CN107494584A - A kind of microcapsule suspension suspending agent containing gamma cyhalothrin and Teflubenzuron and preparation method thereof - Google Patents
A kind of microcapsule suspension suspending agent containing gamma cyhalothrin and Teflubenzuron and preparation method thereof Download PDFInfo
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- CN107494584A CN107494584A CN201710633409.0A CN201710633409A CN107494584A CN 107494584 A CN107494584 A CN 107494584A CN 201710633409 A CN201710633409 A CN 201710633409A CN 107494584 A CN107494584 A CN 107494584A
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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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- 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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Abstract
The invention discloses a kind of microcapsule suspension suspending agent containing gamma cyhalothrin and Teflubenzuron and preparation method thereof, the preparation method comprises the following steps：S1, the mixed amino resin prepolymer aqueous solution and efficient cyhalothrin emulsifiable concentrate, obtain first material；S2, add cushioning liquid into first material and mix, obtain the second material that pH value is 57；S3, add acid solution into second material and mix, obtain the 3 material that pH value is 34；S4,3 material is stirred 27 hours under conditions of being 40 70 DEG C in temperature, obtain 4 materials；S5,4 materials are mixed with Teflubenzuron suspending agent and emulsifying dispersant, obtain the microcapsule suspension suspending agent containing gamma cyhalothrin and Teflubenzuron.The microcapsule suspension suspending agent containing gamma cyhalothrin and Teflubenzuron that the preparation method of the present invention obtains has preferable bin stability, can prevent and treat crop pests slow release long-acting.
Description
Technical field
The present invention relates to technical field of pesticide, in particular it relates to a kind of micro-capsule containing gamma cyhalothrin and Teflubenzuron
Suspension-suspending agent and preparation method thereof.
Background technology
Gamma cyhalothrin is a kind of broad spectrum pesticide, and it can suppress the conduction at insect neural axon position, to insect
Have the function that to walk quickly and keep away, knock down and kill, can also be mixed with most of bactericide, Insecticides (tech) ＆ Herbicides (tech), have preferably anti-
Control effect.Its active ingredient of traditional formulations of pesticide easily fails in the presence of external environment, such as sunshine, soil acidity or alkalinity etc.,
Lasting period is short, thus reduces the preventive effect of agricultural chemicals.The existing preparation containing gamma cyhalothrin is containing a large amount of organic on the market
Solvent, pollute environment.Microcapsule suspending agent forms nucleocapsid structure small container using natural or synthesis high polymer material, can
So that agricultural chemicals cladding wherein and to be suspended with water, being that a kind of lasting period is long, organic solvent amount is few, it is small new that operator is endangered
The formulations of pesticide.The lambda-cyhalothrin microcapsule suspension that traditional preparation methods obtain, reunion, solidification phenomenon easily occurs, leads
Cause is not easy to store, and preventing and treating crop pests effect is poor, it is difficult to meets the preparation demand of preventing and treating crop pests agricultural chemicals.
Therefore, there is an urgent need to develop a kind of novel built formulation of gamma cyhalothrin and Teflubenzuron, to be stored
Stablize and can effectively prevent and treat the insecticide containing gamma cyhalothrin and Teflubenzuron of crop pests.
The content of the invention
It is an object of the invention to provide a kind of microcapsule suspension-suspendinagent agent and its system containing gamma cyhalothrin and Teflubenzuron
Preparation Method, and then the drug effect of the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron is obviously improved, and reduce it
Store difficulty.
On the one hand, the present invention provides a kind of preparation of the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron
Method, the preparation method comprise the following steps：S1, it is by weight (1-5)：The 1 mixed amino resin prepolymer aqueous solution and height
Cyhalothrin emulsifiable concentrate is imitated, obtains first material；Cushioning liquid is added in S2, the first material obtained to step S1 and is mixed
Close, obtain the second material that pH value is 5-7；Acid solution is added in S3, the second material obtained to step S2 and is mixed,
Obtain the 3 material that pH value is 3-4；S4, the 3 material for obtaining step S3 under conditions of being 40-70 DEG C in temperature
2-7 hours are stirred, obtain 4 materials；S5, it is 1 by weight：(0.1-1)：(0.01-2) step S4 is obtained described
4 materials mix with Teflubenzuron suspending agent and emulsifying dispersant, obtain the microcapsule suspension containing gamma cyhalothrin and Teflubenzuron-
Suspending agent.
Alternatively, the amino resins performed polymer aqueous solution described in step S1 passes through the compound containing amino, formaldehyde and water
What prepolymerization obtained, the compound containing amino includes at least one of urea, melamine and benzoguanamine, institute
The mol ratio for stating the compound containing amino and formaldehyde is (0.1-2)：1, the weight ratio of water and formaldehyde is (2-7)：1, the pre-polymerization
The condition of conjunction includes：PH value is 8-10, and temperature is 60-80 DEG C, and the time is 0.5-3 hours.
Alternatively, the efficient cyhalothrin emulsifiable concentrate described in step S1 contain gamma cyhalothrin, organic solvent and
Emulsifying agent, the weight ratio of the gamma cyhalothrin, the organic solvent and the emulsifying agent is 1：(0.1-5)：(0.01-
0.2), the organic solvent includes at least one of petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and solvent naphtha, described
Emulsifying agent include sodium lignin sulfonate, lauryl sodium sulfate, neopelex, styrene-maleic anhydride copolymer,
AEO, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate APEO,
At least one of sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate.
Alternatively, the buffering in the cushioning liquid described in step S2 is to including citric acid-sodium citrate, biphosphate
At least one of potassium-dipotassium hydrogen phosphate and acetic acid-sodium acetate.
Alternatively, the acid solution described in step S3 is included in hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid and ammonium chloride solution
It is at least one.
Alternatively, mixing is realized by being stirred under 1500-3000 revs/min of mixing speed in step S1；Step S2
In pass through under 1000-1200 revs/min of mixing speed stirring realize mixing；By at 1200-1500 revs/min in step S3
Mixing is realized in stirring under the mixing speed of clock；The speed stirred in step S4 is 200-1000 revs/min.
Alternatively, before the preparation method is additionally included in step S5 by the 4 materials and dispersant, thickener and
The step of antifreezing agent mixes；The weight ratio that the 4 materials mix with the dispersant, the thickener and the antifreezing agent
For 1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15)；The dispersant includes neopelex, methylene
Double sodium naphthalene sulfonates, 1- methyl naphthalene sulfonate formaldehyde condensates, 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, NPE and fat
At least one of alcohol APEO；The thickener includes Magnesiumaluminumsilicate, xanthans, polyethylene glycol, polyvinyl alcohol, carboxylic first
At least one of base cellulose, bentonite and white carbon；The antifreezing agent include ethylene glycol, 1,2- propane diols, glycerine and
At least one of urea.
Alternatively, the average grain diameter of Teflubenzuron particulate is 1-5 microns in the Teflubenzuron suspending agent described in step S5.
Alternatively, the emulsifying dispersant described in step S5 include neopelex, sodium methylene bis-naphthalene sulfonate,
1- methyl naphthalene sulfonate formaldehyde condensates, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate,
Desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, NPE and AEO
At least one of.
On the other hand, the present invention also provides contains gamma cyhalothrin and volt according to what described preparation method was prepared
The grand microcapsule suspension-suspendinagent agent of worm.
Have by what the preparation method of the present invention obtained containing the microcapsule suspension-suspendinagent agent of gamma cyhalothrin and Teflubenzuron
There is preferable bin stability, crop pests can be prevented and treated slow release long-acting, reduce times for spraying and dosage, save into
This, alleviates the pollution to environment.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
On the one hand, the present invention provides a kind of preparation of the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron
Method, the preparation method comprise the following steps：S1, can be by weight (1-5)：The 1 mixed amino resin prepolymer aqueous solution
With efficient cyhalothrin emulsifiable concentrate, first material is obtained；Buffering is added in S2, the first material that can be obtained to step S1
Solution simultaneously mixes, and obtains the second material that pH value is 5-7；Acid is added in S3, the second material that can be obtained to step S2
Property solution and mix, obtain the 3 material that pH value is 3-4；S4, step S3 is obtained under conditions of being 40-70 DEG C in temperature
The 3 material stirring 2-7 hours arrived, obtain 4 materials；S5, can be 1 by weight：(0.1-1)：(0.01-2)
The 4 materials that step S4 is obtained mix with Teflubenzuron suspending agent and emulsifying dispersant, obtain containing gamma cyhalothrin
With the microcapsule suspension-suspendinagent agent of Teflubenzuron.
In the present invention, 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 acids-cyano group-(3- Phenoxyphenyls) 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)：
In the present invention, Teflubenzuron, also known as fluorobenzene urea, chemical name be 1- (3,5- bis- chloro- 2,4- difluorophenyls) -3- (2,
6- difluoro benzoyls), English name teflubenzuron, molecular formula C14H6Cl2F4N2O2, relative molecular weight is
381.1, No. CAS is 83121-18-0, shown in structural formula such as formula (2)：
According to the present invention, the preparation method of the amino resins performed polymer aqueous solution described in step S1 can be art technology
Preparation method known to personnel, the present invention have no particular limits to it.Amino resins performed polymer described in step S1 is water-soluble
What liquid can be obtained by the compound containing amino, formaldehyde and water prepolymerization, the compound containing amino can include urea,
At least one of melamine and benzoguanamine, the mol ratio of the compound and formaldehyde containing amino can be
(0.1-2)：1, the weight ratio of water and formaldehyde can be (2-7)：1, the prepolymerized condition includes：PH value can be 8-10,
Temperature can be 60-80 DEG C, and the time can be 0.5-3 hours.
According to the present invention, the preparation method of efficient cyhalothrin emulsifiable concentrate described in step S1 can be people in the art
Preparation method known to member, the present invention have no particular limits to it.Under preferable case, the efficient cyhalothrin emulsifiable concentrate can
Containing gamma cyhalothrin, organic solvent and emulsifying agent, to be by the mixing of gamma cyhalothrin, organic solvent and emulsifying agent
It can obtain described efficient cyhalothrin emulsifiable concentrate.Wherein, the organic solvent can dissolve and dilute efficiently to be various
The material of lambda-cyhalothrin, it is preferable that the organic solvent can include petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and
At least one of solvent naphtha.The emulsifying agent can be the various materials with emulsification, it is preferable that the emulsifying agent can
With including sodium lignin sulfonate, lauryl sodium sulfate, neopelex, styrene-maleic anhydride copolymer, fat
Alcohol APEO, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate APEO, bay
At least one of alcohol sodium sulphate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate.Further to improve micro-capsule in microcapsule suspending agent
Particle diameter distribution and clad ratio, so as to further improve the bin stability of microcapsule suspending agent, under preferable case, it is described efficiently
The weight ratio of lambda-cyhalothrin, organic solvent and emulsifying agent can be 1：(0.1-5)：(0.01-0.2), the proportioning it is organic molten
Agent content is few, can reduce the pollution to environment.
According to the present invention, in order to improve the clad ratio of micro-capsule, the uniformity and softgel shell compactness, contain so as to further improve
The bin stability of the microcapsule suspension-suspendinagent agent of gamma cyhalothrin and Teflubenzuron, it is set to be not susceptible to reunite and solidify existing
As, and there is good crop pests prevention effect, after obtaining first material, cushioning liquid can be respectively adopted and acidity is molten
Liquid carries out pH regulation to it.It is possible, firstly, to which the first material is mixed with cushioning liquid, second that pH value is 5-7 is obtained
Material；It is then possible to which the second material is mixed with acid solution, the 3 material that pH value is 3-4 is obtained.
According to the present invention, the buffering in cushioning liquid described in step S2 is to that can include citric acid-sodium citrate, phosphorus
Acid dihydride potassium-at least one of dipotassium hydrogen phosphate and acetic acid-sodium acetate.In order that the pH value of second material can be adjusted smoothly
To 5-7, the pH value of the cushioning liquid can be 3-5.5, and the total concentration of the buffering pair in the cushioning liquid can be 1-5 weights
Measure %.
According to the present invention, the acid solution described in step S3 can be the conventional material with acidity in this area, excellent
In the case of choosing, at least one of hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid and ammonium chloride solution can be included, the acid solution it is dense
Degree can be 0.5-8 weight %.
According to the present invention, appropriate reaction condition can carry the clad ratio of micro-capsule, improve particle diameter distribution and the thickness of softgel shell
Degree, and then the bin stability of microcapsule suspending agent is improved, can be fast by the stirring at 1500-3000 revs/min in step S1
Mixing is realized in the lower stirring of degree；Mixing can be realized in step S2 by being stirred under 1000-1200 revs/min of mixing speed；
Mixing can be realized in step S3 by being stirred under 1200-1500 revs/min of mixing speed；The speed stirred in step S4
It can be 200-1000 revs/min.
According to the present invention, those skilled in the art should know, when insecticide is in acid or alkaline, not only can
The growth of plant is hindered, will also result in the pollution of environment.Therefore, 4 materials and Teflubenzuron suspending agent and emulsifying dispersant are entered
Before row mixing, the acid-base property of the 4 materials is preferably in neutrality.Therefore, preparation method of the invention is also included described in regulation
For the pH value of 4 materials to the step of neutrality, the method for adjusting pH value can be the conventional method of this area, will not be repeated here.
According to the present invention, phenomena such as assembling in order to avoid there is micro-capsule, precipitate, be hardened, the preparation method can also include
Before step S5 the step of the 4 materials are mixed with dispersant, thickener and antifreezing agent；The 4 materials with
The weight ratio of the dispersant, the thickener and antifreezing agent mixing can be 1：(0.01-0.2)：(0.001-0.02)：
(0.02-0.15)；The dispersant can include neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonic acids
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, NPE and AEO
Kind；The thickener can include Magnesiumaluminumsilicate, xanthans, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and
At least one of white carbon；The antifreezing agent can include at least one in ethylene glycol, 1,2- propane diols, glycerine and urea
Kind.
According to the present invention, the average grain diameter of Teflubenzuron particulate can be 1-5 in the Teflubenzuron suspending agent described in step S5
Micron.
The preparation method of Teflubenzuron suspending agent described in step S5 can be preparation method well known to those skilled in the art,
The present invention has no particular limits to it.For example, being sufficiently mixed, disperseing with dispersant and water by Teflubenzuron, make Teflubenzuron
It is present in aerosol form in the aqueous solution, then sand milling make it that the average grain diameter of Teflubenzuron particulate is 1-5 microns, is lied prostrate
The grand suspending agent of worm.The dispersant can include neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonic acid sodium
Formaldehyde condensation products, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation lignin
At least one of sodium sulfonate, Succinate sodium sulfonate, pull open powder, NPE and AEO.
The weight ratio of the Teflubenzuron and dispersant, water can be 1：(0.2-0.5)：(1.5-3).In addition, the Teflubenzuron suspending agent
In can also include defoamer, thickener, antifreezing agent and at least one of the preservatives.The defoamer can be that polyethers defoams
Agent and/or organic silicon defoamer.The thickener can include Magnesiumaluminumsilicate, xanthans, polyethylene glycol, polyvinyl alcohol, carboxylic first
At least one of base cellulose, bentonite and white carbon etc..The antifreezing agent can include ethylene glycol, 1,2- propane diols, third
At least one of triol and urea.The preservative can include in sodium benzoate, benzoic acid, sorbic acid and potassium sorbate
It is at least one.
According to the present invention, in order to further improve the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron
Bin stability, emulsifying dispersant described in step S5 can include neopelex, sodium methylene bis-naphthalene sulfonate,
1- methyl naphthalene sulfonate formaldehyde condensates, benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate,
Desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, NPE and AEO
At least one of.
On the other hand, the present invention also provides contains gamma cyhalothrin and volt according to what described preparation method was prepared
The grand microcapsule suspension-suspendinagent agent of worm.
The present invention is further described by the following examples, is not intended to limit the invention.
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
The amine-for-aldehyde resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and melamine is 1:0.5, the weight ratio of water and formaldehyde is
2.8:1。
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2.5:0.05.
It is 4 by weight by the melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with
2000 revs/min of mixing speed is well mixed, and obtains first material；Then at ambient temperature, it is 4.5 by pH value, buffering
To total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour,
It is well mixed with 1000 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.2；At ambient temperature, will
Concentration is that 5 weight % hydrochloric acid was evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min of stirring
Speed is well mixed, and obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, by the 3 material with 200
Rev/min speed stir 2 hours, obtain 4 materials and adjust the pH value of the 4 materials to 7；Into 4 materials
Add sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol to be well mixed, obtain lambda-cyhalothrin microcapsule suspension, wherein,
The weight ratio of 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.01：0.005：0.05.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds sodium lignin sulfonate
And water, stir, obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient cyhalothrin
The weight ratio of ester micro capsule suspending agent and Teflubenzuron suspending agent, sodium lignin sulfonate is 1:0.3:0.05.
Embodiment 2
Melamine, formaldehyde and water are mixed, are 9 in pH value, temperature reacts 1.5h under the conditions of being 75 DEG C, obtains melamine
The amine-for-aldehyde resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and melamine is 1:1, the weight ratio of water and formaldehyde is
3.5:1。
Gamma cyhalothrin, 150# solvent naphthas and sodium lignin sulfonate are well mixed, obtain gamma cyhalothrin
Missible oil, wherein, the weight ratio of the gamma cyhalothrin, 150# solvent naphthas and sodium lignin sulfonate is 1:0.5:0.1.
It is 2 by weight by the melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with
1500 revs/min of mixing speed is well mixed, and obtains first material；Then at ambient temperature, it 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 well mixed, and 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, by the 3 material with 1000 revs/min
Speed stir 4 hours, obtain 4 materials and adjust the pH value of the 4 materials to 7；Ten are added into 4 materials
Dialkyl benzene sulfonic acids sodium, xanthans and glycerine, it is well mixed, obtains lambda-cyhalothrin microcapsule suspension, wherein, the 4th
The weight ratio of material and neopelex, xanthans and glycerine is 1：0.05：0.01：0.1.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % di-2-ethylhexylphosphine oxide naphthalene sulfonic acids
Sodium, 0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % benzene first
Sour sodium and 60 weight % water are sufficiently mixed, disperseed, and being passed through sand mill after being uniformly dispersed is sanded, and is sanded small to average grain diameter
In 5 microns of suspension, Teflubenzuron suspending agent is obtained.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds sodium lignin sulfonate
And water, stir, obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient cyhalothrin
The weight ratio of ester micro capsule suspending agent and Teflubenzuron suspending agent, sodium lignin sulfonate is 1:0.5:0.1.
Embodiment 3
Melamine, formaldehyde and water are mixed, are 10 in pH value, temperature reacts 0.5h under the conditions of being 80 DEG C, obtains trimerization
Cyanamide-formaldehyde resin performed polymer the aqueous solution, wherein, the mol ratio of formaldehyde and melamine is 1:1.5, the weight ratio of water and formaldehyde
For 5:1.
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:3:0.15.
It is 3 by weight by the melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with
2500 revs/min of mixing speed is well mixed, and obtains first material；Then at ambient temperature, it is 3.8 by pH value, buffering
To total concentration be 0.55 weight % acetic acid-sodium acetate buffer solution, above-mentioned first thing was evenly added in 1.5 hours
In material, it is well mixed with 1200 revs/min of mixing speed, obtains 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 to be well mixed, obtain the 3 material that pH value is adjusted to 3.5；Under conditions of 45 DEG C, by the 3 material with
600 revs/min of speed stirs 6 hours, obtains 4 materials and adjusts the pH value of the 4 materials to 7；To the 4th thing
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are added in material to be well mixed, and obtain lambda-cyhalothrin microcapsule suspension, its
In, the weight ratio of 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.1：0.015：0.15.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds desugar sulfomethylated lignin
Sour sodium and water, stir, and obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient chlorine fluorine
The weight ratio of Cyano chrysanthemate microcapsule suspending agent and Teflubenzuron suspending agent, desugar sodium lignin sulfonate is 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
The amine-for-aldehyde resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and melamine is 1:2, the weight ratio of water and formaldehyde is 7:
1。
Gamma cyhalothrin, petroleum ether and lauryl sodium sulfate are well mixed, obtain gamma cyhalothrin breast
Oil, wherein, the weight ratio of the gamma cyhalothrin, petroleum ether and lauryl sodium sulfate is 1:5:0.2.
It is 5 by weight by the melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with
3000 revs/min of mixing speed is well mixed, and obtains first material；Then at ambient temperature, it is 4.5 by pH value, buffering
To total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1 hour,
It is well mixed with 1200 revs/min of mixing speed, obtains the second material that pH value is adjusted to 6.5；At ambient temperature, will
Concentration is that 5 weight % hydrochloric acid was evenly added in above-mentioned second material in 1.5 hours, with 1500 revs/min of stirring
Speed is well mixed, and obtains the 3 material that pH value is adjusted to 3.7；Under conditions of 60 DEG C, by the 3 material with 400
Rev/min speed stir 2 hours, obtain 4 materials and adjust the pH value of the 4 materials to 7；Into 4 materials
Add AEO, bentonite and 1,2-PD to be well mixed, obtain lambda-cyhalothrin microcapsule suspension,
Wherein, the weight ratio of 4 materials and AEO, bentonite and 1,2-PD is 1：0.2：0.02：0.15.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % Succinate sodium sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds succinate sulfonic acid
Sodium and water, stir, and obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient chlorine fluorine cyanogen
The weight ratio of chrysanthemum ester micro capsule suspending agent and Teflubenzuron suspending agent, Succinate sodium sulfonate is 1:1:2.
Embodiment 5
Melamine, formaldehyde and water are mixed, are 8.5 in pH value, temperature reacts 2h under the conditions of being 60 DEG C, obtains melamine
The amine-for-aldehyde resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and melamine is 1:0.1, the weight ratio of water and formaldehyde is
2:1。
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:0.1:0.01.
It is 1 by weight by the melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with
2000 revs/min of mixing speed is well mixed, and obtains first material；Then at ambient temperature, it is 4.5 by pH value, buffering
To total concentration be 2 weight % potassium dihydrogen phosphate-dipotassium hydrogen phosphate cushioning liquid, be evenly added in 1 hour above-mentioned
In first material, it is well mixed with 1100 revs/min of mixing speed, obtains the second material that pH value is adjusted to 7；In room temperature
Under the conditions of, the hydrochloric acid that concentration is 5 weight % was evenly added in above-mentioned second material in 1.5 hours, with 1300 revs/min
The mixing speed of clock is well mixed, and obtains the 3 material that pH value is adjusted to 4；Under conditions of 60 DEG C, by the 3rd thing
Material is stirred 2 hours with 800 revs/min of speed, is obtained 4 materials and is adjusted the pH value of the 4 materials to 7；To
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are added in 4 materials to be well mixed, and obtain gamma cyhalothrin microcapsule suspension
Agent, wherein, the weight ratio of 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.02：0.001：0.02.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % pull open powder, 0.2 weight
Measure % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate and 60
Weight % water is sufficiently mixed, disperseed, and being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5 microns
Suspension, obtain Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds polyoxyethylene nonyl phenyl second
Alkene ether and water, stir, and obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient chlorine fluorine
The weight ratio of Cyano chrysanthemate microcapsule suspending agent and Teflubenzuron suspending agent, NPE is 1:0.2:0.5.
Embodiment 6
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 2.5h under the conditions of being 72 DEG C, obtains melamine
The amine-for-aldehyde resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and melamine is 1:0.2, the weight ratio of water and formaldehyde is
2.5:1。
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained, its
In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
It is 4 by weight by the melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with
2000 revs/min of mixing speed is well mixed, and obtains first material；Then at ambient temperature, it is 4.5 by pH value, buffering
To total concentration be 2 weight % acetic acid-sodium acetate buffer solution, above-mentioned first material was evenly added in 0.5 hour
In, it is well 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 % was evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min
Mixing speed is well mixed, and obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, by the 3 material
Stirred 2 hours with 300 revs/min of speed, obtain 4 materials and adjust the pH value of the 4 materials to 7；To the 4th
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are added in material to be well mixed, and obtain lambda-cyhalothrin microcapsule suspension,
Wherein, the weight ratio of 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.15：0.002：0.04.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds 1- methyl naphthalene sulfonic acids
Sodium formaldehyde condensation product and water, stir, and obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein,
The weight ratio of lambda-cyhalothrin microcapsule suspension and Teflubenzuron suspending agent, 1- methyl naphthalene sulfonate formaldehyde condensates is 1:
0.1:0.01。
Embodiment 7
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
The resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and urea is 1:2, the weight ratio of water and formaldehyde is 2.8:1.
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2.5:0.05.
It is 4 by weight by the urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with 2000 turns/
The mixing speed of minute is well mixed, and obtains first material；Then at ambient temperature, by pH value be 4.5, buffering pair it is total dense
Spend for 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in above-mentioned first material in 1.5 hours, with 1000
Rev/min mixing speed be well mixed, obtain the second material that pH value is adjusted to 6.2；At ambient temperature, it is by concentration
5 weight % hydrochloric acid 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, by the 3 material with 200 revs/min
The speed of clock stirs 2 hours, obtains 4 materials and adjusts the pH value of the 4 materials to 7；Added into 4 materials
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are well mixed, and obtain lambda-cyhalothrin microcapsule suspension, wherein, the 4th
The weight ratio of material and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.01：0.005：0.05.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds sodium lignin sulfonate
And water, stir, obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient cyhalothrin
The weight ratio of ester micro capsule suspending agent and Teflubenzuron suspending agent, sodium lignin sulfonate is 1:0.3:0.05.
Embodiment 8
Urea, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 65 DEG C, obtains urea-formaldehyde
The resin prepolymer aqueous solution, wherein, the mol ratio of formaldehyde and urea is 1:1, the weight ratio of water and formaldehyde is 2.8:1.
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2:0.06.
It is 3 by weight by the urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1 with 2000 turns/
The mixing speed of minute is well mixed, and obtains first material；Then at ambient temperature, by pH value be 3.6, buffering pair it is total dense
Spend for 4 weight % citric acid-sodium citrate buffer, be evenly added in above-mentioned first material in 1 hour, with
1000 revs/min of mixing speed is well mixed, and obtains the second material that pH value is adjusted to 6.2；At ambient temperature, will be dense
The phosphoric acid spent for 4 weight % was evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min of stirring speed
Degree is well mixed, obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, by the 3 material with 1000
Rev/min speed stir 2 hours, obtain 4 materials and adjust the pH value of the 4 materials to 7；Into 4 materials
Add sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol to be well mixed, obtain lambda-cyhalothrin microcapsule suspension, wherein,
The weight ratio of 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.02：0.004：0.04.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds sodium lignin sulfonate
And water, stir, obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient cyhalothrin
The weight ratio of ester micro capsule suspending agent and Teflubenzuron suspending agent, sodium lignin sulfonate is 1:0.2:0.03.
Embodiment 9
Benzoguanamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains benzene
Substituted melamine-formaldehyde resin performed polymer the aqueous solution, wherein, the mol ratio of formaldehyde and benzoguanamine is 1:0.5, Shui Hejia
The weight ratio of aldehyde is 2.8:1.
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2:0.06.
It is 4 by weight by benzoguanamine-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate：1
It is well mixed with 2000 revs/min of mixing speed, obtains first material；Then at ambient temperature, it is 4 by pH value, buffering
To total concentration be 4 weight % citric acid-sodium citrate buffer, above-mentioned first thing was evenly added in 1 hour
In material, it is well 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 % was evenly added in above-mentioned second material in 1.5 hours, with 1200 revs/min
Mixing speed is well mixed, and obtains the 3 material that pH value is adjusted to 3.2；Under conditions of 60 DEG C, by the 3 material
Stirred 2 hours with 700 revs/min of speed, obtain 4 materials and adjust the pH value of the 4 materials to 7；To the 4th
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol are added in material to be well mixed, and obtain lambda-cyhalothrin microcapsule suspension,
Wherein, the weight ratio of 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol is 1：0.03：0.005：0.05.
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with Teflubenzuron suspending agent, adds detergent alkylate sulphur
Sour sodium and water, stir, and obtain the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.Wherein, efficient chlorine fluorine
The weight ratio of Cyano chrysanthemate microcapsule suspending agent and Teflubenzuron suspending agent, neopelex is 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 and use concentration that the pH value of material is adjusted into 3.2 for 5 weight % hydrochloric acid.
Comparative example 2
Difference with embodiment 1 is, after obtaining first material, uses pH value for 4.5, the total concentration of buffering pair is 2 weights
After material pH value is adjusted to 4.5 by amount % acetic acid-sodium acetate buffer solution, the step of without second regulation pH value.
Comparative example 3
Difference with embodiment 1 is, uses concentration that the pH value of 3 material is adjusted into 2 for 5 weight % hydrochloric acid.
Comparative example 4
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Efficient cyhalothrin emulsifiable concentrate is obtained, wherein, the gamma cyhalothrin, 200# solvent naphthas and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2.5:0.05.Method same as Example 1 prepares Teflubenzuron suspending agent, by efficient chlorine fluorine
Cyano chrysanthemate missible oil is 1 by weight with Teflubenzuron suspending agent:0.3 mixing, obtains gamma cyhalothrin Teflubenzuron suspension emulsion.
Comparative example 5
Gamma cyhalothrin, 200# solvent naphthas and sorbitan monostearate APEO are well mixed,
Gamma cyhalothrin oil phase is obtained, water is slowly dropped into gamma cyhalothrin oil phase, is stirred when being added dropwise, and add second
Glycol and xanthans, obtain gamma cyhalothrin aqueous emulsion.Wherein, the gamma cyhalothrin, 200# solvent naphthas, dehydration
Sorbitol monostearate APEO, water, the weight ratio of ethylene glycol and xanthans are 1:2.5:0.05:1.2:0.005:
0.001。
Comparative example 6
By 26.3 weight % Teflubenzuron, 2 weight % lauryl sodium sulfate, 6 weight % sodium lignin sulfonate,
0.2 weight % organic silicon defoamer, 5 weight % ethylene glycol, 0.3 weight % xanthans, 0.2 weight % sodium benzoate
It is sufficiently mixed, disperses with 60 weight % water, being passed through sand mill after being uniformly dispersed is sanded, and is sanded to average grain diameter and is less than 5
The suspension of micron, obtains Teflubenzuron suspending agent.
Testing example 1
What this testing example was used in testing example 1-9 and comparative example 1-3 obtain contains gamma cyhalothrin and volt
The heat storage of the micro- suspension emulsion of gamma cyhalothrin Teflubenzuron obtained in the grand microcapsule suspension-suspendinagent agent of worm and comparative example 4 is steady
Qualitative and low-temperature stability.
Heat storage stability is tested：Contain gamma cyhalothrin and Teflubenzuron by what is obtained in embodiment 1-9 and comparative example 1-3
Microcapsule suspension-suspendinagent agent and comparative example 4 in the obtained micro- suspension emulsion of gamma cyhalothrin Teflubenzuron be fitted into container, it is close
It is honored as a queen and is positioned in the constant temperature oven of (54 ± 2) DEG C, is taken out after standing 14 days, it is outstanding according to GB/T14825-2006 standards, measure
Floating rate, the results are shown in Table 1.
Low-temperature stability determines：Contain gamma cyhalothrin and Teflubenzuron by what is obtained in embodiment 1-9 and comparative example 1-3
Microcapsule suspension-suspendinagent agent and comparative example 4 in the obtained micro- suspension emulsion of gamma cyhalothrin Teflubenzuron be fitted into container, it is close
Be honored as a queen and be placed in (0 ± 2) DEG C refrigerator, keep 1h, at interval of 15min stirring once, each 15s, observation outward appearance have it is unchanged,
Continue to place 7 days in (0 ± 2) DEG C, then take out and be placed under room temperature condition after standing recovery, marked according to GB/T14825-2006
Standard, suspensibility is determined, the results are shown in Table 1.
Table 1
As it can be seen from table 1 preparation method provided by the invention obtain it is micro- containing gamma cyhalothrin and Teflubenzuron
Capsule suspension-suspending agent has good thermal storage stability and low tempertaure storage stability.
Testing example 2
This testing example is micro- containing gamma cyhalothrin and Teflubenzuron to obtaining in embodiment 1-9, comparative example 1-3
Gamma cyhalothrin Teflubenzuron suspension emulsion, the efficient chlorine fluorine cyanogen of comparative example 5 obtained in capsule suspension-suspending agent, comparative example 4
Chrysanthemum ester aqueous emulsion and the Teflubenzuron suspending agent of comparative example 6 are tested the prevention effect of leek root maggot on leek.Add before test
Enter a certain amount of distilled water, stir, adjust contain efficient cyhalothrin by what is obtained in embodiment 1-9, comparative example 1-3 respectively
The gamma cyhalothrin Teflubenzuron suspension emulsion that is obtained in the microcapsule suspension-suspendinagent agent of ester and Teflubenzuron, comparative example 4, contrast
Activity component concentration in the gamma cyhalothrin aqueous emulsion of example 5 and the Teflubenzuron suspending agent of comparative example 6 is 10 weight %.
Test site：Dezhou City Shandong Province Ningjin County Dong Cuicun, experimental plot are leek planting base for many years, experimental plot physical features
It is flat, middle fertility, earth in quality.Each treatment region leek routinely production management after dispenser.
Specific steps include, and are 30kg/ mus according to formulation rate, by embodiment 1-9, comparative example using knapsack sprayer
The microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron obtained in 1-3, the efficient chlorine fluorine obtained in comparative example 4
The Teflubenzuron suspending agent decoction of Cyano chrysanthemate Teflubenzuron suspension emulsion, the gamma cyhalothrin aqueous emulsion of comparative example 5 and comparative example 6
Pouring root is carried out to the leek plant of each growing area respectively, blank control group is using equivalent clear water to the leek plant in growing area
Carry out pouring root.
After dispenser 10 days, 20 days, 30 days and 50 days investigation leek root maggot prevention effect, specific test method according to《Agriculture
Medicine field control effectiveness test criterion》Carry out.Each treatment region is investigated 25 clumps of leek, adjusted using random 5 points samplings, each cell that handles
Each treatment region leek root maggot prevention effect is looked into, the death rate is calculated by formula (1) and calculates corrected mortality by formula (2), as a result such as table 2
It is shown.
Concrete outcome is shown in Table 2.
Table 2
Testing example 3
This testing example is micro- containing gamma cyhalothrin and Teflubenzuron to obtaining in embodiment 1-9, comparative example 1-3
The micro- suspension emulsion of gamma cyhalothrin Teflubenzuron, the efficient chlorine fluorine of comparative example 5 obtained in capsule suspension-suspending agent, comparative example 4
Served to Chinese cabbage blue or green worm, the prevention effect of aphid of Cyano chrysanthemate aqueous emulsion and the Teflubenzuron suspending agent of comparative example 6 is tested.Test
It is preceding to add a certain amount of distilled water, stir, what is obtained in regulation embodiment 1-9, comparative example 1-3 contains gamma cyhalothrin
The micro- suspension emulsion of gamma cyhalothrin Teflubenzuron that is obtained in microcapsule suspension-suspendinagent agent, comparative example 4 with Teflubenzuron, contrast
Activity component concentration in the gamma cyhalothrin aqueous emulsion of example 5 and the Teflubenzuron suspending agent of comparative example 6 is 10 weight %.
Test site：Hebei province Baoding Xinshi District Xi great Yuan villages.The plot physical features is flat, and fertility is preferable.After dispenser
Each treatment region Chinese cabbage routinely production management.
Specific steps include, and are 30kg/ mus according to spouting liquid, by embodiment 1-9, comparative example using knapsack sprayer
The microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron obtained in 1-3, the efficient chlorine fluorine obtained in comparative example 4
The Teflubenzuron suspending agent decoction of Cyano chrysanthemate Teflubenzuron suspension emulsion, the gamma cyhalothrin aqueous emulsion of comparative example 5 and comparative example 6
Uniformly spray respectively on the Chinese cabbage plant of each growing area, blank control group is planted using equivalent clear water to the Chinese cabbage in growing area
Strain is sprayed, and during dispenser, is blocked neighbor cell with plastic sheeting, is prevented medicament from interfering.
After dispenser 10 days, 20 days, 30 days and 50 days investigation cabbage caterpillar, control of aphids effect, specific test method according to
《Pesticide field efficacy medicine test criterion》Carry out.Each treatment region uses random 5 points samplings, and each cell that handles investigates 25 plants in vain
Dish, each treatment region cabbage caterpillar, control of aphids effect are investigated, calculate the death rate by formula (1) and calculate corrected mortality by formula (2),
Concrete outcome is shown in Table 3：
Table 3
From table 2 and table 3 as can be seen that preparation method provided by the invention by two step section pH value, is specifically stirring
The microcapsule suspension containing gamma cyhalothrin and Teflubenzuron being prepared under the reaction conditions such as rotating speed, emulsifying dispersant, solvent-
Suspending agent, prevent and treat while slow release long-acting can be obtained the effect of crop pests.And this method prepare contain gamma cyhalothrin
Microcapsule suspension-suspendinagent agent effect with Teflubenzuron is much better than gamma cyhalothrin aqueous emulsion single dose, Teflubenzuron suspending agent
Single dose.The microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron of the present invention is relative to gamma cyhalothrin
Other formulations of Teflubenzuron, have the lasting period it is long the characteristics of, it is cost-effective so as to reduce times for spraying and dosage, wherein
The organic solvent contained is few, can reduce the pollution to environment.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of preparation method of the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron, wherein, the preparation method
Comprise the following steps：
S1, it is by weight (1-5)：The 1 mixed amino resin prepolymer aqueous solution and efficient cyhalothrin emulsifiable concentrate, obtain first
Material；
Cushioning liquid is added in S2, the first material obtained to step S1 and is mixed, obtains the second thing that pH value is 5-7
Material；
Acid solution is added in S3, the second material obtained to step S2 and is mixed, obtains the 3rd thing that pH value is 3-4
Material；
S4, the 3 material for obtaining step S3 under conditions of being 40-70 DEG C in temperature stir 2-7 hours, obtain the 4th
Material；
S5, it is 1 by weight：(0.1-1)：4 materials that (0.01-2) obtains step S4 and Teflubenzuron suspending agent and
Emulsifying dispersant mixes, and obtains the microcapsule suspension-suspendinagent agent containing gamma cyhalothrin and Teflubenzuron.
2. preparation method according to claim 1, wherein, the amino resins performed polymer aqueous solution described in step S1 passes through
What compound, formaldehyde and water prepolymerization containing amino obtained, the compound containing amino includes urea, melamine and benzene generation
At least one of melamine, the mol ratio of the compound and formaldehyde containing amino is (0.1-2)：1, the weight of water and formaldehyde
It is (2-7) to measure ratio：1, the prepolymerized condition includes：PH value is 8-10, and temperature is 60-80 DEG C, and the time is 0.5-3 hours.
3. preparation method according to claim 1, wherein, the efficient cyhalothrin emulsifiable concentrate described in step S1 contains height
Imitate lambda-cyhalothrin, organic solvent and emulsifying agent, the weight of the gamma cyhalothrin, the organic solvent and the emulsifying agent
Amount is than being 1：(0.1-5)：(0.01-0.2), the organic solvent include petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and
At least one of solvent naphtha, the emulsifying agent include sodium lignin sulfonate, lauryl sodium sulfate, DBSA
Sodium, styrene-maleic anhydride copolymer, AEO, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, dehydration mountain
At least one in pears alcohol monostearate ester APEO, sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate
Kind.
4. preparation method according to claim 1, wherein, the buffering in cushioning liquid described in step S2 is to including lemon
At least one of lemon acid-sodium citrate, potassium dihydrogen phosphate-dipotassium hydrogen phosphate and acetic acid-sodium acetate.
5. preparation method according to claim 1, wherein, the acid solution described in step S3 includes hydrochloric acid, sulfuric acid, phosphorus
At least one of acid, acetic acid and ammonium chloride solution.
6. preparation method according to claim 1, wherein, it is fast by the stirring at 1500-3000 revs/min in step S1
Mixing is realized in the lower stirring of degree；In step S2 mixing is realized by being stirred under 1000-1200 revs/min of mixing speed；Step
In S3 mixing is realized by being stirred under 1200-1500 revs/min of mixing speed；The speed stirred described in step S4 is
200-1000 revs/min.
7. preparation method according to claim 1, wherein, the preparation method be additionally included in step S5 before by described
The step of 4 materials mix with dispersant, thickener and antifreezing agent；The 4 materials and the dispersant, the thickener and
The weight ratio of the antifreezing agent mixing is 1：(0.01-0.2)：(0.001-0.02)：(0.02-0.15)；The dispersant includes
Neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensates, the condensation of benzyl naphthalenesulfonateformaldehyde formaldehyde
Thing, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder,
At least one of NPE and AEO；The thickener include Magnesiumaluminumsilicate, xanthans,
At least one of polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon；The antifreezing agent includes second two
At least one of alcohol, 1,2- propane diols, glycerine and urea.
8. preparation method according to claim 1, wherein, Teflubenzuron particulate in the Teflubenzuron suspending agent described in step S5
Average grain diameter be 1-5 microns.
9. preparation method according to claim 1, wherein, the emulsifying dispersant described in step S5 includes detergent alkylate
Sodium sulfonate, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensates, benzyl naphthalene sulfonic acid-formaldehyde condensation product, lignin
Sodium sulfonate, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, polyoxyethylene nonyl phenyl
At least one of vinethene and AEO.
What 10. the preparation method according to any one in claim 1-9 was prepared contains gamma cyhalothrin and volt
The grand microcapsule suspension-suspendinagent agent of worm.
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| CN110050788A (en) * | 2018-05-08 | 2019-07-26 | 华东理工大学 | Gamma cyhalothrin poly-dopamine micro-capsule suspension and preparation method thereof |
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| CN110074128A (en) * | 2019-04-27 | 2019-08-02 | 上海明德立达生物科技有限公司 | A kind of microcapsule suspension-suspendinagent agent and preparation method thereof containing gamma cyhalothrin and fluorine pyrrole furanone |
| WO2022034559A1 (en) * | 2020-08-14 | 2022-02-17 | Upl Limited | A storage stable insecticidal composition |
| CN114600877A (en) * | 2022-03-29 | 2022-06-10 | 山东潍坊润丰化工股份有限公司 | Microcapsule suspension-suspending agent containing efficient cyhalothrin and chlorantraniliprole and preparation method thereof |
| CN114600877B (en) * | 2022-03-29 | 2023-12-29 | 山东潍坊润丰化工股份有限公司 | Microcapsule suspension-suspending agent containing efficient cyhalothrin and chlorantraniliprole and preparation method thereof |
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Application publication date: 20171222 |