CN109479894A - A kind of method and its microcapsule suspension-suspendinagent agent preparing the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron - Google Patents

A kind of method and its microcapsule suspension-suspendinagent agent preparing the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron Download PDF

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Publication number
CN109479894A
CN109479894A CN201811378078.1A CN201811378078A CN109479894A CN 109479894 A CN109479894 A CN 109479894A CN 201811378078 A CN201811378078 A CN 201811378078A CN 109479894 A CN109479894 A CN 109479894A
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China
Prior art keywords
lufenuron
sodium
weight
agent
cyhalothrin
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CN201811378078.1A
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Inventor
高敬雨
刘润峰
潘静
丁文明
陈坤
张孝武
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Jiangsu Mingde Rieter Crop Technology Co Ltd
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Jiangsu Mingde Rieter Crop Technology Co Ltd
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Priority to CN201811378078.1A priority Critical patent/CN109479894A/en
Publication of CN109479894A publication Critical patent/CN109479894A/en
Priority to PCT/CN2019/113603 priority patent/WO2020103646A1/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N53/00Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/26Biocides, 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
    • A01N25/28Microcapsules or nanocapsules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/34Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

This disclosure relates to a kind of method and its microcapsule suspension-suspendinagent agent prepared containing gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent, this method comprises: a, by amino resins performed polymer aqueous solution being by weight (1-5) with efficient cyhalothrin emulsifiable concentrate: 1 mixes, and obtains first material;B, first material is mixed with buffer solution, obtains the second material that pH value is 4-7;C, second material is mixed with acid solution, obtains the third material that pH value is 3-4;D, 4 materials were obtained by third material stirring 2-5 hours under conditions of temperature is 40-70 DEG C;E, by weight it is 1:(0.1-1 with lufenuron suspension agent and emulsifying dispersant by 4 materials): (0.01-2) is mixed.The microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron using disclosed method preparation has preferable storage stability, slow release long-acting it can prevent and treat crop pests, times for spraying and dosage, save the cost are reduced, the pollution to environment is alleviated.

Description

A kind of microcapsule suspension-suspendinagent agent prepared containing gamma cyhalothrin and lufenuron Method and its microcapsule suspension-suspendinagent agent
Technical field
This disclosure relates to pesticide field, and in particular, to it is a kind of prepare it is micro- containing gamma cyhalothrin and lufenuron Capsule suspension-suspending agent method and its microcapsule suspension-suspendinagent agent.
Background technique
Gamma cyhalothrin is a kind of broad spectrum pesticide, it can inhibit the conduction at insect neural axon position, to insect Have the function of walking quickly and keeping away, knock down and killing, can also be mixed with most of fungicide, Insecticides (tech) & Herbicides (tech), have preferable anti- Control effect.Its effective component of traditional formulations of pesticide easily fails under the action of external environment, such as sunshine, soil acidity or alkalinity etc., Lasting period is short, thus reduces the preventive effect of pesticide.The existing preparation containing gamma cyhalothrin contains a large amount of organic on the market Solvent pollutes environment.And gamma cyhalothrin single dose also has certain limitation, and compounding with lufenuron not only can be effective Practical control efficiency is improved, dosage is reduced, reduces cost, delay the generation of drug resistance, but also pesticide species can be extended Service life, reduce pollution to environment.
Microcapsule suspending agent forms nucleocapsid structure small container using natural or synthesis high molecular material, can be by agriculture Pack covers wherein and in suspension and water, is that a kind of lasting period is long, organic solvent amount is few, endangers operator small Novel rural medicament Type.The lambda-cyhalothrin microcapsule suspension that traditional preparation methods obtain is easy to happen reunion, solidification phenomenon, causes to be not easy Storage, prevention and treatment crop pests effect are poor, it is difficult to meet the preparation demand of prevention and treatment crop pests pesticide.
Summary of the invention
Purpose of this disclosure is to provide a kind of gamma cyhalothrins and lufenuron microcapsule suspension-easily stored and drug effect is high The preparation method of suspending agent and by this method preparation gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent.
To achieve the goals above, disclosure first aspect: providing a kind of gamma cyhalothrin and lufenuron micro-capsule is outstanding The preparation method of floating-suspending agent, this method comprises the following steps: a, by amino resins performed polymer aqueous solution and efficient cyhalothrin Emulsifiable concentrate is (1-5) by weight: 1 mixing obtains first material;B, by the first material obtained in step a and buffering Solution mixing, obtains second material, and the pH value of the second material is 4-7;C, by the second material obtained in step b with Acid solution mixing, obtains third material, and the pH value of the third material is 3-4;It d, will under conditions of temperature is 40-70 DEG C The third material obtained in step c is handled 2-5 hours, obtains 4 materials;E, by the 4th object obtained in step d Material is 1:(0.1-1 with lufenuron suspension agent and emulsifying dispersant by weight): (0.01-2) is mixed, and is obtained containing efficient chlorine Microcapsule suspension-suspending agent of flucythrinate and lufenuron.
Preferably, the amino resins performed polymer aqueous solution in step a be by amino-containing compound, formaldehyde and water into Row prepolymerization obtains;The molar ratio of the amino-containing compound and formaldehyde is (0.1-2): 1, the weight of the water and formaldehyde Amount is than being (2-6): 1;The amino-containing compound includes at least one of urea, melamine and benzoguanamine; The prepolymerized condition includes: that pH value is 8-10, and temperature is 60-80 DEG C, and the time is 0.5-3 hours.
Preferably, the efficient cyhalothrin emulsifiable concentrate in step a contains gamma cyhalothrin, organic solvent and cream Agent;The organic solvent includes at least one of petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and solvent naphtha, described Emulsifier include sodium lignin sulfonate, lauryl sodium sulfate, neopelex, styrene-maleic anhydride copolymer, Fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate polyoxyethylene ether, At least one of sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate;It is the gamma cyhalothrin, described The weight ratio of organic solvent and the emulsifier is 1:(0.1-5): (0.01-0.2).
Preferably, the buffer solution in step b contains buffering pair, and the buffering is to including citric acid-citric acid At least one of sodium, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate.
Preferably, the acid solution in step c includes at least one in hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid and ammonium chloride Kind.
Preferably, the mixing in step a carries out under stirring conditions, and the speed of the stirring is 1500-3000 Rev/min;The mixing in step b carries out under stirring conditions, and the speed of the stirring is 1000-1200 revs/min; The mixing in step c carries out under stirring conditions, and the speed of the stirring is 1200-1500 revs/min.
Preferably, in step e, after the 4 materials are mixed with the first dispersing agent, thickener and antifreezing agent, then with institute State emulsifying dispersant mixing;First dispersing agent includes neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene Sodium sulfonate formaldehyde condensation products, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation In sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether at least It is a kind of;The thickener includes aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white At least one of carbon black;The antifreezing agent includes at least one of ethylene glycol, 1,2- propylene glycol, glycerine and urea;Institute The weight ratio for stating 4 materials and first dispersing agent, the thickener and the antifreezing agent is 1:(0.01-0.2): (0.001-0.02): (0.02-0.15).
Preferably, in step e, the 4 materials and the lufenuron suspension agent and the emulsifying dispersant are by weight For 1:(0.2-0.5): (0.02-0.05) mixing.
Preferably, the Acarus tritici suspending agent in step e is after mixing lufenuron with the second dispersing agent and water by obtaining, The weight ratio of the lufenuron and second dispersing agent and water is 1:(0.2-0.5): (1.5-3): the second dispersing agent packet Include neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalenesulfonateformaldehyde formaldehyde Condensation product, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pulls open sodium lignin sulfonate At least one of powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether, the emulsifying dispersant include dodecyl It is benzene sulfonic acid sodium salt, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, wooden Plain sodium sulfonate, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, nonyl phenol are poly- At least one of ethylene oxide ether and fatty alcohol polyoxyethylene ether.
Disclosure second aspect: gamma cyhalothrin and the lufenuron for providing the method preparation of disclosure first aspect are micro- Capsule suspension-suspending agent.
Through the above technical solutions, the present invention adjusts certain ph, the offer lambda-cyhalothrin being prepared by multistep There is preferable storage stability with the microcapsule suspension-suspendinagent agent of lufenuron, be not susceptible to reunion, solidification phenomenon, can be sustained Crop pests are prevented and treated longer, are reduced times for spraying and dosage, save the cost, are alleviated the pollution to environment.
Other feature and advantage of the disclosure will the following detailed description will be given in the detailed implementation section.
Specific embodiment
The specific embodiment of the disclosure is described in detail below.It should be understood that described herein specific Embodiment is only used for describing and explaining the disclosure, is not limited to the disclosure.
Disclosure first aspect: a kind of microcapsule suspension-suspension prepared containing gamma cyhalothrin and lufenuron is provided The method of agent, this method comprises the following steps: amino resins performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate a, being pressed weight Amount is than being (1-5): 1 mixing obtains first material;B, the first material obtained in step a is mixed with buffer solution, Second material is obtained, the pH value of the second material is 4-7;C, by the second material and acid solution obtained in step b Mixing, obtains third material, and the pH value of the third material is 3-4;It d, will be in step c under conditions of temperature is 40-70 DEG C The obtained third material is handled 2-6 hours, obtains 4 materials;E, by the 4 materials and lice obtained in step d Mite urea suspending agent and emulsifying dispersant are 1:(0.1-1 by weight): (0.01-2) mixing is obtained containing efficient cyhalothrin The microcapsule suspension-suspendinagent agent of ester and lufenuron.
In the disclosure, gamma cyhalothrin is compound [1 α (S*), 3 α (Z)]-(RS) -3- (2- chloro- 3,3,3- tri- Fluoro- 1- acrylic) -2,2- dimethyl cyclopropane carboxylic acid-cyano-(3- Phenoxyphenyl) methyl ester trade name, English name For λ-Cyhalothrin, molecular formula C23H19ClF3NO3, relative molecular weight 449.9, No. CAS is 91465-08-6, structure Shown in formula such as formula (1) and formula (2).
In the disclosure, lufenuron is Compound RS) -1- [2,5- bis- chloro- 4- (1,1,2,3,3,3- hexafluoro propoxyl group) benzene Base] -3- (2,6- difluoro benzoyl) urea trade name, English name Lufenuron, molecular formula C17H8Cl2F8N2O3, Relative molecular weight is 511.2, and No. CAS is 103055-07-8, shown in structural formula such as formula (3).
According to the disclosure in a first aspect, the preparation method of the amino resins performed polymer aqueous solution in step a can be with For preparation method well known to those skilled in the art, the disclosure is not particularly limited it.Under preferable case, the amino tree Amino-containing compound, formaldehyde and water can be carried out prepolymerization and obtained by rouge performed polymer aqueous solution, amino-containingization The molar ratio for closing object and formaldehyde can be (0.1-2): 1, the mass ratio of the water and formaldehyde can be (2-6): 1.It is described to contain ammonia The compound of base may include at least one of urea, melamine and benzoguanamine, and the prepolymerized condition can To include: pH value for 8-10, temperature is 60-80 DEG C, and the time is 0.5-3 hours.
According to the disclosure in a first aspect, the preparation method of the efficient cyhalothrin emulsifiable concentrate in step a can be Preparation method well known to those skilled in the art, the disclosure are not particularly limited it.Under preferable case, the efficient chlorine fluorine Cyano chrysanthemate missible oil can contain gamma cyhalothrin, organic solvent and emulsifier, by gamma cyhalothrin, organic solvent and The efficient cyhalothrin emulsifiable concentrate can be obtained in emulsifier mixing.Wherein, the organic solvent can dissolve to be various With the substance of dilution gamma cyhalothrin, it is preferable that the organic solvent may include petroleum ether, ethyl acetate, oleic acid first At least one of ester, dimethylbenzene and solvent naphtha.The emulsifier can be the various substances with emulsification, it is preferable that The emulsifier may include sodium lignin sulfonate, lauryl sodium sulfate, neopelex, styrene-maleic acid Anhydride copolymer, fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate are poly- At least one of ethylene oxide ether, sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate.It is micro- further to improve The particle diameter distribution and clad ratio of micro-capsule in capsule suspending agent, to further increase the storage stability of microcapsule suspending agent, preferably In the case of, the weight ratio of the gamma cyhalothrin, organic solvent and emulsifier can be 1:(0.1-5): (0.01- 0.2), the organic solvent content of the proportion is suitable for that can reduce the pollution to environment.
According to the disclosure in a first aspect, in order to improve the clad ratio of micro-capsule, the uniformity and softgel shell compactness, thus into One step improve gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent storage stability, make its be not susceptible to reunite and Solidification phenomenon, and have good crop pests control efficiency, after obtaining first material, can be respectively adopted buffer solution and Acid solution carries out the adjusting of pH to it.It such as in one embodiment, can be molten by the first material and buffering first Liquid mixing obtains the second material that pH value is 4-7;Then the second material is mixed with acid solution, obtaining pH value is The third material of 3-4.
According to the disclosure in a first aspect, the meaning of the buffer solution in step b is ripe for those skilled in the art Know, for the solution containing buffering pair.Under preferable case, the buffering is to may include citric acid-sodium citrate, citric acid-phosphorus At least one of sour disodium hydrogen and acetic acid-sodium acetate.In order to make the pH value of second material be adjusted to 5-7, the buffer solution PH value can be 3-5.5.The total concentration of buffering pair in the buffer solution can be 1-5 weight %.
According to the disclosure in a first aspect, the acid solution in step c can have acidity for this field routine Substance.Under preferable case, the acid solution may include at least one in hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid and ammonium chloride Kind.Sour concentration can be 0.5-8 weight % in the acid solution.
According to the first aspect of the invention, reaction condition appropriate can mention micro-capsule clad ratio, improve particle diameter distribution with And the thickness of softgel shell, and then improve the storage stability of microcapsule suspending agent.Under preferable case, the mixing in step a can be with It carries out under stirring conditions, the speed of the stirring can be 1500-3000 revs/min.The mixing in step b can To carry out under stirring conditions, the speed of the stirring can be 1000-1200 revs/min.The mixing in step c It can carry out under stirring conditions, the speed of the stirring can be 1200-1500 revs/min.
According to the disclosure in a first aspect, those skilled in the art should know, when insecticide is in acid or alkali When property, the growth of plant can be not only hindered, will also result in the pollution of environment.Therefore, by 4 materials and lufenuron suspension agent and Before emulsifying dispersant is mixed, the 4 materials acid-base property is preferably in neutrality.Therefore, the method for disclosure first aspect Include the steps that the pH value for adjusting the 4 materials to neutrality, the method for adjusting pH value can be the routine side of this field Method, details are not described herein.
According to the disclosure in a first aspect, in order to avoid there is phenomena such as micro-capsule aggregation, precipitate, is hardened, this method may be used also To include, in step e, after first the 4 materials can be mixed with the first dispersing agent, thickener and antifreezing agent, then with it is described Emulsifying dispersant mixing, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron.First dispersing agent It may include neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acids Formaldehyde condensation products, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, At least one of pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether.The thickener may include silicic acid At least one of magnalium, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black.It is described anti- Freezing agent may include at least one of ethylene glycol, 1,2- propylene glycol, glycerine and urea.The 4 materials and the first dispersion The weight ratio of agent, thickener and antifreezing agent can be 1:(0.01-0.2): (0.001-0.02): (0.02-0.15).
Further, in order to improve the shelf characteric of micro-capsule, in step e, the 4 materials and the lufenuron suspend Agent and the emulsifying dispersant are preferably mixed by weight for 1:(0.2-0.5): (0.02-0.05).
According to the disclosure in a first aspect, the preparation method of the lufenuron suspension agent in step e can be this field Preparation method known to technical staff, the disclosure are not particularly limited it.For example, can be by lufenuron and the second dispersing agent It is sufficiently mixed, disperses with water, be present in lufenuron in aqueous solution with aerosol form, be then sanded so that lufenuron particle Average grain diameter be 1-5 microns, obtain lufenuron suspension agent.Second dispersing agent may include neopelex, Sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, Desugar sodium lignin sulfonate, desugar are condensed sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether At least one of with fatty alcohol polyoxyethylene ether.The weight ratio of the lufenuron and the second dispersing agent, water can be 1:(0.2- 0.5): (1.5-3).In addition, in the lufenuron suspension agent can also include defoaming agent, thickener, antifreezing agent, preservative, in At least one.The defoaming agent can be polyether antifoam agent and/or organic silicon defoamer.The thickener may include silicic acid At least one of magnalium, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black etc..It is described Antifreezing agent may include at least one of ethylene glycol, 1,2- propylene glycol, glycerine and urea.
According to the disclosure in a first aspect, outstanding in order to further increase the micro-capsule containing gamma cyhalothrin and lufenuron The storage stability of floating-suspending agent, the emulsifying dispersant in step e may include neopelex, methylene Double sodium naphthalene sulfonates, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar wood Quality sodium sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether and fat At least one of alcohol polyoxyethylene ether.
Disclosure second aspect: provide the method preparation of disclosure first aspect contains gamma cyhalothrin and Acarus tritici The microcapsule suspension-suspendinagent agent of urea.
The disclosure is further described by the following examples, is not limited to the disclosure.
In embodiment and comparative example, gamma cyhalothrin is purchased from Huifeng Agricultural Chemistry Co., Ltd., Jiangsu, and lufenuron (contains 98%) amount is is purchased from Jiangsu Zhong Qi Science and Technology Co., Ltd., melamine is purchased from Beijing Chemical Plant, and urea is purchased from Beijing chemical industry Factory, benzoguanamine are purchased from Beijing Chemical Plant, and formaldehyde is purchased from Beijing Chemical Plant, sorbitan monostearate polyoxyethylene Ether is purchased from Nanjing Teva-Chem. Co., Ltd., and lauryl sodium sulfate is purchased from Beijing Zhong Chuan hongda Science and Technology Ltd., lignin Sodium sulfonate is purchased from Beijing Zhong Chuan hongda Science and Technology Ltd., and neopelex is purchased from the limited public affairs of wound hongda science and technology in Beijing Department;Polyvinyl alcohol is purchased from Zhengzhou Ao Cai industrial chemicals Co., Ltd, and fatty alcohol polyoxyethylene ether is purchased from Xingtai blue star auxiliary reagent factory, silicon Sour magnalium is purchased from Hunan Peng Tai new high-tech material Co., Ltd, and bentonite is purchased from Anji County, Zhejiang Province sky dragon organobentonite Co., Ltd, Organic silicon defoamer is purchased from Shanghai Mitugao New Material Group, and ethylene glycol, glycerine, 1,2-PD are purchased from Beijing Chemical Plant, Xanthan gum is purchased from Shandong Zhong Xuan limited liability company, and sodium benzoate is purchased from the magnificent Zhi Bo Science and Technology Ltd. in Beijing, 200# solvent Oil is purchased from Hualun Chemical Co., Ltd., Jiangsu, and 150# solvent naphtha is purchased from Hualun Chemical Co., Ltd., Jiangsu, and petroleum ether is purchased from western Gansu Province Chemical inc, ethyl acetate are purchased from Xilong Chemical Co., Ltd.
Embodiment 1
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:0.5, the weight ratio of water and formaldehyde For 2.5:1.
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed, Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate The weight ratio of ester APEO is 1:2:0.05.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 4:1 with 2000 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 4.3 by pH value, buffering Pair total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour, It is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;At room temperature, will Concentration is that the hydrochloric acid of 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min of stirring Speed is uniformly mixed, and obtains the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the third material is handled 2 Hour, it obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Into 4 materials be added sodium lignin sulfonate, Aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials and sulfomethylated lignin The weight ratio of sour sodium, aluminum magnesium silicate and ethylene glycol is 1:0.01:0.005:0.05.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron of the present embodiment.Wherein, Lambda-cyhalothrin microcapsule suspension and the weight ratio of lufenuron suspension agent, sodium lignin sulfonate are 1:0.3:0.05.
Embodiment 2
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:1, and the weight ratio of water and formaldehyde is 4:1。
Gamma cyhalothrin, 150# solvent naphtha and sodium lignin sulfonate are uniformly mixed, gamma cyhalothrin is obtained Missible oil, wherein the weight ratio of the gamma cyhalothrin, 150# solvent naphtha and sodium lignin sulfonate is 1:0.5:0.1.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 2:1 with 1500 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 3 by pH value, buffering pair Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour, with 1100 revs/min of mixing speed is uniformly mixed, and obtains the second material that pH value is adjusted to 6;At room temperature, by concentration Hydrochloric acid for 6 weight % is evenly added in above-mentioned second material in 1 hour, mixed with 1300 revs/min of mixing speed It closes uniformly, obtains the third material that pH value is adjusted to 3;Under conditions of 50 DEG C, the third material is handled 4 hours, is obtained 7 are adjusted to 4 materials and by the pH value of the 4 materials;Neopelex, xanthan are added into 4 materials Glue and glycerine are uniformly mixed, obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials and detergent alkylate sulphur The weight ratio of sour sodium, xanthan gum and glycerine is 1:0.05:0.01:0.1.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron of the present embodiment.Wherein, Lambda-cyhalothrin microcapsule suspension and the weight ratio of lufenuron suspension agent, sodium lignin sulfonate are 1:0.5:0.1.
Embodiment 3
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 72 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:1.5, and the weight ratio of water and formaldehyde is 5:1。
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed, Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate The weight ratio of ester APEO is 1:3:0.15.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 3:1 with 2500 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 3.6 by pH value, buffering Pair total concentration be 0.55 weight % acetic acid-sodium acetate buffer solution, above-mentioned first object is evenly added in 1.5 hours In material, it is uniformly mixed with 1200 revs/min of mixing speed, obtains the second material that pH value is adjusted to 4.5;In room temperature condition Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1 hour, with 1400 revs/min Mixing speed is uniformly mixed, and obtains the third material that pH value is adjusted to 3.5;Under conditions of 45 DEG C, by the third material Processing 5 hours, obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Sulfomethylated lignin is added into 4 materials Sour sodium, aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials and wood The weight ratio of quality sodium sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.2:0.015:0.2.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron of the present embodiment.Wherein, Lambda-cyhalothrin microcapsule suspension and the weight ratio of lufenuron suspension agent, sodium lignin sulfonate are 1:0.8:1.
Embodiment 4
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:2, and the weight ratio of water and formaldehyde is 6:1。
Gamma cyhalothrin, petroleum ether and lauryl sodium sulfate are uniformly mixed, gamma cyhalothrin cream is obtained Oil, wherein the weight ratio of the gamma cyhalothrin, petroleum ether and lauryl sodium sulfate is 1:5:0.2.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 5:1 with 3000 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 4.5 by pH value, buffering Pair total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour, It is uniformly mixed with 1200 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.5;At room temperature, will Concentration is that the hydrochloric acid of 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1500 revs/min of stirring Speed is uniformly mixed, and obtains the third material that pH value is adjusted to 3.7;Under conditions of 60 DEG C, the third material is handled 2 Hour, it obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Aliphatic alcohol polyethenoxy is added into 4 materials Ether, bentonite and 1,2-PD are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials and rouge The weight ratio of fat alcohol polyoxyethylene ether, bentonite and 1,2- propylene glycol is 1:0.2:0.02:0.15.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron of the present embodiment.Wherein, Lambda-cyhalothrin microcapsule suspension and the weight ratio of lufenuron suspension agent, sodium lignin sulfonate are 1:1:2.
Embodiment 5
Melamine, formaldehyde and water are mixed, are 7.5 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains three Paracyanogen amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:0.1, the weight of water and formaldehyde Than for 2:1.
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed, Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate The weight ratio of ester APEO is 1:0.1:0.01.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 1:1 with 2000 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 4.5 by pH value, buffering Pair total concentration be 2 weight % citrate-phosphate disodium hydrogen buffer solution, above-mentioned first is evenly added in 1 hour In material, it is uniformly mixed with 1100 revs/min of mixing speed, obtains the second material that pH value is adjusted to 7;In room temperature condition Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1300 revs/min Mixing speed be uniformly mixed, obtain the third material that pH value is adjusted to 3.5;Under conditions of 60 DEG C, by the third object Material processing 2 hours, obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Lignin is added into 4 materials Sodium sulfonate, aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials with The weight ratio of sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.02:0.001:0.02.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron of the present embodiment.Wherein, Lambda-cyhalothrin microcapsule suspension and the weight ratio of lufenuron suspension agent, sodium lignin sulfonate are 1:0.2:0.5.
Embodiment 6
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:0.2, the weight ratio of water and formaldehyde For 2.5:1.
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained, In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 4:1 with 2000 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 4.5 by pH value, buffering Pair total concentration be 2 weight % acetic acid-sodium acetate buffer solution, above-mentioned first material is evenly added in 0.5 hour In, it is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;In room temperature condition Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min Mixing speed be uniformly mixed, obtain the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, by the third object Material processing 2 hours, obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Lignin is added into 4 materials Sodium sulfonate, aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials with The weight ratio of sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.15:0.002:0.04.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron of the present embodiment.Wherein, Lambda-cyhalothrin microcapsule suspension and the weight ratio of lufenuron suspension agent, sodium lignin sulfonate are 1:0.1:0.01.
Embodiment 7
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:0.2, the weight ratio of water and formaldehyde For 2.5:1.
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained, In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 4:1 with 2000 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 4.5 by pH value, buffering Pair total concentration be 2 weight % acetic acid-sodium acetate buffer solution, above-mentioned first material is evenly added in 0.5 hour In, it is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;In room temperature condition Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min Mixing speed be uniformly mixed, obtain the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, by the third object Material processing 2 hours, obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Lignin is added into 4 materials Sodium sulfonate, aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials with The weight ratio of sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.15:0.002:0.04.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro- The weight ratio of capsule suspending agent and lufenuron suspension agent, sodium lignin sulfonate is 1:0.3:0.03.
Embodiment 8
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine Amine-formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and melamine is 1:0.2, the weight ratio of water and formaldehyde For 2.5:1.
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained, In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate be by weight 4:1 with 2000 revs/min of mixing speed is uniformly mixed, and obtains first material;It then at room temperature, is 4.5 by pH value, buffering Pair total concentration be 2 weight % acetic acid-sodium acetate buffer solution, above-mentioned first material is evenly added in 0.5 hour In, it is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;In room temperature condition Under, the hydrochloric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min Mixing speed be uniformly mixed, obtain the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, by the third object Material processing 2 hours, obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Lignin is added into 4 materials Sodium sulfonate, aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials with The weight ratio of sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.4:0.03:0.2.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro- The weight ratio of capsule suspending agent and lufenuron suspension agent, sodium lignin sulfonate is 1:0.1:0.01.
Embodiment 9
Urea, formaldehyde and water are mixed, are 7.5 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains urea-first Urea formaldehyde performed polymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:2, and the weight ratio of water and formaldehyde is 2.6:1.
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed, Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate The weight ratio of ester APEO is 1:2.5:0.05.
It is by weight 4:1 with 2000 by urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate Rev/min mixing speed be uniformly mixed, obtain first material;It then at room temperature, is 4.5 by pH value, buffering pair Total concentration is acetic acid-sodium acetate buffer solution of 2 weight %, is evenly added in above-mentioned first material in 1.5 hours, It is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;At room temperature, will Concentration is that the hydrochloric acid of 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min of stirring Speed is uniformly mixed, and obtains the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the third material is handled 2 Hour, it obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Into 4 materials be added sodium lignin sulfonate, Aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials and sulfomethylated lignin The weight ratio of sour sodium, aluminum magnesium silicate and ethylene glycol is 1:0.01:0.004:0.05.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro- The weight ratio of capsule suspending agent and lufenuron suspension agent, sodium lignin sulfonate is 1:1:0.05.
Embodiment 10
Urea, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains urea-formaldehyde Resin prepolymer aqueous solution, wherein the molar ratio of formaldehyde and urea is 1:1, and the weight ratio of water and formaldehyde is 2.8:1.
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed, Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate The weight ratio of ester APEO is 1:1.5:0.06.
It is by weight 3:1 with 2000 by urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate Rev/min mixing speed be uniformly mixed, obtain first material;It then at room temperature, is 3.6 by pH value, buffering pair Total concentration is the citric acid-sodium citrate buffer of 4 weight %, is evenly added in above-mentioned first material in 1 hour, It is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;At room temperature, will Concentration is that the phosphoric acid of 4 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min of stirring Speed is uniformly mixed, and obtains the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, the third material is handled 2 Hour, it obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Into 4 materials be added sodium lignin sulfonate, Aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials and sulfomethylated lignin The weight ratio of sour sodium, aluminum magnesium silicate and ethylene glycol is 1:0.02:0.005:0.05.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro- The weight ratio of capsule suspending agent and lufenuron suspension agent, sodium lignin sulfonate is 1:0.3:0.03.
Embodiment 11
Benzoguanamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 2h under the conditions of being 70 DEG C, obtains benzene generation Melamine formaldehyde resin performed polymer aqueous solution, wherein the molar ratio of formaldehyde and benzoguanamine is 1:0.5, water and formaldehyde Weight ratio be 2.8:1.
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed, Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate The weight ratio of ester APEO is 1:2:0.06.
It is by weight 3:1 by benzoguanamine-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate It is uniformly mixed with 2000 revs/min of mixing speed, obtains first material;It then at room temperature, is 4 by pH value, buffering Pair total concentration be 4 weight % citric acid-sodium citrate buffer, above-mentioned first object is evenly added in 1 hour In material, it is uniformly mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2;In room temperature condition Under, the sulfuric acid that concentration is 5 weight % is evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min Mixing speed be uniformly mixed, obtain the third material that pH value is adjusted to 3.2;Under conditions of 60 DEG C, by the third object Material processing 2 hours, obtains 4 materials and the pH value of the 4 materials is adjusted to 7;Lignin is added into 4 materials Sodium sulfonate, aluminum magnesium silicate and ethylene glycol are uniformly mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein 4 materials with The weight ratio of sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.03:0.005:0.05.
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with lufenuron suspension agent, sodium lignin sulfonate is added And water, it stirs evenly, obtains gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro- The weight ratio of capsule suspending agent and lufenuron suspension agent, sodium lignin sulfonate is 1:0.15:0.05.
Comparative example 1
The difference from embodiment 1 is that adjusting pH value without acetic acid-sodium acetate buffer solution, directly after obtaining first material It connects and uses concentration that the pH value of material is adjusted to 3.2 for the hydrochloric acid of 5 weight %.
Comparative example 2
The difference from embodiment 1 is that after obtaining first material, using pH value for the total concentration of 4.4, buffering pair is 2 weights After material pH value is adjusted to 4.4 by acetic acid-sodium acetate buffer solution of amount %, without the step of adjusting pH value for the second time.
Comparative example 3
The difference from embodiment 1 is that concentration is used to be adjusted to the pH value of third material for the hydrochloric acid of 5 weight % 2。
Comparative example 4
By weight by gamma cyhalothrin, 200# solvent naphtha, sorbitan monostearate polyoxyethylene ether and water Than for 1:0.6:0.1: being uniformly mixed, obtain gamma cyhalothrin aqueous emulsion, it is outstanding that method same as Example 1 prepares lufenuron Gamma cyhalothrin aqueous emulsion with lufenuron suspension agent is to mix by floating agent by weight, obtain gamma cyhalothrin with The micro- suspoemulsion of lufenuron.
Comparative example 5
By weight by gamma cyhalothrin, 200# solvent naphtha, sorbitan monostearate polyoxyethylene ether and water Than being uniformly mixed for 1:0.5:0.1:5, gamma cyhalothrin aqueous emulsion is obtained.
Comparative example 6
By the lufenuron (content 95%) of 20 weight %, the lauryl sodium sulfate of 2 weight %, 6 weight % it is wooden Plain sodium sulfonate, the organic silicon defoamer of 0.2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight % Sodium benzoate and the water of 60 weight % be sufficiently mixed, disperse, be passed through sand mill after being uniformly dispersed and be sanded, is sanded to average Suspension of the partial size less than 5 microns, obtains lufenuron suspension agent.
Testing example 1
This testing example is for gamma cyhalothrin and Acarus tritici obtained in testing example 1-11 and comparative example 1-3 The height of gamma cyhalothrin obtained in urea microcapsule suspension-suspendinagent agent and comparative example 4 and the micro- suspoemulsion of lufenuron, comparative example 5 Imitate the heat storage stability and low-temperature stability of the lufenuron suspension agent of lambda-cyhalothrin aqueous emulsion and comparative example 6.
Heat storage stability test: by gamma cyhalothrin and lufenuron obtained in embodiment 1-11 and comparative example 1-3 Gamma cyhalothrin obtained in microcapsule suspension-suspendinagent agent and comparative example 4 and the micro- suspoemulsion of lufenuron, comparative example 5 it is efficient Lambda-cyhalothrin aqueous emulsion and the lufenuron suspension agent of comparative example 6 are fitted into container, and the constant temperature of (54 ± 2) DEG C is placed in after sealing It in baking oven, is taken out after standing 14 days, according to GB/T14825-2006 standard, measures suspensibility, the results are shown in Table 1.
Low-temperature stability measurement: by gamma cyhalothrin and lufenuron obtained in embodiment 1-11 and comparative example 1-3 Gamma cyhalothrin obtained in microcapsule suspension-suspendinagent agent and comparative example 4 and the micro- suspoemulsion of lufenuron, comparative example 5 it is efficient Lambda-cyhalothrin aqueous emulsion and the lufenuron suspension agent of comparative example 6 are fitted into container, and sealing is placed in (0 ± 2) DEG C refrigerator, 1h is kept, stirs primary, each 15s at interval of 15min, observation appearance has unchanged, continues to place 7 days in (0 ± 2) DEG C, so It is taken out after being placed in standing recovery under room temperature afterwards, according to GB/T14825-2006 standard, measures suspensibility, the results are shown in Table 1.
Table 1
As it can be seen from table 1 the gamma cyhalothrin and lufenuron micro-capsule that preparation method provided by the invention obtains are outstanding Floating-suspending agent has good thermal storage stability and low tempertaure storage stability.
Testing example 2
This testing example is to gamma cyhalothrin obtained in embodiment 1-11, comparative example 1-3 and lufenuron micro-capsule The efficient chlorine fluorine cyanogen of gamma cyhalothrin obtained in suspension-suspending agent, comparative example 4 and the micro- suspoemulsion of lufenuron, comparative example 5 Pyrethroids aqueous emulsion and the lufenuron suspension agent of comparative example 6 test the control efficiency of wild cabbage plutella xylostella on wild cabbage.Before test A certain amount of distilled water is added, stirs evenly, is adjusted respectively by efficient chlorine fluorine cyanogen obtained in embodiment 1-11, comparative example 1-3 It is gamma cyhalothrin obtained in pyrethroids and lufenuron microcapsule suspension-suspendinagent agent, comparative example 4 and the micro- suspoemulsion of lufenuron, right Activity component concentration in the gamma cyhalothrin aqueous emulsion of ratio 5 and the lufenuron suspension agent of comparative example 6 is 10 weight %.
Test site: Weifang City, Shandong Province, experimental plot are many years wild cabbage planting base, and experimental plot topography is flat, in fertility Deng earth in quality.Wild cabbage routinely production management in area's is managed everywhere in after application.
Specific steps include, and are 30kg/ mus according to formulation rate using knapsack sprayer, by embodiment 1-11, comparison Efficient chlorine fluorine cyanogen obtained in gamma cyhalothrin obtained in example 1-3 and lufenuron microcapsule suspension-suspendinagent agent, comparative example 4 The lufenuron suspension agent medical fluid of pyrethroids and the micro- suspoemulsion of lufenuron, the gamma cyhalothrin aqueous emulsion of comparative example 5 and comparative example 6 It carries out the page to the cabbage plant of each growing area respectively to be sprayed, blank control group is using equivalent clear water to the wild cabbage in growing area It is spraying that plant carries out the page.
10 days, 20 days, the 30 days and 50 days investigation wild cabbage plutella xylostella control efficiency after application, specific test method according to " pesticide field efficacy medicine test criterion " carries out.For each treatment region using random 5 points samplings, each the investigation of processing cell 25 clumps sweet Indigo plant investigates each treatment region wild cabbage plutella xylostella control efficiency, calculates the death rate by formula (1) and calculates corrected mortality, knot by formula (2) Fruit is as shown in table 2.
Concrete outcome is shown in Table 2.
Table 2
Testing example 3
This testing example is to gamma cyhalothrin obtained in embodiment 1-11, comparative example 1-3 and lufenuron micro-capsule The efficient chlorine fluorine cyanogen of gamma cyhalothrin obtained in suspension-suspending agent, comparative example 4 and the micro- suspoemulsion of lufenuron, comparative example 5 Pyrethroids aqueous emulsion and the lufenuron suspension agent of comparative example 6 test the control efficiency of aleyrodid on Chinese cabbage, aphid.Add before test Enter a certain amount of distilled water, stir evenly, adjusts gamma cyhalothrin and lice obtained in embodiment 1-11, comparative example 1-3 Gamma cyhalothrin obtained in mite urea microcapsule suspension-suspending agent, comparative example 4 and the micro- suspoemulsion of lufenuron, comparative example 5 Activity component concentration in the lufenuron suspension agent of gamma cyhalothrin aqueous emulsion and comparative example 6 is 10 weight %.
Test site: Hebei province's Dingzhou City.The plot topography is flat, and fertility is preferable.Area Chinese cabbage is managed everywhere in after application Routinely production management.
Specific steps include, and are 30kg/ mus according to spouting liquid using knapsack sprayer, by embodiment 1-11, comparison Efficient chlorine fluorine cyanogen obtained in gamma cyhalothrin obtained in example 1-3 and lufenuron microcapsule suspension-suspendinagent agent, comparative example 4 The lufenuron suspension agent medical fluid of pyrethroids and the micro- suspoemulsion of lufenuron, the gamma cyhalothrin aqueous emulsion of comparative example 5 and comparative example 6 It is uniformly sprayed on the Chinese cabbage plant of each growing area respectively, blank control group plants the Chinese cabbage in growing area using equivalent clear water Strain is sprayed, and when application, is blocked neighboring community with plastic film, is prevented medicament from interfering with each other.
10 days, 20 days, 30 days and 50 days investigation aleyrodids, the prevention and control of aphids effects after application, specific test method is according to " agriculture Medicine field control effectiveness test criterion " it carries out.Each treatment region investigates 25 plants of Chinese cabbages using random 5 points samplings, each processing cell, adjusts Each treatment region aleyrodid, prevention and control of aphids effect are looked into, calculate the death rate by formula (1) and calculates corrected mortality, concrete outcome by formula (2) It is shown in Table 3:
Table 3
From table 2 and 3 as can be seen that the preparation method that the disclosure provides passes through two step section pH value, turn in specific stirring The gamma cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent being prepared under the reaction conditions such as speed, emulsifier, solvent, energy Prevent and treat the effect of crop pests with enough obtaining slow release long-acting.And the gamma cyhalothrin and lufenuron micro-capsule of this method preparation Suspension-suspending agent effect is much better than gamma cyhalothrin aqueous emulsion single dose, lufenuron suspension agent single dose.Height of the invention Lambda-cyhalothrin and lufenuron microcapsule suspension-suspendinagent agent are imitated relative to other of gamma cyhalothrin and lufenuron dosage form, tool Have the characteristics that the lasting period long, so as to reduce times for spraying and dosage, save the cost, wherein the organic solvent contained is few, it can To reduce the pollution to environment.
The preferred embodiment of the disclosure is described in detail above, still, during the disclosure is not limited to the above embodiment Detail a variety of simple variants can be carried out to the technical solution of the disclosure in the range of the technology design of the disclosure, this A little simple variants belong to the protection scope of the disclosure.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the disclosure to it is various can No further explanation will be given for the combination of energy.
In addition, any combination can also be carried out between a variety of different embodiments of the disclosure, as long as it is without prejudice to originally Disclosed thought equally should be considered as disclosure disclosure of that.

Claims (10)

1. a kind of method for preparing the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron, which is characterized in that should Method includes the following steps:
A, be by weight (1-5) with efficient cyhalothrin emulsifiable concentrate by amino resins performed polymer aqueous solution: 1 mixes, and obtains One material;
B, the first material obtained in step a is mixed with buffer solution, obtains second material, the pH of the second material Value is 4-7;
C, the second material obtained in step b is mixed with acid solution, obtains third material, the pH of the third material Value is 3-4;
D, third material stirring 2-5 hours obtained in step c are obtained the 4th under conditions of temperature is 40-70 DEG C Material;
It e, is by weight 1:(0.1- by the 4 materials obtained in step d and lufenuron suspension agent and emulsifying dispersant 1): (0.01-2) mixing obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron.
2. the method according to claim 1, wherein the amino resins performed polymer aqueous solution in step a is The progress prepolymerization of amino-containing compound, formaldehyde and water is obtained;The molar ratio of the amino-containing compound and formaldehyde is (0.1-2): 1, the weight ratio of water and formaldehyde is (2-6): 1;The amino-containing compound includes urea, melamine and benzene generation At least one of melamine;The prepolymerized condition includes: that pH value is 8-10, and temperature is 60-80 DEG C, time 0.5- 3 hours.
3. method according to claim 1 or 2, which is characterized in that the efficient cyhalothrin emulsifiable concentrate in step a contains There are gamma cyhalothrin, organic solvent and emulsifier;The organic solvent includes petroleum ether, ethyl acetate, methyl oleate, two At least one of toluene and solvent naphtha, the emulsifier include sodium lignin sulfonate, lauryl sodium sulfate, detergent alkylate Sodium sulfonate, fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, loses styrene-maleic anhydride copolymer In water sorbitol monostearate polyoxyethylene ether, sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate at least It is a kind of;The weight ratio of the gamma 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 contain buffering pair, it is described Buffering is to including at least one of citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate.
5. the method according to claim 1, wherein the acid solution in step c include hydrochloric acid, sulfuric acid, At least one of phosphoric acid, acetic acid and ammonium chloride.
6. according to claim 1, method described in any one of 2,4 and 5, which is characterized in that be blended in described in step a It is carried out under conditions of stirring, the speed of the stirring is 1500-3000 revs/min;The item for being blended in stirring in step b It is carried out under part, the speed of the stirring is 1000-1200 revs/min;The mixing in step c under stirring conditions into Row, the speed of the stirring are 1200-1500 revs/min.
7. the method according to claim 1, wherein this method further includes, in step e, by the 4 materials After being mixed with the first dispersing agent, thickener and antifreezing agent, then mix with the emulsifying dispersant;First dispersing agent includes ten Dialkyl benzene sulfonic acids sodium, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, the condensation of benzyl naphthalenesulfonateformaldehyde formaldehyde Object, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, At least one of nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether;The thickener include aluminum magnesium silicate, xanthan gum, At least one of polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black;The antifreezing agent includes second two At least one of alcohol, 1,2- propylene glycol, glycerine and urea;The 4 materials and first dispersing agent, the thickening The weight ratio of agent and the antifreezing agent is 1:(0.01-0.2): (0.001-0.02): (0.02-0.15).
8. method according to claim 1 or claim 7, which is characterized in that in step e, the 4 materials and the lufenuron Suspending agent and the emulsifying dispersant are 1:(0.2-0.5 by weight): (0.02-0.05) mixing.
9. according to the method described in claim 8, it is characterized in that, the Acarus tritici suspending agent in step e is by by lufenuron It is obtained after being mixed with the second dispersing agent and water, the lufenuron is 1:(0.2- with the weight ratio of second dispersing agent and water 0.5): (1.5-3): second dispersing agent includes neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonic acid Sodium formaldehyde condensation product, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation are wooden At least one in plain sodium sulfonate, Succinate sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether Kind, the emulsifying dispersant includes neopelex, sodium methylene bis-naphthalene sulfonate, the condensation of 1- methyl naphthalene sulfonic acid sodium formaldehyde Object, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar are condensed sodium lignin sulfonate, fourth At least one of two acid esters sodium sulfonates, pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether.
10. the micro-capsule containing gamma cyhalothrin and lufenuron of the preparation of method described in any one of claim 1-9 Suspension-suspending agent.
CN201811378078.1A 2018-11-19 2018-11-19 A kind of method and its microcapsule suspension-suspendinagent agent preparing the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and lufenuron Pending CN109479894A (en)

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