调节至7；加入木质素磺酸钠、聚乙二醇和丙三醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂(第四物料)，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、聚乙二醇和丙三醇的重量比为1：0.02:0.006:0.04。
将50重量％的阿特拉津、1重量％的十二烷基硫酸钠、2重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39.5重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入亚甲基双萘磺酸钠，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、亚甲基双萘磺酸钠的重量比为1:2:0.05。
实施例6
将尿素与浓度为45重量％的甲醛水溶液混合均匀，在pH值为9，温度 为75℃条件下进行反应2小时；加入蒸馏水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:1，水和甲醛水溶液的体积比为1:1。
将精异丙甲草胺、乙酸乙酯和十二烷基苯磺酸钠混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与乙酸乙酯和十二烷基苯磺酸钠的重量比为1:0.5:0.05。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1：0.5；在室温条件下，将pH值为4.5、缓冲对的总浓度为2重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以200转/分钟的搅拌速度混合均匀，以调节pH值为6.2，得到第二物料；在室温条件下，将浓度为5重量％的盐酸在0.5小时内匀速地加入到上述第二物料中，以400转/分钟的搅拌速度混合均匀，以调节pH值为3.2，得到第三物料；在60℃的条件下，将第三物料进行固化缩聚2小时，得到固化缩聚后的物料；并且通过氢氧化钠溶液将固化缩聚后的物料的pH值调节至7；加入聚羧酸盐、聚乙烯醇和尿素混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，精异丙甲草胺微胶囊悬浮剂与聚羧酸盐、聚乙烯醇和尿素的重量比为1：0.01：0.005：0.05。
将50重量％的阿特拉津、0.5重量％的拉开粉、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入1-甲基萘磺酸钠甲醛缩合物，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、1-甲基萘磺酸钠甲醛缩合物的重量比为1:3:0.15。
实施例7
将尿素与浓度为35重量％的甲醛水溶液混合均匀，在pH值为9，温度为70℃条件下进行反应2小时；加入蒸馏水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:1。
将精异丙甲草胺、溶剂油S-150和苯乙烯-马来酸酐共聚物混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与二氯甲烷、苯乙烯-马来酸酐共聚物的重量比为1:0.3:0.1。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:2；在室温条件下，将pH值为4.5、缓冲对的总浓度为2重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为5.5，得到第二物料；在室温条件下，将浓度为5重量％的盐酸在0.5小时内匀速地加入到上述第二物料中，以200转/分钟的搅拌速度混合均匀，以调节pH值为4.0，得到第三物料；在45℃的条件下，将第三物料进行固化缩聚2小时，得到固化缩聚后的物料；并且通过三乙胺溶液将固化缩聚后的物料的pH值调节至7；加入木质素磺酸钠、羧甲基纤维素和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、羧甲基纤维素和乙二醇的重量比为1：0.01：0.005：0.05。
将50重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与39重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入脱糖木质素磺酸钠，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、脱糖木质素磺酸钠的重量比为1:5:0.05。
实施例8
将尿素与浓度为35重量％的甲醛水溶液混合均匀，在pH值为8，温度为70℃条件下反应1.5h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:2。
将精异丙甲草胺、溶剂油S-150和脂肪醇聚氧乙烯醚混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与三氯甲烷和脂肪醇聚氧乙烯醚的重量比为1:0.3:0.15。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得 到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:1；在室温条件下，将pH值为4.5、缓冲对的总浓度为2重量％的乙酸-乙酸钠缓冲溶液，在0.5小时内匀速地加入到上述第一物料中，以300转/分钟的搅拌速度混合均匀，以调节pH值为6.2，得到第二物料；在室温条件下，将浓度为5重量％的盐酸在1.5小时内匀速地加入到上述第二物料中，以500转/分钟的搅拌速度混合均匀，以调节pH值为3.2，得到第三物料；在60℃的条件下，将第三物料进行固化缩聚2小时，得到固化缩聚后的物料；并且通过盐酸溶液将固化缩聚后的物料的pH值调节至7；加入木质素磺酸钠、膨润土和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、膨润土和乙二醇的重量比为1：0.01：0.005：0.05。
将32重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与57重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入丁二酸酯磺酸钠，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、丁二酸酯磺酸钠的重量比为1:4:0.01。
实施例9
将尿素与浓度为40重量％的甲醛水溶液混合均匀，在pH值为9，温度为65℃条件下反应1h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:2。
将精异丙甲草胺、溶剂油S-150和失水山梨醇聚氧乙烯聚氧丙烯醚混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与S-150和失水山梨醇聚氧乙烯聚氧丙烯醚的重量比为1:0.5:0.05。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:2；在室温条件下，将pH值为4.5、缓冲对的总浓度为2重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以200转/分钟的搅拌速度混合均匀，以调节pH值为6.2，得到第二物料；在室温条 件下，将浓度为5重量％的盐酸在1小时内匀速地加入到上述第二物料中，以500转/分钟的搅拌速度混合均匀，以调节pH值为3.2，得到第三物料；在60℃的条件下，将第三物料进行固化缩聚2小时，得到固化缩聚后的物料；并且通过乙酸溶液将固化缩聚后的物料的pH值调节至7；加入木质素磺酸钠、白炭黑和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、白炭黑和乙二醇的重量比为1：0.01：0.005：0.05。
将32重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与57重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入拉开粉，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、拉开粉的重量比为1:0.8:0.02。
实施例10
将尿素与浓度为35重量％的甲醛水溶液混合均匀，在pH值为8，温度为75℃条件下反应1h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:2。
将精异丙甲草胺、溶剂油S-200和月桂醇硫酸钠混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与溶剂油S-200和月桂醇硫酸钠的重量比为1:0.3:0.06。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:2；在室温条件下，将pH值为3.6、缓冲对的总浓度为4重量％的柠檬酸-柠檬酸钠缓冲溶液，在0.5小时内匀速地加入到上述第一物料中，以400转/分钟的搅拌速度混合均匀，以调节pH值为6.2，得到第二物料；在室温条件下，将浓度为4重量％的磷酸在0.5小时内匀速地加入到上述第二物料中，以200转/分钟的搅拌速度混合均匀，以调节pH值为2.5，得到第三物料；在60℃的条件下，将第三物料进行固化缩聚4小时，得到固化缩聚后的物料；并且通过磷酸溶液将固化缩聚后的物料的pH值调节至7；加 入木质素磺酸钠、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、硅酸铝镁和乙二醇的重量比为1：0.02：0.004：0.04。
将32重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与57重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入壬基酚聚氧乙烯醚，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、壬基酚聚氧乙烯醚的重量比为1:1.2:0.05。
实施例11
将尿素与浓度为35重量％的甲醛水溶液混合均匀，在pH值为8，温度为70℃条件下反应1.5h；加入水稀释，得到尿素-甲醛树脂预聚体水溶液，其中，甲醛与尿素的摩尔比为1:0.5，水和甲醛水溶液的体积比为1:2。
将精异丙甲草胺、溶剂油S-200和聚乙烯醇混合均匀，得到精异丙甲草胺乳油，其中，精异丙甲草胺与溶剂油S-200和聚乙烯醇的重量比为1:0.4:0.06。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1：0.5，在室温条件下，将pH值为4.0、缓冲对的总浓度为4重量％的柠檬酸-磷酸氢二钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以400转/分钟的搅拌速度混合均匀，以调节pH值为5.5，得到第二物料；在室温条件下，将浓度为2重量％的硫酸在0.5小时内匀速地加入到上述第二物料中，以400转/分钟的搅拌速度混合均匀，以调节pH值为4.5，得到第三物料；在65℃的条件下，将第三物料进行固化缩聚2小时，得到固化缩聚后的物料；并且将固化缩聚后的物料的pH值调节至7；加入木质素磺酸钠、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，精异丙甲草胺微胶囊悬浮剂与木质素磺酸钠、硅酸铝镁和乙二醇的重量比为1：0.03：0.005：0.05。
将32重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚 甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与57重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入木质素磺酸钠，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、木质素磺酸钠的重量比为1:1.5:0.04。
对比例1
根据实施例1中的制备方法，制备尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1：4；在室温条件下，将浓度为5重量％的磷酸在2小时内匀速地加入到上述第一物料中，以500转/分钟的搅拌速度混合均匀，以调节pH值为3.2，得到第二物料；在35℃条件下，将第二物料进行固化缩聚2小时，得到固化缩聚产物，并且将固化缩聚产物的pH值调节至7；加入木质素磺酸钠、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，固化缩聚产物与木质素磺酸钠、硅酸铝镁和乙二醇的重量比为1：0.01：0.005：0.05。
将32重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与57重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入木质素磺酸钠，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、木质素磺酸钠的重量比为1:0.3:0.05。
对比例2
根据实施例1中的制备方法，制备尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油。
将所得尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油混合均匀，得到第一物料，其中尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油的重量比为1:4；在室温条件下，将pH值为4.5、缓冲对的总浓度为2重量％的乙酸-乙酸钠缓冲溶液，在1小时内匀速地加入到上述第一物料中，以500转/分钟的搅拌速度混合均匀，以调节pH值为6.5，得到第二物料；在60℃条件下，将所述第二物料进行固化缩聚2.5小时，得到固化缩聚产物，并且将所述固化缩聚产物的pH值调节至7；加入木质素磺酸钠、硅酸铝镁和乙二醇混合均匀，得到精异丙甲草胺微胶囊悬浮剂，其中，固化缩聚产物与木质素磺酸钠、硅酸铝镁和乙二醇的重量比为1：0.01：0.005：0.05。
将32重量％的阿特拉津、0.5重量％的十二烷基硫酸钠、3重量％的亚甲基双萘磺酸钠、2重量％的有机硅消泡剂、5重量％的乙二醇、0.3重量％的黄原胶、0.2重量％的苯甲酸钠与57重量％的水充分混合、分散，分散均匀后通入砂磨机进行砂磨，砂磨至平均粒径小于5微米的悬浮液，得到阿特拉津悬浮剂。
最后，将精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂混合，再加入木质素磺酸钠，搅拌均匀，得到的药剂可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用。其中，精异丙甲草胺微胶囊悬浮剂与阿特拉津悬浮剂、木质素磺酸钠的重量比为1:0.5:0.05。
对比例3
根据实施例1中的制备方法，制备得到可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用的药剂，不同在于第三物料的pH值为2.0。
对比例4
根据实施例1中的制备方法，制备得到可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用的药剂，不同在于第三物料的pH值为9。
对比例5：精异丙甲草胺·阿特拉津悬乳剂的制备
采用实施例1中的原料，不同在于将精异丙甲草胺、溶剂油S-200和失水山梨醇单硬脂酸酯聚氧乙烯醚和水混合均匀，得到精异丙甲草胺水乳剂，与阿特拉津悬浮剂混合为悬乳剂，其中，精异丙甲草胺、溶剂油S-200、失水山梨醇单硬脂酸酯聚氧乙烯醚、水的重量比为1:4:0.06:6，精异丙甲草胺水乳剂与阿特拉津悬浮剂的重量比为1:1。
对比例6：精异丙甲草胺微囊悬浮剂的制备
采用实施例中1的原料和制备方法，不同在于不加入阿特拉津悬浮剂。
对比例7：阿特拉津悬浮剂的制备
采用实施例中1的原料和制备方法，不同在于不加入精异丙甲草胺微囊悬浮剂。
测试实施例1
本测试实施例用于测试实施例1-11得到的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂和对比例1-7中得到的相应药剂的热贮稳定性和低温稳定性。
热贮稳定性测试：将实施例1-11得到的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂和对比例1-7中得到的相应药剂分别装入容器中，密封后放置于(54±2)℃的恒温烘箱中，静置14天后取出，根据GB/T14825-2006标准，测定微胶囊悬浮剂的悬浮率，结果见表1。
低温稳定性测定：将实施例1-11得到的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂和对比例1-7中得到的相应药剂分别装入容器中，密封后置于(0±2)℃制冷器中，保持1h，每间隔15min搅拌一次，每次15s，观察外观有无变化，在(0±2)℃继续放置7天，然后取出置于室温条件下静置恢复后，根据GB/T14825-2006标准，测定微囊悬浮-悬浮剂的悬浮率，结果见表1。
表1
  热贮稳定性 低温稳定性
实施例1 流动性良好，无分层结块，悬浮率为97.3％ 流动性良好，无分层结块，悬浮率为97.9％
实施例2 流动性良好，析水5％，无结块，悬浮率92.5％ 流动性良好，无分层结块，悬浮率为93.4％
实施例3 流动性良好，析水3％，无结块，悬浮率94.6％ 流动性良好，无分层结块，悬浮率为94.7％
实施例4 流动性良好，无分层结块，悬浮率为96.9％ 流动性良好，无分层结块，悬浮率为97.0％
实施例5 流动性良好，无分层结块，悬浮率为96.4％ 流动性良好，无分层结块，悬浮率为96.2％
实施例6 流动性良好，无分层结块，悬浮率为96.6％ 流动性良好，无分层结块，悬浮率为96.7％
实施例7 流动性良好，无分层结块，悬浮率为93.4％ 流动性良好，无分层结块，悬浮率为94.8％
实施例8 流动性良好，无分层结块，悬浮率为95.2％ 流动性良好，无分层结块，悬浮率为95.4％
实施例9 流动性良好，无分层结块，悬浮率为94.9％ 流动性良好，无分层结块，悬浮率为95.3％
实施例10 流动性良好，无分层结块，悬浮率为93.1％ 流动性良好，无分层结块，悬浮率为93.7％
实施例11 流动性良好，无分层结块，悬浮率为96.3％ 流动性良好，无分层结块，悬浮率为94.9％
对比例1 黏度增大，流动性稍差，悬浮率为72.4％ 流动性稍差，悬浮率为73.5％
对比例2 黏度增大，流动性差，悬浮率为70.8％ 流动性稍差，悬浮率为74.8％
对比例3 黏度增大，流动性差，悬浮率为65.6％ 黏度增大，流动性差，悬浮率为61.2％
对比例4 凝固 凝固
对比例5 黏度增大，流动性差，悬浮率为67.8％ 黏度增大，流动性差，悬浮率为71.8％
对比例6 流动性良好，无分层结块，悬浮率为95.3％ 流动性良好，无分层结块，悬浮率为94.9％
对比例7 流动性良好，无分层结块，悬浮率为97.6％ 流动性良好，无分层结块，悬浮率为95.8％
从表1可以看出，本发明提供的制备方法得到的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂具有良好的热贮存稳定性和低温贮存稳定性。
测试实施例2
本测试实施例对实施例1-11得到的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂和对比例1-7中得到的相应药剂对玉米田中马唐、藜的防治效果进行测试。测试进行二次稀释，按照精异丙甲草胺-阿特拉津浓度分别为10重量％将实施例1-11和对比例1-7的药剂分别配制成药液。
试验地点：广西省南宁市。该地块地势平坦，肥力较好。施药后的各处理区玉米按常规生产管理。
具体步骤包括，使用背负式喷雾器，按照施药液量为30kg/亩，将实施例1-11和对比例1-7中得到的精异丙甲草胺-阿特拉津微囊悬浮-悬浮剂药液分别对各个种植区的玉米田于播后苗前进行均匀喷药，并设置清水对照。
于施药后10天、20天、30天和50天调查稗草的防治效果，具体试验方法按照《农药田间药效试验准则》进行。每个处理区采用随机5点取样，调查各处理区马唐、藜植株的防治效果，在施药后分别10、20、30、50天时，对杂草进行识别计数，按式(A)计算株防效，具体结果见表2:
Figure PCTCN2019113602-appb-000003
表2
Figure PCTCN2019113602-appb-000004
从表2可以看出，本公开提供的制备方法利用缓冲溶液和酸性pH调节剂的特定组合、分步调节反应体系酸性、相应转速、选取相应乳化剂、溶剂等特定的反应条件下制备得到的可以作为含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂使用的药剂，能够取得缓释长效地防治农作物害虫的效果。
本公开的含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂相对于精异丙甲草胺·阿特拉津的其他剂型，具有持效期长的特点，从而可降低用药次数和用药量，节约成本；其中含有的有机溶剂少，可以降低对环境的污染。
以上详细描述了本公开的优选实施方式，但是，本公开并不限于上述实施方式中的具体细节，在本公开的技术构思范围内，可以对本公开的技术方案进行多种简单变型，这些简单变型均属于本公开的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本公开对各种可能的组合方式不再另行说明。
此外，本公开的各种不同的实施方式之间也可以进行任意组合，只要其不违背本公开的思想，其同样应当视为本公开所公开的内容。
工业实用性
本发明实施例提供的一种制备含有阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的方法及其微囊悬浮-悬浮剂，所述方法包括：a、将尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油按照重量比为1：(0.5-2)混合，得到第一物料；b、调整所述第一物料的pH值为5.0-6.5，得到第二物料；c、调整所述第二物料的pH值为2.5-4.5，得到第三物料；d、第三物料进行固化缩聚，然后将固化缩聚后的物料的pH值调节至中性后与第一分散剂、增稠剂和防冻剂混合均匀，得到第四物料；e、第四物料与阿特拉津悬浮剂混合后加入第二分散剂并混合均匀；通过所述方法制备的含有阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂，显著提高了含阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的贮存稳定性和对杂草的防治效果。

Claims (10)

  1. 一种制备含有阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂的方法，其特征在于，该方法包括以下步骤：
    a、将尿素-甲醛树脂预聚体水溶液和精异丙甲草胺乳油按照重量比为1：(0.5-2)混合均匀，得到第一物料；
    b、将步骤a中得到的第一物料与缓冲溶液混合均匀，调整所述第一物料的pH值为5.0-6.5，得到第二物料；
    c、将步骤b中得到的所述第二物料与酸性pH值调节剂混合均匀，调整所述第二物料的pH值为2.5-4.5，得到第三物料；
    d、将步骤c中得到的所述第三物料进行固化缩聚，得到固化缩聚后的物料，然后将所述固化缩聚后的物料的pH值调节至中性后与第一分散剂、增稠剂和防冻剂混合均匀，得到第四物料；
    e、将步骤d中得到的所述第四物料与阿特拉津悬浮剂混合后加入第二分散剂并混合均匀。
  2. 根据权利要求1所述的方法，其特征在于，步骤a中的所述尿素-甲醛树脂预聚体水溶液为将尿素、甲醛和水进行预聚合得到的；
    可选地，所述预聚合的条件包括：pH值为8-9，温度为65-75℃，时间为1-2h。
  3. 根据权利要求1或2所述的方法，其特征在于，步骤a中的所述精异丙甲草胺乳油含有精异丙甲草胺、有机溶剂和乳化剂；
    可选地，所述有机溶剂包括石油醚、乙酸乙酯、二氯甲烷、三氯甲烷、二甲苯、溶剂油S-150和溶剂油S-200中的一种或多种；
    可选地，所述乳化剂包括十二烷基硫酸钠、十二烷基苯磺酸钠、苯乙烯-马来酸酐共聚物、烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、聚氧乙烯失水山梨醇酯类、月桂醇硫酸钠、聚乙烯醇和蓖麻油聚氧乙烯醚中的一种或多种；
    可选地，所述精异丙甲草胺、所述有机溶剂和所述乳化剂的重量比为1：(0.1-1)：(0.05-0.2)。
  4. 根据权利要求1所述的方法，其特征在于，步骤b中的所述缓冲溶液含有缓冲对；
    可选地，所述缓冲对包括柠檬酸-柠檬酸钠、柠檬酸-磷酸氢二钠和乙酸-乙酸钠中的一种或多种；
    可选地，所述缓冲溶液中缓冲对的总浓度为1-5重量％，所述缓冲溶液的pH值为3-5。
  5. 根据权利要求1所述的方法，其特征在于，步骤c中的所述酸性pH值调节剂包括盐酸、硫酸、磷酸、乙酸和氯化铵溶液中的一种或多种；
    和/或，所述酸性pH值调节剂的浓度为1-10重量％。
  6. 根据权利要求1所述的方法，其特征在于，步骤d中，所述固化缩聚的温度为40-65℃、时间为2-4h；
    和/或，该方法包括：通过碱性pH调节剂将所述固化缩聚后的物料的pH值调节至中性；可选地，所述碱性pH调节剂包括三乙胺、三乙醇胺、氢氧化钠和氢氧化钾溶液中的一种或多种；可选地，所述第四物料、所述第一分散剂、所述第一增稠剂和所述第一防冻剂的重量比为1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15)。
  7. 根据权利要求1所述的方法，其特征在于，步骤e中，所述第四物料、所述阿特拉津悬浮剂和所述第二分散剂的重量比为1：(0.5-5)：(0.01-0.2)。
  8. 根据权利要求1或7所述的方法，其特征在于，该方法还包括：在步骤e之前，将阿特拉津原药、第三分散剂、第二增稠剂、第二防冻剂和水混合、分散和磨砂，得到步骤e中的所述阿特拉津悬浮剂；
    可选地，所述阿特拉津悬浮剂为平均粒径为1-5μm的悬浮微粒。
  9. 根据权利要求1所述的方法，其特征在于，所述方法包括下述特征中的一种或多种：
    步骤a中的所述混合的条件包括：搅拌速度为200-400r/min，搅拌时间为30-60min；
    步骤b包括，在25-35℃下，在0.5-1h内将所述缓冲溶液匀速加入所述第一物料中，并以200-500r/min的转速搅拌混合均匀；
    步骤c包括，在25-35℃下，在0.5-1h内将所述酸性pH调节剂匀速加入所述第二物料中，并以200-500r/min的转速搅拌混合均匀；
    步骤d中的所述混合的条件包括：搅拌速度为200-300r/min，搅拌时间为1-3h；
    步骤e中的所述混合的条件包括：搅拌速度为200-300r/min，搅拌时间 为30-60min。
  10. 根据权利要求1-9中任意一项所述的方法制备得到的含有阿特拉津和精异丙甲草胺的微囊悬浮-悬浮剂。
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