CN106386800A - Preparation method of cyhalothrin and chlorfluazuron microcapsule suspension-suspension and microcapsule suspension-suspension - Google Patents
Preparation method of cyhalothrin and chlorfluazuron microcapsule suspension-suspension and microcapsule suspension-suspension Download PDFInfo
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- CN106386800A CN106386800A CN201610799962.7A CN201610799962A CN106386800A CN 106386800 A CN106386800 A CN 106386800A CN 201610799962 A CN201610799962 A CN 201610799962A CN 106386800 A CN106386800 A CN 106386800A
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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
- A01N25/02—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
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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
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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
- A01N47/00—Biocides, 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
- A01N47/08—Biocides, 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
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/34—Ureas 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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- 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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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Abstract
The invention relates to a preparation method of a cyhalothrin and chlorfluazuron microcapsule suspension-suspension and the microcapsule suspension-suspension. The method comprises the following steps: a, an aqueous solution of an amino resin prepolymer is mixed with cyhalothrin emulsifiable concentrate, and a first material is obtained; b, the first material is mixed with a buffer solution, and a second material with the pH value being 5-7 is obtained; the second material is mixed with an acid solution, and a third material with the pH value being 3-4 is obtained; d, the third material is processed at the temperature of 40-70 DEG C for 2-7 h, and a fourth material is obtained; e, the fourth material is mixed with a chlorfluazuron suspension and an emulsion dispersant, and the cyhalothrin and chlorfluazuron microcapsule suspension-suspension is obtained. The cyhalothrin and chlorfluazuron microcapsule suspension-suspension prepared with the method has better storage stability and can control crop pests in a slow-release and long-acting manner, the use times and use amount are reduced, the cost is saved, and environmental pollution is reduced.
Description
Technical field
A kind of it relates to pesticide field, in particular it relates to gamma cyhalothrin chlorfluazuron microcapsule suspension-suspension
The preparation method of agent and microcapsule suspension-suspendinagent agent.
Background technology
Gamma cyhalothrin is a kind of broad spectrum pesticide, and it can suppress the conduction at insecticide neural axon position, to insecticide
There is the effect walked quickly and kept away, knock down and kill it is also possible to mixed with most of antibacterial, Insecticides (tech) ＆ Herbicides (tech), all have preferably anti-
Control effect.Its effective ingredient of traditional formulations of pesticide easily in external environment, such as sunshine, lost efficacy in the presence of soil acidity or alkalinity etc.,
Lasting period is short, thus reduces the preventive effect of pesticide.Existing preparation containing gamma cyhalothrin is all containing organic in a large number on the market
Solvent, pollutes environment.And gamma cyhalothrin single dose also has certain limitation, it is compounded with chlorfluazuron not only can be effective
Improve actual prevention effect, reduce dosage, reduces cost, delay drug-fast generation, but also pesticide species can be extended
Service life, reduce pollution to environment.
Microcapsule suspending agent utilizes natural or synthesis macromolecular material to form nucleocapsid structure small container, can be by agriculture
Medicated bag cover wherein and suspend with water in, be few, little to the operator's harm Novel rural medicament of a kind of lasting period length, organic solvent amount
Type.The lambda-cyhalothrin microcapsule suspension that traditional preparation methods obtain, is susceptible to reunion, solidification phenomenon, leads to be difficult
Storage, preventing and treating crop pests effect difference is it is difficult to meet the preparation demand of preventing and treating crop pests pesticide.
Therefore, in the urgent need to developing the novel built dosage form of a kind of gamma cyhalothrin and chlorfluazuron, to be stored
The insecticide containing gamma cyhalothrin and chlorfluazuron that is stable and can effectively preventing and treating crop pests.
Content of the invention
The purpose of the disclosure be provide a kind of easy storage and the high gamma cyhalothrin chlorfluazuron microcapsule suspension of drug effect-
The preparation method of suspending agent and the gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent prepared by the method.
To achieve these goals, disclosure first aspect：A kind of gamma cyhalothrin chlorfluazuron microcapsule is provided to hang
The preparation method of floating-suspending agent, the method comprises the 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 described first material obtaining in step a and buffering
Solution mixes, and obtains second material, the pH value of described second material is 5-7；C, by the described second material obtaining in step b with
Acid solution mixes, and obtains 3 material, the pH value of described 3 material is 3-4；D, under conditions of temperature is for 40-70 DEG C will
The described 3 material obtaining in step c processes 2-7 hour, obtains 4 materials；E, by described 4th thing obtaining in step d
Material and chlorfluazuron suspending agent and emulsifying dispersant are by weight for 1：(0.1-1)：(0.01-2) mix, obtain efficient cyhalothrin
Ester chlorfluazuron microcapsule suspension-suspendinagent agent.
Preferably, the described amino resins performed polymer aqueous solution in step a is to carry out the compound containing amino and formaldehyde
Prepolymerization obtains, and the described compound containing amino is (0.1-2) with the mol ratio of formaldehyde：1, the weight ratio of described water and formaldehyde
For (2-7)：1, the described compound containing amino includes at least one in carbamide, tripolycyanamide and benzoguanamine, described
Prepolymerized condition includes：PH value is 8-10, and temperature is 60-80 DEG C, and the time is 0.5-3 hour.
Preferably, the described efficient cyhalothrin emulsifiable concentrate in step a contains gamma cyhalothrin, organic solvent and breast
Agent, described organic solvent includes at least one in petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and solvent naphtha, described
Emulsifying agent include sodium lignin sulfonate, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, styrene-maleic anhydride copolymer,
Fatty alcohol-polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate polyoxyethylene ether,
At least one in sodium laurylsulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate, described gamma cyhalothrin, organic
The weight of solvent and emulsifying agent is than for 1：(0.1-5)：(0.01-0.2).
Preferably, the described buffer solution in step b contain buffering right, described buffering to include citric acid-sodium citrate,
At least one in citrate-phosphate disodium hydrogen and acetic acid-sodium acetate.
Preferably, the described acid solution in step c includes in hydrochloric acid, sulphuric acid, phosphoric acid, acetic acid and ammonium chloride at least one
Kind.
Preferably, carry out under conditions of being blended in stirring described in step a, the speed of described stirring is 1500-3000
Rev/min；Carry out under conditions of being blended in stirring described in step b, the speed of described stirring is 1000-1200 rev/min；
Carry out under conditions of being blended in stirring described in step c, the speed of described stirring is 1200-1500 rev/min.
Preferably, the method also includes, and in step e, described 4 materials is mixed with dispersant, thickening agent and antifreezing agent
Afterwards, then with described emulsifying dispersant mix, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent；Described dispersion
Agent includes dodecylbenzene sodium sulfonate, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl LOMAR PWA EINECS 246-676-2 first
Aldehyde condensate, sodium lignin sulfonate, desaccharide sodium lignin sulfonate, desaccharide are condensed sodium lignin sulfonate, Succinate sodium sulfonate, draw
Open at least one in powder, NPE and fatty alcohol-polyoxyethylene ether；Described thickening agent includes Magnesiumaluminumsilicate, Huang
At least one in virgin rubber, Polyethylene Glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon；Described antifreezing agent includes
At least one in ethylene glycol, 1,2- propylene glycol, glycerol and carbamide；Described 4 materials and dispersant, thickening agent and antifreeze
The weight of agent is than for 1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15).
Preferably, in the described chlorfluazuron suspending agent in step e, the mean diameter of chlorfluazuron microgranule is 1-5 micron.
Preferably, the described emulsifying dispersant in step e include dodecylbenzene sodium sulfonate, sodium methylene bis-naphthalene sulfonate,
1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desaccharide sodium lignin sulfonate,
Desaccharide condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, NPE and fatty alcohol-polyoxyethylene ether
In at least one.
Disclosure second aspect：There is provided the gamma cyhalothrin chlorfluazuron of the method preparation of disclosure first aspect micro-
Capsule suspension-suspending agent.
By technique scheme, the gamma cyhalothrin chlorfluazuron microcapsule using disclosed method preparation hangs
Floating-suspending agent has preferable bin stability, being capable of slow release long-acting ground preventing and treating crop pests, reduction times for spraying and medication
Amount, cost-effective, alleviate the pollution to environment.
Other feature and advantage of the disclosure will be described in detail in subsequent specific embodiment part.
Specific embodiment
Specific embodiment of this disclosure is described in detail below.It should be appreciated that it is described herein concrete
Embodiment is merely to illustrate and explains the disclosure, is not limited to the disclosure.
Disclosure first aspect：A kind of preparation side of gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent is provided
Method, the method comprises the steps：A, amino resins performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are by weight
(1-5)：1 mixing, obtains first material；B, the described first material obtaining in step a is mixed with buffer solution, obtain second
Material, the pH value of described second material is 5-7；C, the described second material obtaining in step b is mixed with acid solution, obtain
3 material, the pH value of described 3 material is 3-4；D, will obtain in step c under conditions of temperature is for 40-70 DEG C described in
3 material processes 2-7 hour, obtains 4 materials；E, by the described 4 materials obtaining in step d and chlorfluazuron suspending agent
With emulsifying dispersant by weight for 1：(0.1-1)：(0.01-2) mix, obtain gamma cyhalothrin chlorfluazuron microcapsule and hang
Floating-suspending agent.
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's-cyano group-(3- Phenoxyphenyl) methyl ester trade name, English name
For λ-Cyhalothrin, molecular formula is C23H19ClF3NO3, relative molecular weight is 449.9, and No. CAS is 91465-08-6, structure
Shown in formula such as formula (1).
In the disclosure, chlorfluazuron is compound 1- [3,5- bis- chloro- 4- (3- chloro- 5- trifluoromethyl -2- pyridyloxy) benzene
Base] -3- (2,6- difluoro benzoyl) urea trade name, English name is Chlorfluazuron, and molecular formula is
C20H9Cl3F5N3O3, relative molecular weight is 540.7, and No. CAS is 71422-67-8, shown in structural formula such as formula (2).
According to the disclosure in a first aspect, the preparation method of described amino resins performed polymer aqueous solution in step a is permissible
For preparation method well known to those skilled in the art, the disclosure has no particular limits to it.Under preferable case, described amino tree
Fat performed polymer aqueous solution can be the compound containing amino, formaldehyde and water to be carried out prepolymerization obtain, the described change containing amino
Compound can be (0.1-2) with the mol ratio of formaldehyde：1, described water can be (2-7) with the mass ratio of formaldehyde：1.Described containing ammonia
The compound of base can include at least one in carbamide, tripolycyanamide and benzoguanamine, and described prepolymerized condition can
To include：PH value is 8-10, and temperature is 60-80 DEG C, and the time is 0.5-3 hour.
According to the disclosure in a first aspect, the preparation method of described efficient cyhalothrin emulsifiable concentrate in step a can be
Preparation method well known to those skilled in the art, the disclosure has no particular limits to it.Under preferable case, described efficient chlorine fluorine
Cyano chrysanthemate cream can contain gamma cyhalothrin, organic solvent and emulsifying agent, by gamma cyhalothrin, organic solvent and
Emulsifying agent mixing can get described efficient cyhalothrin emulsifiable concentrate.Wherein, described organic solvent can be able to dissolve for various
With dilution gamma cyhalothrin material it is preferable that described organic solvent can include petroleum ether, ethyl acetate, Oleic acid first
At least one in ester, dimethylbenzene and solvent naphtha.Described emulsifying agent can for the various materials with emulsification it is preferable that
Described emulsifying agent can include sodium lignin sulfonate, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, styrene-maleic acid
Anhydride copolymer, fatty alcohol-polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate gather
At least one in oxygen vinyl Ether, sodium laurylsulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate.Micro- for improving further
The particle diameter distribution of microcapsule and clad ratio in capsule suspending agent, thus improve the bin stability of microcapsule suspending agent further, preferably
In the case of, the weight ratio of described gamma cyhalothrin, organic solvent and emulsifying agent can be 1：(0.1-5)：(0.01-0.2),
The organic solvent content of this proportioning is few, can reduce the pollution to environment.
According to the disclosure in a first aspect, clad ratio, the uniformity and softgel shell compactness in order to improve microcapsule, thus entering
One step improve gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent bin stability so as to be not susceptible to reunite and
Solidification phenomenon, and there is good crop pests prevention effect, after obtaining first material, it is respectively adopted buffer solution and acidity
Solution carries out the regulation of pH to it.First described first material is mixed with buffer solution, obtain the second thing that pH value is 5-7
Material；Then described second material is mixed with acid solution, obtain the 3 material that pH value is 3-4.
According to the disclosure in a first aspect, the implication of described buffer solution in step b is ripe for those skilled in the art
Know, be containing buffering to solution.Under preferable case, described buffering is to inclusion citric acid-sodium citrate, citrate-phosphate hydrogen
At least one in disodium and acetic acid-sodium acetate.In order that the pH value of second material is adjusted to 5-7, the pH of described buffer solution
Value can be 3-5.5.In described buffer solution buffering to total concentration can be 1-5 weight %.
According to the disclosure in a first aspect, described acid solution in step c can for this area conventional there is acidity
Material.Under preferable case, described acid solution includes at least one in hydrochloric acid, sulphuric acid, phosphoric acid, acetic acid and ammonium chloride.Institute
The concentration stating acid solution can be 0.5-8 weight %.
According to the first aspect of the invention, suitable reaction condition can carry microcapsule clad ratio, improve particle diameter distribution with
And the thickness of softgel shell, and then improve the bin stability of microcapsule suspending agent.Under preferable case, it is blended in described in step a and stirs
Carry out under conditions of mixing, the speed of described stirring can be 1500-3000 rev/min.It is blended in stirring described in step b
Under the conditions of carry out, the speed of described stirring can be 1000-1200 rev/min.It is blended in the condition of stirring described in step c
Under carry out, the speed of described stirring can be 1200-1500 rev/min.
According to the disclosure in a first aspect, those skilled in the art should know, when insecticide is in acid or alkali
During property, not only can hinder the growth of plant, will also result in the pollution of environment.Therefore, by 4 materials and chlorfluazuron suspending agent and
Before emulsifying dispersant is mixed, it is in neutrality that described 4 materials Acidity of Aikalinity is preferably.Therefore, the method for disclosure first aspect
Also include the step adjusting the pH value of described 4 materials to neutrality, the method adjusting pH value can be the routine side of this area
Method, will not be described here.
According to the disclosure in a first aspect, assemble in order to avoid microcapsule occurs, precipitation, the phenomenon such as hardened, the method also wraps
Include, in step e, after can first described 4 materials being mixed with dispersant, thickening agent and antifreezing agent, then with described emulsion dispersion
Agent mixes, and obtains gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Described dispersant can include detergent alkylate
Sodium sulfonate, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, lignin
Sodium sulfonate, desaccharide sodium lignin sulfonate, desaccharide condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, polyoxyethylene nonyl phenyl
At least one in vinyl Ether and fatty alcohol-polyoxyethylene ether.Described thickening agent can include Magnesiumaluminumsilicate, xanthan gum, poly- second two
At least one in alcohol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon.Described antifreezing agent can include ethylene glycol,
At least one in 1,2- propylene glycol, glycerol and carbamide.Described 4 materials and the weight of dispersant, thickening agent and antifreezing agent
Ratio can be 1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15).
According to the disclosure in a first aspect, the preparation method of described chlorfluazuron suspending agent in step e can be this area
Preparation method known to technical staff, the disclosure has no particular limits to it.For example, it is possible to by chlorfluazuron and dispersant and water
It is sufficiently mixed, disperses, so that chlorfluazuron is present in aqueous solution with aerosol form, then sand milling makes the flat of chlorfluazuron microgranule
All particle diameter is 1-5 micron, obtains chlorfluazuron suspending agent.Described dispersant can include dodecylbenzene sodium sulfonate, di-2-ethylhexylphosphine oxide
Sodium naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desaccharide are wooden
Plain sodium sulfonate, desaccharide condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, NPE and fatty alcohol
At least one in polyoxyethylene ether.Described chlorfluazuron can be 1 with the weight ratio of dispersant, water：(0.2-0.5)：(1.5-
3).Additionally, defoamer, thickening agent, antifreezing agent and at least one of the preservatives can also be included in described chlorfluazuron suspending agent.
Described defoamer can be polyether antifoam agent and/or organic silicon defoamer.Described thickening agent can include Magnesiumaluminumsilicate, xanthan
At least one in glue, Polyethylene Glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon etc..Described antifreezing agent is permissible
Including at least one in ethylene glycol, 1,2- propylene glycol, glycerol and carbamide.Described preservative can include sodium benzoate, benzene
At least one in formic acid, sorbic acid and potassium sorbate.
According to the disclosure in a first aspect, in order to improve gamma cyhalothrin chlorfluazuron microcapsule suspension-outstanding further
The bin stability of floating agent, the described emulsifying dispersant in step e can include dodecylbenzene sodium sulfonate, di-2-ethylhexylphosphine oxide naphthalene sulphur
Sour sodium, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desaccharide sulfomethylated lignin
Sour sodium, desaccharide condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, NPE and fatty alcohol polyoxy
At least one in vinyl Ether.
Disclosure second aspect：There is provided the gamma cyhalothrin chlorfluazuron of the method preparation of disclosure first aspect micro-
Capsule suspension-suspending agent.
Further describe the disclosure by the following examples, be not limited to the disclosure.
In embodiment and comparative example, gamma cyhalothrin is purchased from Huifeng Agricultural Chemistry Co., Ltd., Jiangsu；Chlorfluazuron (contains
Measure as 95%) it is purchased from Zhejiang Heben Science ＆ Technology Co., Ltd.；Tripolycyanamide is purchased from Beijing Chemical Plant；Carbamide is purchased from Beijing Chemical Plant；
Benzoguanamine is purchased from Beijing Chemical Plant；Formaldehyde is purchased from Beijing Chemical Plant；Sorbitan monostearate polyoxyethylene ether
Purchased from Nanjing Teva-Chem. Co., Ltd.；Sodium lauryl sulphate is purchased from Beijing Science and Technology Ltd. of Zhong Chuan HTC；Sulfomethylated lignin
Sour sodium is purchased from Beijing Science and Technology Ltd. of Zhong Chuan HTC；Dodecylbenzene sodium sulfonate is purchased from the limited public affairs of Beijing Zhong Chuan HTC science and technology
Department；Polyvinyl alcohol is purchased from Zhengzhou Ao Cai industrial chemicals company limited；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 company limited；Bentonite is purchased from Anji County, Zhejiang Province Gekko Swinhonis organobentonite company limited；
Organic silicon defoamer is purchased from Shanghai Mitugao New Material Group；Ethylene glycol, glycerol and 1,2- propylene glycol are purchased from Beijing Chemical Plant；
Xanthan gum is purchased from Shandong Zhong Xuan limited company；Sodium benzoate is purchased from Beijing magnificent Zhi Bo Science and Technology Ltd.；200# solvent
Oil is purchased from Hualun Chemical Co., Ltd., Jiangsu；150# solvent naphtha is purchased from Hualun Chemical Co., Ltd., Jiangsu；Petroleum ether is purchased from western Gansu Province
Chemical inc；Ethyl acetate is purchased from Xilong Chemical Co., Ltd.
Embodiment 1
Tripolycyanamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-for-aldehyde resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:0.5, the weight ratio of water and formaldehyde is
2.8:1.
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:2.5:0.05.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 4：1 with
2000 revs/min of mixing speed mix homogeneously, obtains first material；Then at ambient temperature, pH value is 4.5, buffers
To total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in 1 hour in above-mentioned first material,
With 1000 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2；At ambient temperature, will
Concentration is that the hydrochloric acid of 5 weight % was evenly added in above-mentioned second material, with 1200 revs/min of stirring in 1.5 hours
Speed mix homogeneously, obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, described 3 material is processed 2
Hour, obtain 4 materials and adjust the pH value of described 4 materials to 7；To in 4 materials add sodium lignin sulfonate,
Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials and sulfomethylated lignin
The weight of sour sodium, Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.01：0.005：0.05.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.3:0.05.
Embodiment 2
Tripolycyanamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-for-aldehyde resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:1, the weight ratio of water and formaldehyde is
3.5:1.
By gamma cyhalothrin, 150# solvent naphtha and sodium lignin sulfonate mix homogeneously, obtain gamma cyhalothrin
Cream, wherein, the weight of described gamma cyhalothrin, 150# solvent naphtha and sodium lignin sulfonate is than for 1:0.5:0.1.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 2：1 with
1500 revs/min of mixing speed mix homogeneously, obtains first material；Then at ambient temperature, by pH value be 3, buffering right
Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in 1 hour in above-mentioned first material, with
1100 revs/min of mixing speed mix homogeneously, obtains the second material that pH value is adjusted to 6；At ambient temperature, by concentration
Hydrochloric acid for 6 weight % was evenly added in above-mentioned second material in 1 hour, was mixed with 1300 revs/min of mixing speed
Close uniformly, obtain the 3 material that pH value is adjusted to 3；Under conditions of 50 DEG C, described 3 material is processed 4 hours, obtains
Adjust to 7 to 4 materials and by the pH value of described 4 materials；Dodecylbenzene sodium sulfonate, xanthan is added in 4 materials
Glue and glycerol, mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials and detergent alkylate sulphur
The weight of sour sodium, xanthan gum and glycerol is than for 1：0.05：0.01：0.1.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.5:0.1.
Embodiment 3
Tripolycyanamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-for-aldehyde resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:1.5, the weight ratio of water and formaldehyde is
5:1.
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:3:0.15.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 3：1 with
2500 revs/min of mixing speed mix homogeneously, obtains first material；Then at ambient temperature, pH value is 3.8, buffers
To total concentration be 0.55 weight % acetic acid-sodium acetate buffer solution, be evenly added to above-mentioned first thing in 1.5 hours
In material, with 1200 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 5.5；In room temperature condition
Under, the hydrochloric acid that concentration is 5 weight % was evenly added in above-mentioned second material in 1 hour, with 1400 revs/min stir
Mix speed mix homogeneously, obtain the 3 material that pH value is adjusted to 3.5；Under conditions of 45 DEG C, at described 3 material
Reason 6 hours, obtains 4 materials and adjusts the pH value of described 4 materials to 7；Lignin sulfonic acid is added in 4 materials
Sodium, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials with wooden
The weight of plain sodium sulfonate, Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.1：0.015：0.15.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.8:1.
Embodiment 4
Tripolycyanamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-for-aldehyde resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:2, the weight of water and formaldehyde is than for 7:
1.
By gamma cyhalothrin, petroleum ether and sodium lauryl sulphate mix homogeneously, obtain gamma cyhalothrin breast
Oil, wherein, the weight of described gamma cyhalothrin, petroleum ether and sodium lauryl sulphate is than for 1:5:0.2.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 5：1 with
3000 revs/min of mixing speed mix homogeneously, obtains first material；Then at ambient temperature, pH value is 4.5, buffers
To total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in 1 hour in above-mentioned first material,
With 1200 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.5；At ambient temperature, will
Concentration is that the hydrochloric acid of 5 weight % was evenly added in above-mentioned second material, with 1500 revs/min of stirring in 1.5 hours
Speed mix homogeneously, obtains the 3 material that pH value is adjusted to 3.7；Under conditions of 60 DEG C, described 3 material is processed 2
Hour, obtain 4 materials and adjust the pH value of described 4 materials to 7；Aliphatic alcohol polyethenoxy is added in 4 materials
Ether, bentonite and 1,2-PD mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials and fat
The weight of fat polyoxyethylenated alcohol, bentonite and 1,2- propylene glycol is than for 1：0.2：0.02：0.15.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:1:2.
Embodiment 5
Tripolycyanamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-for-aldehyde resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:0.1, the weight ratio of water and formaldehyde is
2:1.
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:0.1:0.01.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 1：1 with
2000 revs/min of mixing speed mix homogeneously, obtains first material；Then at ambient temperature, pH value is 4.5, buffers
To total concentration be 2 weight % citrate-phosphate disodium hydrogen buffer solution, be evenly added to above-mentioned first in 1 hour
In material, with 1100 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 7；In room temperature condition
Under, the hydrochloric acid that concentration is 5 weight % was evenly added in above-mentioned second material in 1.5 hours, with 1300 revs/min
Mixing speed mix homogeneously, obtains the 3 material that pH value is adjusted to 4；Under conditions of 60 DEG C, at described 3 material
Reason 2 hours, obtains 4 materials and adjusts the pH value of described 4 materials to 7；Lignin sulfonic acid is added in 4 materials
Sodium, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials with wooden
The weight of plain sodium sulfonate, Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.02：0.001：0.02.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.2:0.5.
Embodiment 6
Tripolycyanamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-for-aldehyde resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:0.2, the weight ratio of water and formaldehyde is
2.5:1.
By gamma cyhalothrin, ethyl acetate and polyvinyl alcohol uniformly, obtain efficient cyhalothrin emulsifiable concentrate, its
In, the weight of described gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is than for 1:1.5:0.02.
By melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 4：1 with
2000 revs/min of mixing speed mix homogeneously, obtains first material；Then at ambient temperature, pH value is 4.5, buffers
To total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added to above-mentioned first material in 0.5 hour
In, with 1000 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2；In room temperature condition
Under, the hydrochloric acid that concentration is 5 weight % was evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min
Mixing speed mix homogeneously, obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, by described 3 material
Process 2 hours, obtain 4 materials and adjust the pH value of described 4 materials to 7；Sulfomethylated lignin is added in 4 materials
Sour sodium, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials with wood
The weight of quality sodium sulfonate, Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.15：0.002：0.04.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.1:0.01.
Embodiment 7
Carbamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains urea-formaldehyde
Resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of carbamide:2, the weight of water and formaldehyde is than for 2.8:1.
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:2.5:0.05.
By urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 4：1 with 2000 turns/
The mixing speed mix homogeneously of minute, obtains first material；Then at ambient temperature, by pH value be 4.5, buffering to always dense
Spend the acetic acid-sodium acetate buffer solution for 2 weight %, be evenly added in 1.5 hours in above-mentioned first material, with 1000
Rev/min mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2；At ambient temperature, concentration is
The hydrochloric acid of 5 weight % was evenly added in above-mentioned second material in 1.5 hours, was mixed with 1200 revs/min of mixing speed
Close uniformly, obtain the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, described 3 material is processed 2 hours,
Obtain 4 materials and adjust the pH value of described 4 materials to 7；Sodium lignin sulfonate, aluminium silicate is added in 4 materials
Magnesium and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials and sodium lignin sulfonate,
The weight of Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.01：0.005：0.05.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.3:0.05.
Embodiment 8
Carbamide, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains urea-formaldehyde
Resin prepolymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of carbamide:1, the weight of water and formaldehyde is than for 2.8:1.
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:2:0.06.
By urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 3：1 with 2000 turns/
The mixing speed mix homogeneously of minute, obtains first material；Then at ambient temperature, by pH value be 3.6, buffering to always dense
Spend the citric acid-sodium citrate buffer for 4 weight %, be evenly added in 1 hour in above-mentioned first material, with
1000 revs/min of mixing speed mix homogeneously, obtains the second material that pH value is adjusted to 6.2；At ambient temperature, will be dense
Spend the phosphoric acid for 4 weight % to be evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min of stirring speed
Degree mix homogeneously, obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, described 3 material is processed 2 little
When, obtain 4 materials and adjust the pH value of described 4 materials to 7；Sodium lignin sulfonate, silicon is added in 4 materials
Sour magnalium and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials and lignin sulfonic acid
The weight of sodium, Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.02：0.004：0.04.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.2:0.03.
Embodiment 9
Benzoguanamine, formaldehyde and water are mixed, is 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains benzene
Substituted melamine-formaldehyde resin performed polymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of benzoguanamine:0.5, Shui Hejia
The weight of aldehyde is than for 2.8:1.
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:2:0.06.
By benzoguanamine-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight for 4：1
With 2000 revs/min of mixing speed mix homogeneously, obtain first material；Then at ambient temperature, pH value is 4, buffers
To total concentration be 4 weight % citric acid-sodium citrate buffer, be evenly added to above-mentioned first thing in 1 hour
In material, with 1000 revs/min of mixing speed mix homogeneously, obtain the second material that pH value is adjusted to 6.2；In room temperature condition
Under, the sulphuric acid that concentration is 5 weight % was evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min
Mixing speed mix homogeneously, obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, by described 3 material
Process 2 hours, obtain 4 materials and adjust the pH value of described 4 materials to 7；Sulfomethylated lignin is added in 4 materials
Sour sodium, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain lambda-cyhalothrin microcapsule suspension, wherein, 4 materials with wood
The weight of quality sodium sulfonate, Magnesiumaluminumsilicate and ethylene glycol is than for 1：0.03：0.005：0.05.
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with chlorfluazuron suspending agent, add sodium lignin sulfonate
And water, stir, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.Wherein, gamma cyhalothrin is micro-
Capsule suspending agent and chlorfluazuron suspending agent, the weight of sodium lignin sulfonate are than for 1:0.15:0.04.
Comparative example 1
Difference with embodiment 1 is, after obtaining first material, adjusts pH value without acetic acid-sodium acetate buffer solution, directly
Connect the hydrochloric acid being 5 weight % using concentration and the pH value of material is adjusted to 3.2.
Comparative example 2
Difference with embodiment 1 is, after obtaining first material, using pH value be 4.5, buffering to total concentration be 2 weights
After material pH value is adjusted to 4.5 by the acetic acid-sodium acetate buffer solution of amount %, the step that do not carry out second regulation pH value.
Comparative example 3
Difference with embodiment 1 is, using the hydrochloric acid that concentration is 5 weight %, the pH value of 3 material is adjusted to 2.
Comparative example 4
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein, described gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight of ester APEO is than for 1:2.5:0.05.Method same as Example 1 prepares fluazinam suspending agent, by efficient chlorine fluorine
Cyano chrysanthemate cream and fluazinam suspending agent are by weight for 1:0.3 mixing, obtains the micro- outstanding breast of gamma cyhalothrin chlorfluazuron
Agent.
Comparative example 5
By gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether mix homogeneously,
Obtain gamma cyhalothrin oil phase, water is slowly dropped in gamma cyhalothrin oil phase, stirs in Deca, and add second
Glycol and xanthan gum, obtain gamma cyhalothrin aqueous emulsion.Wherein, described gamma cyhalothrin, 200# solvent naphtha, dehydration
The weight of sorbitol monostearate polyoxyethylene ether, water, ethylene glycol and xanthan gum is than for 1:2.5:0.05:1.2:0.005:
0.001.
Comparative example 6
By the chlorfluazuron of 26.3 weight % (content is 95%), the sodium lauryl sulphate of 2 weight %, 6 weight % wood
Quality 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
The sodium benzoate of amount % is sufficiently mixed, disperses with the water of 60 weight %, is passed through sand mill and carries out sand milling, sand milling is extremely after being uniformly dispersed
The suspension that mean diameter is less than 5 microns, obtains chlorfluazuron suspending agent.
Testing example 1
This testing example is used for the gamma cyhalothrin fluorine pyridine obtain in testing example 1-9 and comparative example 1-3
The heat storage stability of the micro- suspension emulsion of gamma cyhalothrin chlorfluazuron obtaining in urea microcapsule suspension-suspendinagent agent and comparative example 4
And low-temperature stability.
Heat storage stability is tested：Will be micro- for the gamma cyhalothrin chlorfluazuron obtaining in embodiment 1-9 and comparative example 1-3
The micro- suspension emulsion of gamma cyhalothrin chlorfluazuron obtaining in capsule suspension-suspending agent and comparative example 4 loads in container, after sealing
It is positioned in the constant temperature oven of (54 ± 2) DEG C, standing was taken out after 14 days, according to GB/T14825-2006 standard, measure suspensibility,
The results are shown in Table 1.
Low-temperature stability measures：Will be micro- for the gamma cyhalothrin chlorfluazuron obtaining in embodiment 1-9 and comparative example 1-3
The micro- suspension emulsion of gamma cyhalothrin chlorfluazuron obtaining in capsule suspension-suspending agent and comparative example 4 loads in container, after sealing
It is placed in (0 ± 2) DEG C refrigerator, keeps 1h, stir once at interval of 15min, each 15s, observation outward appearance has unchanged, (0
± 2) a DEG C continuation is placed 7 days, then takes out after being placed in standing recovery under room temperature condition, according to GB/T14825-2006 standard, surveys
Determine suspensibility, the results are shown in Table 1.
Table 1
As it can be seen from table 1 the gamma cyhalothrin chlorfluazuron microcapsule that the preparation method that the present invention provides obtains hangs
Floating-suspending agent has good thermal storage stability and low tempertaure storage stability.
Testing example 2
This testing example is hanged to the gamma cyhalothrin chlorfluazuron microcapsule obtaining in embodiment 1-9, comparative example 1-3
The micro- suspension emulsion of gamma cyhalothrin chlorfluazuron that obtains in floating-suspending agent, comparative example 4, the efficient cyhalothrin of comparative example 5
The chlorfluazuron suspending agent of ester aqueous emulsion and comparative example 6 is tested to the prevention effect of Folium Allii tuberosi root maggot on Folium Allii tuberosi.Add before test
A certain amount of distilled water, stirs, and adjusts the gamma cyhalothrin that will obtain in embodiment 1-9, comparative example 1-3 respectively
The micro- suspension emulsion of gamma cyhalothrin chlorfluazuron that obtains in chlorfluazuron microcapsule suspension-suspendinagent agent, comparative example 4, comparative example 5
Activity component concentration in the chlorfluazuron suspending agent of gamma cyhalothrin aqueous emulsion and comparative example 6 is 10 weight %.
Test site：Dezhou City Shandong Province Ningjin County Dong Cuicun, experimental plot is Folium Allii tuberosi planting base for many years, experimental plot physical features
Flat, middle fertility, earth in quality.Each treatment region Folium Allii tuberosi routinely production management after dispenser.
Concrete steps include, and using knapsack sprayer, are 30kg/ mu according to formulation rate, by embodiment 1-9, comparative example
The efficient cyhalothrin obtaining in the gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent that obtains in 1-3, comparative example 4
The chlorfluazuron suspending agent medicinal liquid of the micro- suspension emulsion of ester chlorfluazuron, the gamma cyhalothrin aqueous emulsion of comparative example 5 and comparative example 6 divides
The other Folium Allii tuberosi plant to each growing area carries out pouring root, and blank control group is entered to the Folium Allii tuberosi plant in growing area using equivalent clear water
Row pouring root.
10 days after dispenser, 20 days, 30 days and 50 days investigation Folium Allii tuberosi root maggot prevention effect, concrete test method according to《Agriculture
Medicine field control effectiveness test criterion》Carry out.Each treatment region adopts random 5 points of samplings, and each processes cell and investigates 25 clumps of Folium Allii tuberosi, adjusts
Look into each treatment region Folium Allii tuberosi root maggot prevention effect, calculate mortality rate and by formula (2) calculating corrected mortality, result such as table 2 by formula (1)
Shown.
Concrete outcome is shown in Table 2.
Table 2
Testing example 3
This testing example is hanged to the gamma cyhalothrin chlorfluazuron microcapsule obtaining in embodiment 1-9, comparative example 1-3
The micro- suspension emulsion of gamma cyhalothrin chlorfluazuron that obtains in floating-suspending agent, comparative example 4, the efficient cyhalothrin of comparative example 5
The chlorfluazuron suspending agent of ester aqueous emulsion and comparative example 6 Chinese cabbage is served Kattapillar, the prevention effect of aphid is tested.Add before test
Enter a certain amount of distilled water, stir, the gamma cyhalothrin fluorine pyridine obtaining in regulation embodiment 1-9, comparative example 1-3
The micro- suspension emulsion of gamma cyhalothrin chlorfluazuron that obtains in urea microcapsule suspension-suspendinagent agent, comparative example 4, comparative example 5 efficient
Activity component concentration in the chlorfluazuron suspending agent of lambda-cyhalothrin aqueous emulsion and comparative example 6 is 10 weight %.
Test site：Hebei province Baoding Xinshi District Xi great Yuan village.This plot physical features is flat, and fertility is preferable.After dispenser
Each treatment region Chinese cabbage routinely production management.
Concrete steps include, and using knapsack sprayer, are 30kg/ mu according to spouting liquid, by embodiment 1-9, comparative example
The efficient cyhalothrin obtaining in the gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent that obtains in 1-3, comparative example 4
The chlorfluazuron suspending agent medicinal liquid of the micro- suspension emulsion of ester chlorfluazuron, the gamma cyhalothrin aqueous emulsion of comparative example 5 and comparative example 6 divides
Uniformly do not spray on the Chinese cabbage plant of each growing area, blank control group uses equivalent clear water to the Chinese cabbage plant in growing area
Sprayed, during dispenser, blocked neighbor cell with plastic sheeting, prevent medicament from interfering.
10 days after dispenser, 20 days, 30 days and 50 days investigation Pieris rapae, control of aphids effect, concrete test method according to
《Pesticide field efficacy medicine test criterion》Carry out.Each treatment region adopts random 5 points of samplings, and each processes cell and investigates 25 plants in vain
Dish, investigates each treatment region Pieris rapae, control of aphids effect, calculates mortality rate and by formula (2) calculating corrected mortality by formula (1),
Concrete outcome is shown in Table 3：
Table 3
From table 2 and table 3 as can be seen that the preparation method that the disclosure provides passes through two step section pH value, stir specific
The gamma cyhalothrin chlorfluazuron microcapsule suspension-suspension preparing under the reaction conditions such as rotating speed, emulsifying dispersant, solvent
Agent, prevents and treats the effect of crop pests with can obtaining slow release long-acting.And the gamma cyhalothrin fluorine pyridine of this method preparation
Urea microcapsule suspension-suspendinagent agent effect is all much better than gamma cyhalothrin aqueous emulsion single dose, chlorfluazuron suspending agent single dose.This public affairs
The gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent opened is with respect to other agent of gamma cyhalothrin chlorfluazuron
Type, has the characteristics that the lasting period is long, thus times for spraying and dosage can be reduced, cost-effective, the organic solvent wherein containing
Few, the pollution to environment can be reduced.
The preferred implementation of the disclosure described in detail above, but, the disclosure is not limited in above-mentioned embodiment
Detail, in the range of the technology design of the disclosure, multiple simple variant can be carried out with technical scheme of this disclosure, this
A little simple variant belong to the protection domain of the disclosure.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the disclosure to various can
The compound mode of energy no longer separately illustrates.
Additionally, combination in any can also be carried out between the various different embodiment of the disclosure, as long as it is without prejudice to this
Disclosed thought, it equally should be considered as disclosure disclosure of that.
Claims (10)
1. a kind of preparation method of gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent is it is characterised in that the method bag
Include following steps：
A, by amino resins performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate by weight being (1-5)：1 mixing, obtains the
One material；
B, the described first material obtaining in step a is mixed with buffer solution, obtain second material, the pH of described second material
It is worth for 5-7；
C, the described second material obtaining in step b is mixed with acid solution, obtain 3 material, the pH of described 3 material
It is worth for 3-4；
D, under conditions of temperature is for 40-70 DEG C, the described 3 material obtaining in step c is processed 2-7 hour, obtain the 4th
Material；
E, by the described 4 materials obtaining in step d and chlorfluazuron suspending agent and emulsifying dispersant by weight for 1：(0.1-
1)：(0.01-2) mix, obtain gamma cyhalothrin chlorfluazuron microcapsule suspension-suspendinagent agent.
2. method according to claim 1, wherein, the described amino resins performed polymer aqueous solution in step a is by containing ammonia
The compound of base, formaldehyde and water carry out what prepolymerization obtained, and the described compound containing amino is (0.1- with the mol ratio of formaldehyde
2)：1, described water is (2-7) with the weight ratio of formaldehyde：1, the described compound containing amino includes carbamide, tripolycyanamide and benzene generation
At least one in tripolycyanamide, described prepolymerized condition includes：PH value is 8-10, and temperature is 60-80 DEG C, and the time is 0.5-
3 hours.
3. method according to claim 1, wherein, the described efficient cyhalothrin emulsifiable concentrate in step a contains efficient chlorine
Flucythrinate, organic solvent and emulsifying agent, described organic solvent includes petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and molten
Agent oil at least one, described emulsifying agent include sodium lignin sulfonate, sodium lauryl sulphate, dodecylbenzene sodium sulfonate,
Styrene-maleic anhydride copolymer, fatty alcohol-polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, Sorbitan
At least one in alcohol monostearate ester APEO, sodium laurylsulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate,
The weight of described gamma cyhalothrin, organic solvent and emulsifying agent is than for 1：(0.1-5)：(0.01-0.2).
4. method according to claim 1, wherein, the described buffer solution in step b contain buffering right, described buffering right
Including at least one in citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate.
5. method according to claim 1, wherein, the described acid solution in step c includes hydrochloric acid, sulphuric acid, phosphoric acid, second
At least one in acid and ammonium chloride.
6. method according to claim 1, wherein, is carried out under conditions of being blended in stirring described in step a, described stirs
The speed mixed is 1500-3000 rev/min；Carry out under conditions of being blended in stirring described in step b, the speed of described stirring
For 1000-1200 rev/min；Carry out under conditions of being blended in stirring described in step c, the speed of described stirring is 1200-
1500 revs/min.
7. method according to claim 1, wherein, the method also includes, in step e, by described 4 materials and dispersion
After agent, thickening agent and antifreezing agent mixing, then mix with described emulsifying dispersant, obtain gamma cyhalothrin chlorfluazuron microcapsule
Suspension-suspending agent；Described dispersant includes dodecylbenzene sodium sulfonate, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonic acid sodium first
Aldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desaccharide sodium lignin sulfonate, desaccharide condensation sulfomethylated lignin
At least one in sour sodium, Succinate sodium sulfonate, pull open powder, NPE and fatty alcohol-polyoxyethylene ether；Institute
State thickening agent to include in Magnesiumaluminumsilicate, xanthan gum, Polyethylene Glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon
At least one；Described antifreezing agent includes at least one in ethylene glycol, 1,2- propylene glycol, glycerol and carbamide；Described 4th thing
Material and the weight of dispersant, thickening agent and antifreezing agent ratio is for 1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15).
8. method according to claim 1, wherein, in the described chlorfluazuron suspending agent in step e, chlorfluazuron microgranule flat
All particle diameter is 1-5 micron.
9. method according to claim 1, wherein, the described emulsifying dispersant in step e includes DBSA
Sodium, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, lignin sulfonic acid
Sodium, desaccharide sodium lignin sulfonate, desaccharide condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, Nonyl pheno
At least one in ether and fatty alcohol-polyoxyethylene ether.
10. the gamma cyhalothrin chlorfluazuron microcapsule suspension that in claim 1-9 prepared by the method described in any one-outstanding
Floating agent.
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