CN109526976A - A kind of method and its microcapsule suspension-suspendinagent agent preparing the microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin - Google Patents
A kind of method and its microcapsule suspension-suspendinagent agent preparing the microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin Download PDFInfo
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- CN109526976A CN109526976A CN201811378087.0A CN201811378087A CN109526976A CN 109526976 A CN109526976 A CN 109526976A CN 201811378087 A CN201811378087 A CN 201811378087A CN 109526976 A CN109526976 A CN 109526976A
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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
- A01N47/40—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 a double or triple bond to nitrogen, e.g. cyanates, cyanamides
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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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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Abstract
This disclosure relates to a kind of method and its microcapsule suspension-suspendinagent agent for preparing the microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin, this method comprises: a, by amino-formaldehyde resins performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate being by weight (1-5): 1 mixing obtains first material；B, buffer solution is added into first material to be uniformly mixed, makes mixed solution pH value 4-7, obtains second material；C, acidic ph modifier is added into second material to be uniformly mixed, makes mixed solution pH value 3-4, obtains third material；D, third material is subjected to solidification bunching, obtains solidification bunching product, adjusting the solidification bunching product pH value is 6-8, obtains 4 materials；E, by the 4 materials with thiacloprid suspending agent by weight 1:(0.1-1) be uniformly mixed.The microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin prepared using disclosed method, the anti-crop pests lasting period processed is long, and stores stabilization.
Description
Technical field
The present invention relates to technical field of pesticide, and in particular, to a kind of to prepare containing thiacloprid and gamma cyhalothrin
Microcapsule suspension-suspendinagent agent method and its microcapsule suspension-suspendinagent agent.
Background technique
Gamma cyhalothrin is a kind of insecticide, has the function of walking quickly and keeping away, knock down and killing to insect.Traditional is efficient
Lambda-cyhalothrin dosage form easily fails under the action of external environment due to existing, and such as sunshine, soil acidity or alkalinity etc., the lasting period is short,
Thus reduce the preventive effect of pesticide.In addition, other preparations of gamma cyhalothrin are polluted containing a large amount of organic solvents in the market
Environment.The lambda-cyhalothrin microcapsule suspension that traditional preparation methods obtain is easy to happen reunion, solidification phenomenon, causes not
Easily storage, prevention and treatment crop pests effect are poor, it is difficult to meet the preparation demand of prevention and treatment crop pests pesticide.And efficient chlorine fluorine
Cyano chrysanthemate single dose also has certain limitation, and practical control efficiency can not only be effectively improved by compounding with thiacloprid, reduces medication
Amount, reduces cost, delays the generation of drug resistance.
But the combination medicament of existing gamma cyhalothrin and thiacloprid has a variety of defects, such as wettable powder
Product bonding is easily caused, should not disperse to suspend in water, precipitating keeps medicament sprinkling uneven in sprayer, and existing medicine
The storage stability of agent is lower, and synergy is not obvious enough.
Summary of the invention
The object of the present invention is to provide a kind of gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent preparation method
And the gamma cyhalothrin and thiacloprid microcapsule suspension-suspending agent prepared by this method.
To achieve the goals above, disclosure first aspect provides a kind of micro-capsule containing thiacloprid and gamma cyhalothrin
Suspension-suspending agent preparation method, this method comprises the following steps: a, being uniformly mixed the first solution and the second solution, obtains
First material；First solution contains amino-formaldehyde resins performed polymer aqueous solution；Second solution contains efficient chlorine fluorine cyanogen
Pyrethroids missible oil；The weight ratio of first solution and second solution is (1-5): 1；B, it is added in Xiang Suoshu first material slow
It rushes solution to be uniformly mixed, makes mixed solution pH value 4-7, obtain second material；C, acid pH is added in Xiang Suoshu second material
Regulator is uniformly mixed, and is made mixed solution pH value 3-4, is obtained third material；D, the third material is subjected to solidification bunching,
Solidification bunching product is obtained, adjusting the solidification bunching product pH value is 6-8, obtains 4 materials；E, by the 4 materials
It is uniformly mixed with thiacloprid suspending agent, obtains the microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin；Described
The weight ratio of 4 materials and the thiacloprid suspending agent is 1:(0.1-1).
Preferably, the amino-formaldehyde resins performed polymer aqueous solution in step a is by amino-containing compound, the first
The material liquid prepolymerization of aldehyde and water obtains；The amino-containing compound includes in urea, melamine and benzoguanamine
At least one；The weight ratio of the formaldehyde, amino-containing compound and water is 1:(0.2-12): (2-6)；It is described prepolymerized
Condition includes: that pH value is 8-10, and temperature is 60-80 DEG C, and the reaction time is 0.5-3 hours.
Preferably, the efficient cyhalothrin emulsifiable concentrate in step a contains gamma cyhalothrin, organic solvent and cream
Agent；The organic solvent includes at least one of petroleum ether, ethyl acetate, methyl oleate, dimethylbenzene and solvent naphtha；It is described
Emulsifier include sodium lignin sulfonate, lauryl sodium sulfate, neopelex, styrene-maleic anhydride copolymer,
Fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate polyoxyethylene ether,
At least one of sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate；It is the gamma cyhalothrin, described
The weight ratio of organic solvent and the emulsifier is 1:(0.1-5): (0.01-0.2).
Preferably, the pH value of the buffer solution in step b is 3-5.5；The buffer solution contains buffering pair, described
Buffering is to including at least one of citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate；The buffering
The total concentration of buffering pair is 1-5 weight % in solution.
Preferably, the acidic ph modifier in step c contains in hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid and ammonium chloride extremely
Few one kind；The concentration of the acidic ph modifier is 1-10 weight %.
Preferably, this method includes, in step e, by the 4 materials and the first dispersing agent, the first thickener and first
After the mixing of at least one of antifreezing agent, then mix with the thiacloprid suspending agent；First dispersing agent includes dodecyl
It is benzene sulfonic acid sodium salt, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, wooden
Plain sodium sulfonate, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pull open powder, nonyl phenol are poly-
At least one of ethylene oxide ether and fatty alcohol polyoxyethylene ether；First thickener includes aluminum magnesium silicate, xanthan gum, poly- second
At least one of glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black；First antifreezing agent includes second two
At least one of alcohol, 1,2- propylene glycol, glycerine and urea；The 4 materials, first dispersing agent, described first increase
The weight ratio of thick dose and first antifreezing agent is 1:(0.01-0.2): (0.001-0.02): (0.02-0.15).
Preferably, this method includes, in step e, after the 4 materials and the third dispersant, then with institute
State the mixing of thiacloprid suspending agent；The weight ratio of the 4 materials, the thiacloprid suspending agent and the third dispersing agent is 1:
(0.1-1): (0.01-2).
Preferably, the thiacloprid suspending agent in step e contains thiacloprid particle, water and auxiliary of the partial size less than 5 μm
Agent；The weight ratio of the thiacloprid particle, the adjuvant and the water is 1:(1-2): (2-5)；Preferably, the auxiliary
Agent includes the second dispersing agent, defoaming agent, the second thickener, the second antifreezing agent and at least one of the preservatives；The thiacloprid
Particle, second dispersing agent, the defoaming agent, second thickener, second antifreezing agent and the preservative weight
Amount is than being 1:(0.15-0.3): (0.003-0.01): (0.003-0.01): (0.15-0.3): (0.003-0.01).
Preferably, it is 1500-3000 revs/min that the mixed condition in step a, which includes: mixing speed,；Step b
In the mixed condition include: mixing speed be 1000-1200 revs/min；The mixed condition packet in step c
Include: mixing speed is 1200-1500 revs/min；The condition of the solidification bunching in step d includes: under the conditions of 40-70 DEG C
Processing 2-6 hours.
Disclosure second aspect: provide the method preparation of disclosure first aspect contains thiacloprid and efficient cyhalothrin
The microcapsule suspension-suspendinagent agent of ester.
Through the above technical solutions, the present invention adjusts certain ph by multistep, the offer being prepared contains efficient chlorine
The microcapsule suspension-suspendinagent agent of flucythrinate and thiacloprid is capable of the prevention and treatment crop pests of slow release long-acting, and has good speed
Effect property, storage stability, be not susceptible to reunite, solidification phenomenon can reduce dosage and times for spraying, so that save the cost is simultaneously
Reduce the pollution to environment.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
First aspect present invention: a kind of prepare containing the microcapsule suspension-containing thiacloprid and gamma cyhalothrin is provided
The method of suspending agent, this method comprises the following steps: a, being uniformly mixed the first solution and the second solution, obtains first material；
Wherein, first solution contains amino-formaldehyde resins performed polymer aqueous solution；Second solution contains gamma cyhalothrin
Missible oil；The weight ratio of first solution and second solution is (1-5): 1；B, it is molten that buffering is added in Xiang Suoshu first material
Liquid is uniformly mixed, and is made mixed solution pH value 4-7, is obtained second material；C, acid pH is added in Xiang Suoshu second material to adjust
Agent is uniformly mixed, and is made mixed solution pH value 3-4, is obtained third material；D, the third material is subjected to solidification bunching, obtained
Solidify bunching product, adjusting the solidification bunching product pH value is 6-8, obtains 4 materials；E, by the 4 materials and thiophene
Worm quinoline suspending agent is uniformly mixed, and obtains the microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin；4th object
The weight ratio of material and the thiacloprid suspending agent is 1:(0.1-1).
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 acid-cyano-(3- Phenoxyphenyl) methyl ester trade name, English name
For λ-Cyhalothrin, molecular formula C23H19ClF3NO3, relative molecular weight 449.9, No. CAS is 91465-08-6, structure
Shown in formula such as formula (1) and formula (2).
In the disclosure, thiacloprid is compound (3- ((6- chloro-3-pyridyl base) methyl) -1,3-thiazoles quinoline -2- subunit) cyanogen
Amine.Molecular formula C10H9ClN4S, relative molecular weight 252.7, No. CAS: 111988-49-9, structural formula such as formula (3):
According to the present invention, the microcapsule suspension-containing gamma cyhalothrin and thiacloprid obtained by above-mentioned preparation method
Suspending agent is not susceptible to reunion and coacervation, is capable of the prevention and treatment crop pests of slow release long-acting, and have good quick-acting
Property, dosage and times for spraying can be reduced, thus the pollution of save the cost and reduction to environment.
In disclosed method, in step a, the amino-formaldehyde resins performed polymer aqueous solution can be by containing amino
The material liquid prepolymerization of compound, formaldehyde and water obtains；The amino-containing compound may include urea, melamine and benzene
At least one of substituted melamine；Under preferable case, the weight ratio of the formaldehyde, amino-containing compound and water can be 1:
(0.2-12): (2-6)；Under preferable case, the prepolymerized condition may include: that pH value is 8-10, and temperature is 60-80 DEG C,
Reaction time is 0.5-3 hours.
In disclosed method, in step a, the preparation method of the efficient cyhalothrin emulsifiable concentrate can be this field
Preparation method well known to technical staff, the present invention are not particularly limited this.Under preferable case, in order to further improve efficiently
The stability of cyhalothrin emulsifiable concentrate, the efficient cyhalothrin emulsifiable concentrate can contain gamma cyhalothrin, organic solvent
And emulsifier；The weight ratio of gamma cyhalothrin, the organic solvent and the emulsifier can be 1:(0.1-5):
(0.01-0.2).The organic solvent may include petroleum ether, ethyl acetate, toluene, N,N-dimethylformamide, three chloromethanes
At least one of alkane, isopropanol, dimethylbenzene and solvent naphtha；The emulsifier may include sodium lignin sulfonate, dodecyl
Sodium sulphate, neopelex, styrene-maleic anhydride copolymer, fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxy
Ethylene polyethenoxy ether, sorbitan monostearate polyoxyethylene ether, sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate
At least one of with naphthalene sulfonate.
In disclosed method, in order to improve clad ratio, the uniformity and the softgel shell compactness of micro-capsule, in step b, institute
The pH value for stating buffer solution can be 3-5.5；The buffer solution contains buffering pair, and under preferable case, the buffering is to can be with
Including at least one of citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-sodium acetate；In the buffer solution
The total concentration of buffering pair can be 1-5 weight %.
In disclosed method, under preferable case, in step c, the acidic ph modifier can contain hydrochloric acid, sulphur
At least one of acid, phosphoric acid, acetic acid and ammonium chloride；The concentration of the acidic ph modifier can be 1-10 weight %.
In order to further improve thiacloprid and lambda-cyhalothrin microcapsule suspension-suspending agent particle diameter distribution and storage
Stability is deposited, so that it is not susceptible to reunion and solidification phenomenon, and there is good crop pests control efficiency, in the disclosure
In a kind of preferred embodiment, in step e, the 4 materials and the first dispersing agent, the first thickener and first can be prevented
After freezing at least one of agent mixing, then mix with the thiacloprid suspending agent；Under preferable case, by the 4 materials and
After one dispersing agent, the first thickener and the mixing of the first antifreezing agent, then mix with the thiacloprid suspending agent.First dispersing agent
Including neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalenesulfonateformaldehyde formaldehyde
Condensation product, desugar sodium lignin sulfonate, desugar condensation sodium lignin sulfonate, Succinate sodium sulfonate, pulls open sodium lignin sulfonate
At least one of powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether；First thickener may include silicic acid
At least one of magnalium, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black；Described
One antifreezing agent may include at least one of ethylene glycol, 1,2- propylene glycol, glycerine and urea.It is the 4 materials, described
The weight ratio of first dispersing agent, first thickener and first antifreezing agent can be 1:(0.01-0.2): (0.001-
0.02): (0.02-0.15).
Further, in order to avoid occur microcapsule suspension-suspendinagent agent aggregation, precipitating, it is hardened phenomena such as, can be in step e
It is mixed after the 4 materials and the third dispersant, then with the thiacloprid suspending agent；The 4 materials, institute
The weight ratio for stating thiacloprid suspending agent and the third dispersing agent can be 1:(0.1-1): (0.01-2).Wherein, the third
Dispersing agent can be identical or different with first dispersing agent, and the preferably described third dispersing agent can be dodecyl benzene sulfonic acid
Salt, di-2-ethylhexylphosphine oxide naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulfonic acid-formaldehyde condensation product, lignin sulfonic acid
Salt, desugar lignosulfonates, desugar are condensed lignosulfonates, succinate sulfonate, pull open powder, phosphoric acid ester, poly- carboxylic
At least one of Barbiturates and fatty alcohol polyoxyethylene ether.
In disclosed method, in step e, the preparation method of the thiacloprid suspending agent can be those skilled in the art
Preparation method known to member, the present invention are not particularly limited it；For example, can be sufficiently mixed by thiacloprid and adjuvant and water
Splitting or integrating dissipates, and is present in thiacloprid in aqueous solution with aerosol form, and the average grain diameter so that thiacloprid particle is then sanded
To obtain thiacloprid suspending agent less than 5 μm.The weight ratio of the thiacloprid particle, the adjuvant and water can be 1:(1-
2): (2-5).The adjuvant may include in the second dispersing agent, defoaming agent, the second thickener, the second antifreezing agent and preservative
At least one.Wherein, second dispersing agent can be identical or different with first dispersing agent, second point preferably described
Powder can be dodecyl benzene sulfonate, di-2-ethylhexylphosphine oxide naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate, benzyl naphthalene sulphur
Sour formaldehyde condensation products, lignosulfonates, desugar lignosulfonates, desugar are condensed lignosulfonates, succinate sulfonic acid
At least one of salt, pull open powder, phosphoric acid ester, polycarboxylic acid salt and fatty alcohol polyoxyethylene ether；The defoaming agent can be
At least one of silicone oil, higher alcohol, mineral oil or vegetable oil；Second thickener can be identical as first thickener
Or it is different, preferably described second thickener can be aluminum magnesium silicate, xanthan gum, polyvinyl alcohol, sodium alginate, guar gum, carboxylic first
At least one of base sodium cellulosate, organobentonite, white carbon black；Second antifreezing agent can be with the first antifreezing agent phase
Same or different, preferably described second antifreezing agent can be ethylene glycol, 1,2-PD, glycerine, urea, polyethylene glycol, mountain
At least one of pears alcohol, sodium chloride；The preservative can be formaldehyde, Kathon CG, benzoic acid, sodium benzoate, sorbic acid, sorb
At least one of sour potassium.Further, the adjuvant may include the second dispersing agent, defoaming agent, the second thickener, second
Antifreezing agent and preservative；The thiacloprid particle, second dispersing agent, the defoaming agent, second thickener, described
The weight ratio of two antifreezing agents and the preservative can be 1:(0.15-0.3): (0.003-0.01): (0.003-0.01):
(0.15-0.3): (0.003-0.01).
In disclosed method, reaction condition appropriate can mention the clad ratio of micro-capsule, improve particle diameter distribution and capsule
The thickness of shell, and then improve the storage stability of microcapsule suspending agent；Under preferable case, in step a, the mixing condition includes:
Mixing speed is 1500-3000 revs/min；In step b, the mixing condition include: mixing speed be 1000-1200 turn/
Minute；In step c, the mixing condition includes: that mixing speed is 1200-1500 revs/min；In step d, the solidification
Bunching condition includes: to handle 2-6 hours under the conditions of 40-70 DEG C.
Second aspect of the present invention: provide the method preparation of disclosure first aspect contains thiacloprid and efficient cyhalothrin
The microcapsule suspension-suspendinagent agent of ester.
Present invention be described in more detail by the following examples, is not intended to restrict the invention.
In embodiment and comparative example, gamma cyhalothrin is purchased from Shandong Weifang Rainbow Chemical Co., Ltd., thiophene worm
Quinoline (content 95%) is purchased from Shijiazhuang Xingbai Biological Engineering Co., Ltd., and melamine is purchased from Beijing Chemical Plant, urea purchase
From Beijing Chemical Plant, benzoguanamine is purchased from Beijing Chemical Plant, and formaldehyde is purchased from Beijing Chemical Plant, anhydrous sorbitol monostearate
Ester APEO is purchased from Nanjing Teva-Chem. Co., Ltd., and lauryl sodium sulfate is purchased from the limited public affairs of wound hongda science and technology in Beijing
Department, sodium lignin sulfonate are purchased from Beijing Zhong Chuan hongda Science and Technology Ltd., and neopelex is purchased from Beijing and creates hongda
Science and Technology Ltd., polyvinyl alcohol are purchased from Zhengzhou Ao Cai industrial chemicals Co., Ltd, and fatty alcohol polyoxyethylene ether is blue purchased from Xingtai
Star auxiliary reagent factory, aluminum magnesium silicate are purchased from Hunan Peng Tai new high-tech material Co., Ltd, and bentonite is purchased from the organic swelling of Anji County, Zhejiang Province sky dragon
Native Co., Ltd, organic silicon defoamer are purchased from Shanghai Mitugao New Material Group, and ethylene glycol, glycerine and 1,2-PD are purchased from
Beijing Chemical Plant, xanthan gum are purchased from Shandong Zhong Xuan limited liability company, and sodium benzoate is purchased from the magnificent limited public affairs of intelligence Boke skill in Beijing
Department, 200# solvent naphtha are purchased from Hualun Chemical Co., Ltd., Jiangsu, and 150# solvent naphtha is purchased from Hualun Chemical Co., Ltd., Jiangsu, petroleum
Ether is purchased from Xilong Chemical Co., Ltd, and ethyl acetate is purchased from Xilong Chemical Co., Ltd.
Embodiment 1
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:2.2:2.5.
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2.5:0.05.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 4:1,
It is stirred evenly with 2000 revs/min of rate, obtains first material；It then at room temperature, is 4.5 by pH value, buffering pair
Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in the first material in 1 hour, with
1000 revs/min of mixing speed is uniformly mixed, and is adjusted mixed solution pH value as 6.2 and is obtained second material；At room temperature,
The hydrochloric acid that concentration is 5 weight % is evenly added in the second material in 1.5 hours, with 1200 revs/min stir
It mixes speed to be uniformly mixed, adjusts mixed solution pH value as 3.2 and obtain third material；Under conditions of 60 DEG C, by the third object
Material processing obtains solidification bunching product for 2 hours, and adding 5 weight % ammonium hydroxide to adjust pH value into the solidification bunching product is 7
Obtain 4 materials, i.e. lambda-cyhalothrin microcapsule suspension；Sodium lignin sulfonate, silicic acid are added into the 4 materials
Magnalium and ethylene glycol are uniformly mixed；Wherein, the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol
For 1:0.01:0.005:0.05.
By the thiacloprid (content 95%) of 26.3 weight %, the lauryl sodium sulfate 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 water of the sodium benzoate and 60 weight % of measuring % is sufficiently mixed, disperses, and is passed through sand mill after being uniformly dispersed and is sanded, and is sanded extremely
Suspension of the average grain diameter less than 5 microns, obtains thiacloprid suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
Than obtaining 22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent for 1:0.3:0.05.
Embodiment 2
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:4.0:3.3.
Gamma cyhalothrin, 150# solvent naphtha and sodium lignin sulfonate are uniformly mixed, gamma cyhalothrin is obtained
Missible oil, wherein the weight ratio of the gamma cyhalothrin, 150# solvent naphtha and sodium lignin sulfonate is 1:0.5:0.1.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 2:1,
It is stirred evenly with 1500 revs/min of rate, obtains first material；It then at room temperature, is 3 by pH value, buffering pair
Total concentration is acetic acid-sodium acetate buffer solution of 2 weight %, is evenly added in the first material in 1 hour, with
1100 revs/min of mixing speed is uniformly mixed, and is adjusted pH value as 6 and is obtained second material；It at room temperature, is 6 by concentration
The hydrochloric acid of weight % is evenly added in the second material in 1 hour, equal with 1300 revs/min of mixing speed mixing
It is even, pH value, which is adjusted, as 3 obtains third material；Under conditions of 50 DEG C, the third material is handled 4 hours, it is poly- to obtain solidification
Contracting product, it is 7 that 5 weight % ammonium hydroxide are added into the solidification bunching product and adjust pH value, obtains 4 materials, i.e., efficient chlorine fluorine
Cyano chrysanthemate microcapsule suspending agent；Neopelex, xanthan gum and glycerine are added into the 4 materials to be uniformly mixed,
Wherein, the weight ratio of the 4 materials and neopelex, xanthan gum and glycerine is 1:0.05:0.01:0.1.
Embodiment 1 is identical more than the preparation method of thiacloprid suspending agent.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight ratio of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
For 1:0.5:0.1,22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent are obtained.
Embodiment 3
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:6:5.
The preparation method of efficient cyhalothrin emulsifiable concentrate is same as Example 1, wherein the gamma cyhalothrin,
The weight ratio of 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether is 1:3:0.15.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 3:1,
It is stirred evenly with 2500 revs/min of rate, obtains first material；It then at room temperature, is 3.8 by pH value, buffering pair
Total concentration be 0.55 weight % acetic acid-sodium acetate buffer solution, the first material is evenly added in 1.5 hours
In, it is uniformly mixed with 1200 revs/min of mixing speed, adjusts pH value as 5.5 and obtain second material；At room temperature, will
Concentration is that the hydrochloric acid of 5 weight % is evenly added in the second material in 1 hour, with 1400 revs/min of stirring speed
Degree is uniformly mixed, and is adjusted pH value as 3.5 and is obtained third material；Under conditions of 43 DEG C, the third material is handled 6 hours
To solidification bunching product, and 5 weight % ammonium hydroxide are added, the pH value for solidifying bunching product are adjusted to 7, obtains 4 materials,
That is lambda-cyhalothrin microcapsule suspension；Sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol are added into the 4 materials
It is uniformly mixed, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.1:
0.015:0.15.
The preparation method of thiacloprid suspending agent is same as Example 1.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
Than obtaining 22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent for 1:0.8:1.
Embodiment 4
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:8.5:7.5.
Gamma cyhalothrin, petroleum ether and lauryl sodium sulfate are uniformly mixed, gamma cyhalothrin cream is obtained
Oil, wherein the weight ratio of the gamma cyhalothrin, petroleum ether and lauryl sodium sulfate is 1:5:0.2.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 5:1,
It is stirred evenly with 3000 revs/min of rate, obtains first material；It then at room temperature, is 4.5 by pH value, buffering pair
Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in the first material in 1 hour,
It is uniformly mixed with 1200 revs/min of mixing speed, adjusts pH value as 6.5 and obtain second material；At room temperature, by concentration
Hydrochloric acid for 5 weight % is evenly added in the second material in 1.5 hours, with 1500 revs/min of mixing speed
It is uniformly mixed, adjusts pH value as 3.7 and obtain third material；Under conditions of 60 DEG C, the third material is handled 2 hours and is obtained
Solidify bunching product, and the pH value for solidifying bunching product is adjusted to 6, obtains 4 materials, i.e. gamma cyhalothrin
Microcapsule suspending agent；Fatty alcohol polyoxyethylene ether, bentonite and 1,2-PD are added into the 4 materials to be uniformly mixed,
In, the weight ratio of the 4 materials and fatty alcohol polyoxyethylene ether, bentonite and 1,2-PD is 1:0.3:0.03:
0.25。
The preparation method of thiacloprid suspending agent is same as Example 1.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
Than obtaining 22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent for 1:1:2.
Embodiment 5
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:0.4:2.
It is same as Example 1 that efficient cyhalothrin emulsifiable concentrate obtains preparation method, wherein the gamma cyhalothrin,
The weight ratio of 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether is 1:0.1:0.01.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 1:1,
It is stirred evenly with 2000 revs/min of rate, obtains first material；It then at room temperature, is 4.5 by pH value, buffering pair
Total concentration be 2 weight % citrate-phosphate disodium hydrogen buffer solution, first object is evenly added in 1 hour
It in material, is uniformly mixed with 1100 revs/min of mixing speed, adjusts pH value as 7 and obtain second material；At room temperature, will
Concentration is that the hydrochloric acid of 5 weight % is evenly added in the second material in 1.5 hours, with 1300 revs/min of stirring
Speed is uniformly mixed, and is adjusted pH value as 4 and is obtained third material；Under conditions of 60 DEG C, the third material is handled 2 hours,
Obtain solidification bunching product, the 4 materials and be added into the solidification bunching product 5 weight % ammonium hydroxide adjusting pH value be
8, obtain 4 materials, i.e. lambda-cyhalothrin microcapsule suspension；Sodium lignin sulfonate, silicon are added into the 4 materials
Sour magnalium and ethylene glycol are uniformly mixed, wherein the weight of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol
Than for 1:0.02:0.001:0.02.
The preparation method of thiacloprid suspending agent is same as Example 1.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight ratio of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
For 1:0.2:0.5,22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent are obtained.
Embodiment 6
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:0.84:2.5.
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained,
In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 4:1,
It is stirred evenly with 2000 revs/min of rate, obtains first material；It then at room temperature, is 4.5 by pH value, buffering pair
Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in the first material in 0.5 hour,
It is uniformly mixed with 1000 revs/min of mixing speed, adjusts pH value as 6.2 and obtain second material；At room temperature, by concentration
Hydrochloric acid for 5 weight % is evenly added in the second material in 1.5 hours, with 1200 revs/min of mixing speed
It is uniformly mixed, adjusts pH value as 3.2 and obtain third material；Under conditions of 60 DEG C, the third material is handled 2 hours and is obtained
Solidify bunching product, and it is 7 that 5 weight % ammonium hydroxide, which are added, to adjust pH value into the solidification bunching product, obtains 4 materials, i.e.,
Lambda-cyhalothrin microcapsule suspension；It is mixed that sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol are added into the 4 materials
It closes uniform, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.15:
0.002:0.04.
It is same as Example 1 that thiacloprid suspending agent obtains preparation method.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight ratio of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
For 1:0.1:0.01,22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent are obtained.
Embodiment 7
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:0.84:2.5.
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained,
In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 4:1,
It is stirred evenly with 2000 revs/min of rate, obtains first material；It then at room temperature, is 4.5 by pH value, buffering pair
Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in the first material in 0.5 hour,
It is uniformly mixed with 1000 revs/min of mixing speed, adjusts pH value as 6.2 and obtain second material；At room temperature, by concentration
Hydrochloric acid for 5 weight % is evenly added in the second material in 1.5 hours, with 1200 revs/min of mixing speed
It is uniformly mixed, adjusts pH value as 3.2 and obtain third material；Under conditions of 60 DEG C, the third material is handled 2 hours and is obtained
Solidify bunching product, and it is 7 that 5 weight % ammonium hydroxide, which are added, to adjust pH value into the solidification bunching product, obtains 4 materials, i.e.,
Lambda-cyhalothrin microcapsule suspension；It is mixed that sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol are added into the 4 materials
It closes uniform, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.15:
0.002:0.04.
It is same as Example 1 that thiacloprid suspending agent obtains preparation method.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, water is added, is stirred evenly,
Wherein lambda-cyhalothrin microcapsule suspension and the weight ratio of thiacloprid suspending agent are 1:0.1, obtain the 22 efficient chlorine of weight %
Flucythrinate and thiacloprid microcapsule suspension-suspending agent.
Embodiment 8
Melamine, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains melamine
Amine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, melamine and water is 1:0.84:2.5.
Gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is uniform, efficient cyhalothrin emulsifiable concentrate is obtained,
In, the weight ratio of the gamma cyhalothrin, ethyl acetate and polyvinyl alcohol is 1:1.5:0.02.
Melamine formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 4:1,
It is stirred evenly with 2000 revs/min of rate, obtains first material；It then at room temperature, is 4.5 by pH value, buffering pair
Total concentration be 2 weight % acetic acid-sodium acetate buffer solution, be evenly added in the first material in 0.5 hour,
It is uniformly mixed with 1000 revs/min of mixing speed, adjusts pH value as 6.2 and obtain second material；At room temperature, by concentration
Hydrochloric acid for 5 weight % is evenly added in the second material in 1.5 hours, with 1200 revs/min of mixing speed
It is uniformly mixed, adjusts pH value as 3.2 and obtain third material；Under conditions of 60 DEG C, the third material is handled 2 hours and is obtained
Solidify bunching product, and it is 7 that 5 weight % ammonium hydroxide, which are added, to adjust pH value into the solidification bunching product, obtains 4 materials, i.e.,
Lambda-cyhalothrin microcapsule suspension；It is mixed that sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol are added into the 4 materials
It closes uniform, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.001:0.1:
0.2。
It is same as Example 1 that thiacloprid suspending agent obtains preparation method.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight ratio of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
For 1:0.1:0.01,22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent are obtained.
Embodiment 9
Urea, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains urea-formaldehyde
Resin prepolymer aqueous solution, wherein the weight ratio of formaldehyde, urea and water is 1:4:2.8.
The preparation method of efficient cyhalothrin emulsifiable concentrate is same as Example 1.
Urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 4:1, with 2000
Rev/min rate stir evenly, obtain first material；Then at room temperature, by pH value be 4.5, buffering pair it is total dense
Degree is acetic acid-sodium acetate buffer solution of 2 weight %, is evenly added in the first material in 1.5 hours, with
1000 revs/min of mixing speed is uniformly mixed, and is adjusted pH value as 6.2 and is obtained second material；At room temperature, it is by concentration
The hydrochloric acid of 5 weight % is evenly added in the second material in 1.5 hours, mixed with 1200 revs/min of mixing speed
It closes uniformly, adjusts pH value as 3.2 and obtain third material；Under conditions of 60 DEG C, the third material is handled 2 hours and is consolidated
Change bunching product, and it is 7 that 5 weight % ammonium hydroxide, which are added, to adjust pH value into the solidification bunching product, obtains 4 materials, i.e., it is high
Imitate lambda-cyhalothrin microcapsule suspending agent；Sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol mixing are added into the 4 materials
Uniformly, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.01:0.005:
0.05。
It is same as Example 1 that thiacloprid suspending agent obtains preparation method.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
Than obtaining 22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent for 1:0.3:0.05.
Embodiment 10
Urea, formaldehyde and water are mixed, are 8 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains urea-formaldehyde
Resin prepolymer aqueous solution, wherein the weight ratio of formaldehyde, urea and water is 1:2:2.8.
The preparation method of efficient cyhalothrin emulsifiable concentrate is same as Example 1, wherein the gamma cyhalothrin,
The weight ratio of 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether is 1:2:0.06.
Urea-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 3:1, with 2000
Rev/min rate stir evenly, obtain first material；Then at room temperature, by pH value be 3.6, buffering pair it is total dense
Degree is the citric acid-sodium citrate buffer of 4 weight %, is evenly added in the first material in 1 hour, with
1000 revs/min of mixing speed is uniformly mixed, and is adjusted pH value as 6.2 and is obtained second material；At room temperature, it is by concentration
The phosphoric acid of 4 weight % is evenly added in the second material in 1.5 hours, mixed with 1200 revs/min of mixing speed
It closes uniformly, adjusts pH value as 3.2 and obtain third material；Under conditions of 60 DEG C, the third material is handled 2 hours and is consolidated
Change bunching product, and it is 7 that 5 weight % ammonium hydroxide, which are added, to adjust pH value into the solidification bunching product, obtains 4 materials, i.e., it is high
Imitate lambda-cyhalothrin microcapsule suspending agent；Sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol mixing are added into the 4 materials
Uniformly, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:0.02:0.004:
0.04。
The preparation method of thiacloprid suspending agent is same as Example 1.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight ratio of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
For 1:0.2:0.03,22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent are obtained.
Embodiment 11
Benzoguanamine, formaldehyde and water are mixed, are 7.5 in pH value, temperature reacts 1.5h under the conditions of being 70 DEG C, obtains
Benzoguanamine-formaldehyde resin performed polymer aqueous solution, wherein the weight ratio of formaldehyde, benzoguanamine and water is 1:3.2:
2.8。
It is same as Example 1 that efficient cyhalothrin emulsifiable concentrate obtains preparation method, wherein the gamma cyhalothrin,
The weight ratio of 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether is 1:2:0.06.
Benzoguanamine-formaldehyde resin performed polymer aqueous solution and efficient cyhalothrin emulsifiable concentrate are mixed by weight 4:1
It closes, is stirred evenly with 2000 revs/min of rate, obtain first material；It then at room temperature, is 4 by pH value, buffering pair
Total concentration be 4 weight % citric acid-sodium citrate buffer, the first material is evenly added in 1 hour
In, it is uniformly mixed with 1000 revs/min of mixing speed, adjusting pH value is 6.2, obtains second material；At room temperature, will
Concentration is that the sulfuric acid of 5 weight % is evenly added in the second material in 1.5 hours, with 1200 revs/min of stirring
Speed is uniformly mixed, and adjusting pH value is 3.2, obtains third material；It is under conditions of 60 DEG C, third material processing 2 is small
When obtain solidification bunching product, and it is 7 that 5 weight % ammonium hydroxide, which are added into the solidification bunching product, to adjust pH value, obtains the 4th
Material, i.e. lambda-cyhalothrin microcapsule suspension；Sodium lignin sulfonate, aluminum magnesium silicate and second are added into the 4 materials
Glycol is uniformly mixed, wherein the weight ratio of the 4 materials and sodium lignin sulfonate, aluminum magnesium silicate and ethylene glycol is 1:
0.03:0.005:0.05.
The preparation method of thiacloprid suspending agent is same as Example 1.
Finally, lambda-cyhalothrin microcapsule suspension is mixed with thiacloprid suspending agent, sodium lignin sulfonate is added
And water, it stirs evenly, wherein the weight ratio of lambda-cyhalothrin microcapsule suspension and thiacloprid suspending agent, sodium lignin sulfonate
For 1:0.15:0.04,22 weight % gamma cyhalothrins and thiacloprid microcapsule suspension-suspending agent are obtained.
Comparative example 1
This comparative example preparation method the difference from embodiment 1 is that, be added in Xiang Suoshu first material pH value be 4.5, it is slow
The total concentration of punching pair is acetic acid-sodium acetate buffer solution of 2 weight %, adjusts pH value as 4 and obtains second material；It is prepared 22
Weight % gamma cyhalothrin and thiacloprid microcapsule suspension-suspending agent.
Comparative example 2
This comparative example preparation method the difference from embodiment 1 is that, be added in Xiang Suoshu first material pH value be 4.5, it is slow
The total concentration of punching pair is acetic acid-sodium acetate buffer solution of 2 weight %, adjusts pH value as 8 and obtains second material；It is prepared 22
Weight % gamma cyhalothrin and thiacloprid microcapsule suspension-suspending agent.
Comparative example 3
This comparative example preparation method the difference from embodiment 1 is that, the salt of 6 weight % is added in Xiang Suoshu second material
Acid adjusts pH value as 2 and obtains second material；22 weight % gamma cyhalothrins are prepared and thiacloprid microcapsule suspends-hangs
Floating agent.
Comparative example 4
This comparative example preparation method the difference from embodiment 1 is that, the salt of 6 weight % is added in Xiang Suoshu second material
Acid adjusts pH value as 5 and obtains third material；22 weight % gamma cyhalothrins are prepared and thiacloprid microcapsule suspends-hangs
Floating agent.
Comparative example 5
This comparative example preparation method the difference from embodiment 1 is that, the pH value for solidifying bunching product is adjusted to 5
Obtain 4 materials.
Comparative example 6
This comparative example preparation method the difference from embodiment 1 is that, the pH value for solidifying bunching product is adjusted to 9
Obtain 4 materials.
Comparative example 7
This comparative example preparation method the difference from embodiment 1 is that, after obtaining first material, without using pH value to be
4.5, it is 6.2 to obtain second that the acetic acid that the total concentration of buffering pair is 2 weight %-sodium acetate buffer solution, which adjusts mixed solution pH value,
The step of material.
Comparative example 8
This comparative example preparation method the difference from embodiment 1 is that, after obtaining second material, without concentration be 5 weight %
Hydrochloric acid to adjust mixed solution pH value be 3.2 the step of obtaining third material.
Comparative example 9
This comparative example preparation method the difference from embodiment 1 is that, after obtaining third material, solidify bunching without 60 DEG C
Step.
Comparative example 10
This comparative example preparation method the difference from embodiment 1 is that, obtain solidification bunching product after, without adjust pH be 7
The step of obtaining 4 materials.
Comparative example 11
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed,
Obtain efficient cyhalothrin emulsifiable concentrate, wherein the gamma cyhalothrin, 200# solvent naphtha and anhydrous sorbitol monostearate
The weight ratio of ester APEO is 1:2.5:0.05.Fluazinam suspending agent is prepared with 1 same procedure of embodiment, by efficient chlorine
Flucythrinate missible oil is that 1:0.3 is mixed with fluazinam suspending agent by weight, obtains 22 weight % gamma cyhalothrins and thiophene
The micro- suspoemulsion of worm quinoline.
Comparative example 12
Gamma cyhalothrin, 200# solvent naphtha and sorbitan monostearate polyoxyethylene ether are uniformly mixed,
Gamma cyhalothrin oil phase is obtained, water is slowly dropped into gamma cyhalothrin oil phase, is stirred when being added dropwise, and second is added
Two pure and mild xanthan gum, wherein the gamma cyhalothrin, 200# solvent naphtha, sorbitan monostearate polyoxyethylene
Ether, water, ethylene glycol and xanthan gum weight ratio be 1:2.5:0.05:1.2:0.005:0.001, obtain the efficient chlorine of 21 weight %
Flucythrinate aqueous emulsion.
Comparative example 13
By the thiacloprid (content 95%) of 26.3 weight %, the lauryl sodium sulfate 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 water of the sodium benzoate and 60 weight % of measuring % is sufficiently mixed, disperses, and is passed through sand mill after being uniformly dispersed and is sanded, and is sanded extremely
Suspension of the average grain diameter less than 5 microns, obtains thiacloprid suspending agent.
Testing example 1
This testing example is for gamma cyhalothrin and thiophene obtained in testing example 1-11 and comparative example 1-10
Gamma cyhalothrin obtained in worm quinoline microcapsule suspension-suspendinagent agent and comparative example 11 and the micro- suspoemulsion of thiacloprid, comparative example 12
Gamma cyhalothrin aqueous emulsion and comparative example 13 thiacloprid suspending agent heat storage stability and low-temperature stability.
Heat storage stability test: by gamma cyhalothrin and thiacloprid obtained in embodiment 1-11 and comparative example 1-10
The height of gamma cyhalothrin obtained in microcapsule suspension-suspendinagent agent and comparative example 11 and the micro- suspoemulsion of thiacloprid, comparative example 12
Effect lambda-cyhalothrin aqueous emulsion and the thiacloprid suspending agent of comparative example 13 are fitted into container, and (54 ± 2) DEG C are placed in after sealing
It in constant temperature oven, is taken out after standing 14 days, according to GB/T14825-2006 standard, measures suspensibility, the results are shown in Table 1.
Low-temperature stability measurement: by gamma cyhalothrin and thiacloprid obtained in embodiment 1-11 and comparative example 1-10
The height of gamma cyhalothrin obtained in microcapsule suspension-suspendinagent agent and comparative example 11 and the micro- suspoemulsion of thiacloprid, comparative example 12
Effect lambda-cyhalothrin aqueous emulsion and the thiacloprid suspending agent of comparative example 13 are fitted into container, and sealing is placed on (0 ± 2) DEG C refrigerator
In, 1h is kept, stirs primary, each 15s at interval of 15min, observation appearance has unchanged, continues to place 7 days in (0 ± 2) DEG C,
It then takes out after being placed in standing recovery under room temperature, according to GB/T14825-2006 standard, measures suspensibility, the results are shown in Table 1.
Table 1
As it can be seen from table 1 the gamma cyhalothrin and thiacloprid microcapsule that preparation method provided by the invention obtains are outstanding
Floating-suspending agent has good thermal storage stability and low tempertaure storage stability.
Testing example 2
This testing example is to gamma cyhalothrin and thiacloprid microcapsule obtained in embodiment 1-11, comparative example 1-10
The efficient chlorine fluorine of gamma cyhalothrin obtained in suspension-suspending agent, comparative example 11 and the micro- suspoemulsion of thiacloprid, comparative example 12
Cyano chrysanthemate aqueous emulsion and the thiacloprid suspending agent of comparative example 13 test the control efficiency of the flea beetle on potato.Before test
A certain amount of distilled water is added, stirs evenly, is adjusted respectively by efficient chlorine fluorine cyanogen obtained in embodiment 1-11, comparative example 1-10
It is gamma cyhalothrin obtained in pyrethroids and thiacloprid microcapsule suspension-suspending agent, comparative example 11 and the micro- suspoemulsion of thiacloprid, right
Activity component concentration in the gamma cyhalothrin aqueous emulsion of ratio 12 and the thiacloprid suspending agent of comparative example 13 is 10 weights
Measure %.
Test site: Hebei province's Zhangjiakou City, experimental plot are many years potato planting base, and experimental plot topography is flat, fertilizer
Power is medium, earth in quality.The routinely production management of area potato is managed everywhere in after application.
Specific steps include, and are 30kg/ mus according to formulation rate using knapsack sprayer, by embodiment 1-11, comparison
Efficient chlorine fluorine obtained in gamma cyhalothrin obtained in example 1-10 and thiacloprid microcapsule suspension-suspending agent, comparative example 11
The thiacloprid suspending agent of Cyano chrysanthemate and the micro- suspoemulsion of thiacloprid, the gamma cyhalothrin aqueous emulsion of comparative example 12 and comparative example 13
Medical fluid is respectively sprayed the potato plant of each growing area, and blank control group is using equivalent clear water to the horse in growing area
Bell potato plant is sprayed.
10 days, 20 days, the 30 days and 50 days investigation flea beetle control efficiency after application, specific test method is according to " pesticide field
Between pharmacodynamic test criterion " carry out.For each treatment region using random 5 points samplings, each processing cell investigates 25 clumps of potatos, investigation
Each treatment region flea beetle control efficiency calculates the death rate by formula (1) and calculates corrected mortality by formula (2), and the results are shown in Table 2.
Table 2
Testing example 3
This testing example is micro- to gamma cyhalothrin obtained in embodiment 1-11 and comparative example 1-10 and thiacloprid
Capsule suspension-suspending agent tests the control efficiency of diamondback moth on Chinese cabbage, aphid.A certain amount of distillation is added before test
Water stirs evenly, and the gamma cyhalothrin and thiacloprid microcapsule that adjusting embodiment 1-11 and comparative example 1-10 is obtained suspend-hang
The gamma cyhalothrin of gamma cyhalothrin and the micro- suspoemulsion of thiacloprid, comparative example 12 obtained in floating agent, comparative example 11
Activity component concentration in aqueous emulsion and the thiacloprid suspending agent of comparative example 13 is 10 weight %.
Test site: Shijiazhuang City of Hebei Province.The plot topography is flat, and fertility is preferable.Qu great Bai is managed everywhere in after application
Dish routinely production management.
Specific steps include, and are 30kg/ mus according to spouting liquid, by embodiment 1-11 and comparison using knapsack sprayer
Efficient chlorine fluorine obtained in gamma cyhalothrin obtained in example 1-10 and thiacloprid microcapsule suspension-suspending agent, comparative example 11
The thiacloprid suspending agent of Cyano chrysanthemate and the micro- suspoemulsion of thiacloprid, the gamma cyhalothrin aqueous emulsion of comparative example 12 and comparative example 13
Medical fluid is uniformly sprayed respectively on the Chinese cabbage plant of each growing area, and blank control group is using equivalent clear water in growing area
Chinese cabbage plant is sprayed, and when application, is blocked neighboring community with plastic film, is prevented medicament from interfering with each other.
10 days, 20 days, 30 days and 50 days investigation diamondback moths, the prevention and control of aphids effects after application, specific test method according to
" pesticide field efficacy medicine test criterion " carries out.Each treatment region investigates 25 plants of great Bai using random 5 points samplings, each processing cell
Dish investigates each treatment region Chinese cabbage diamondback moth, prevention and control of aphids effect, the same testing example of the calculating of the death rate and corrected mortality
2, concrete outcome is shown in Table 3:
Table 3
Through embodiment 1-11 as can be seen that preparation method provided by the invention is adjusted by multistep compared with comparative example 1-10
PH value, the gamma cyhalothrin and thiophene being prepared under the reaction conditions such as specific speed of agitator, emulsifying dispersant, solvent
Worm quinoline microcapsule suspension-suspendinagent agent prevents and treats the effect of crop pests in which can obtain slow release long-acting.And this method preparation is efficient
Lambda-cyhalothrin and thiacloprid microcapsule suspension-suspending agent effect are much better than gamma cyhalothrin aqueous emulsion single dose, thiophene worm
Quinoline suspending agent single dose.Through embodiment 1-11 it can be seen that gamma cyhalothrin and thiophene of the invention compared with comparative example 11-13
Worm quinoline microcapsule suspension-suspendinagent agent has lasting period length relative to containing other of gamma cyhalothrin and/or thiacloprid dosage form
Feature, wherein the organic solvent contained is few, can be reduced to environment so as to reduce times for spraying and dosage, save the cost
Pollution.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
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 equally should be considered as the content that the present invention is invented.
Claims (10)
1. a kind of method for preparing the microcapsule suspension-suspendinagent agent containing thiacloprid and gamma cyhalothrin, which is characterized in that should
Method includes the following steps:
A, the first solution and the second solution are uniformly mixed, obtain first material；First solution contains amino-formaldehyde resins
Performed polymer aqueous solution；Second solution contains efficient cyhalothrin emulsifiable concentrate；First solution and second solution
Weight ratio is (1-5): 1；
B, buffer solution is added in Xiang Suoshu first material to be uniformly mixed, makes mixed solution pH value 4-7, obtains second material；
C, acidic ph modifier is added in Xiang Suoshu second material to be uniformly mixed, makes mixed solution pH value 3-4, obtains third object
Material；
D, the third material is subjected to solidification bunching, obtains solidification bunching product, adjusting the solidification bunching product pH value is
6-8 obtains 4 materials；
E, the 4 materials are uniformly mixed with thiacloprid suspending agent, are obtained micro- containing thiacloprid and gamma cyhalothrin
Capsule suspension-suspending agent；The weight ratio of the 4 materials and the thiacloprid suspending agent is 1:(0.1-1).
2. the method according to claim 1, wherein the amino-formaldehyde resins performed polymer in step a is water-soluble
Liquid is obtained by the material liquid prepolymerization of amino-containing compound, the formaldehyde and water；The amino-containing compound include urea,
At least one of melamine and benzoguanamine；The weight ratio of the formaldehyde, the amino-containing compound and water is
1:(0.2-12): (2-6)；The prepolymerized condition includes: that pH value is 8-10, and temperature is 60-80 DEG C, reaction time 0.5-
3 hours.
3. method according to claim 1 or 2, which is characterized in that the efficient cyhalothrin emulsifiable concentrate in step a contains
There are gamma cyhalothrin, organic solvent and emulsifier；The organic solvent includes petroleum ether, ethyl acetate, methyl oleate, two
At least one of toluene and solvent naphtha；The emulsifier includes sodium lignin sulfonate, lauryl sodium sulfate, detergent alkylate
Sodium sulfonate, fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, loses styrene-maleic anhydride copolymer
In water sorbitol monostearate polyoxyethylene ether, sldium lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate at least
It is a kind of；The weight ratio of the gamma cyhalothrin, the organic solvent and the emulsifier is 1:(0.1-5): (0.01-
0.2)。
4. the method according to claim 1, wherein the pH value of the buffer solution in step b is 3-5.5；
The buffer solution contains buffering pair, and the buffering is to including citric acid-sodium citrate, citrate-phosphate disodium hydrogen and acetic acid-
At least one of sodium acetate；The total concentration of buffering pair described in the buffer solution is 1-5 weight %.
5. the method according to claim 1, wherein the acidic ph modifier in step c contains hydrochloric acid, sulphur
At least one of acid, phosphoric acid, acetic acid and ammonium chloride；The concentration of the acidic ph modifier is 1-10 weight %.
6. the method according to claim 1, wherein this method includes, in step e, by the 4 materials with
After the mixing of at least one of first dispersing agent, the first thickener and first antifreezing agent, then mix with the thiacloprid suspending agent；
First dispersing agent include neopelex, sodium methylene bis-naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensate,
Benzyl naphthalene sulfonic acid-formaldehyde condensation product, sodium lignin sulfonate, desugar sodium lignin sulfonate, desugar are condensed sodium lignin sulfonate, fourth two
At least one of acid esters sodium sulfonate, pull open powder, nonylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether；First thickening
Agent includes at least one in aluminum magnesium silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black
Kind；First antifreezing agent includes at least one of ethylene glycol, 1,2- propylene glycol, glycerine and urea；The 4 materials,
The weight ratio of first dispersing agent, first thickener and first antifreezing agent is 1:(0.01-0.2): (0.001-
0.02): (0.02-0.15).
7. method according to claim 1 or 6, which is characterized in that this method includes, in step e, by the 4 materials
It is mixed after the third dispersant, then with the thiacloprid suspending agent；The 4 materials, the thiacloprid suspending agent
Weight ratio with the third dispersing agent is 1:(0.1-1): (0.01-2).
8. method according to claim 1 or 6, which is characterized in that the thiacloprid suspending agent in step e contains partial size
Thiacloprid particle, water and adjuvant less than 5 μm；The weight ratio of the thiacloprid particle, the adjuvant and the water is 1:
(1-2): (2-5)；Preferably, the adjuvant includes the second dispersing agent, defoaming agent, the second thickener, the second antifreezing agent and prevents
At least one of rotten agent；It is the thiacloprid particle, second dispersing agent, the defoaming agent, second thickener, described
The weight ratio of second antifreezing agent and the preservative is 1:(0.15-0.3): (0.003-0.01): (0.003-0.01): (0.15-
0.3): (0.003-0.01).
9. the method according to claim 1, wherein the mixed condition in step a includes: mixing speed
It is 1500-3000 revs/min；The mixed condition in step b includes: that mixing speed is 1000-1200 revs/min；Step
The mixed condition in rapid c includes: that mixing speed is 1200-1500 revs/min；The solidification bunching in step d
Condition includes: to handle 2-6 hours under the conditions of 40-70 DEG C.
10. according to claim 1 method described in any one of -9 preparation containing thiacloprid and gamma cyhalothrin
Microcapsule suspension-suspendinagent agent.
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| WO2022034559A1 (en) * | 2020-08-14 | 2022-02-17 | Upl Limited | A storage stable insecticidal composition |
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Application publication date: 20190329 |