CN106561640A - Micro-capsule suspension-suspending agent containing abamectin and etoxazole and preparation method of micro-capsule suspension-suspending agent - Google Patents
Micro-capsule suspension-suspending agent containing abamectin and etoxazole and preparation method of micro-capsule suspension-suspending agent Download PDFInfo
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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Abstract
The invention discloses a micro-capsule suspension-suspending agent containing abamectin and etoxazole and a preparation method of the micro-capsule suspension-suspending agent. The preparation method comprises the following steps: (1) a first solution containing benzoperoxide and methyl methacrylate is mixed with a second solution containing an abamectin emulsifiable concentrate uniformly, and a first material is obtained; (2) the first material is mixed with water uniformly, and after stirring and emulsification, a second material is obtained; (3) a NaHSO3 solution is added to the second material and is mixed uniformly, and a third material is obtained; (4) the third material is subjected to solidified and condensed, a solidified and condensed product is obtained, the pH value of the solidified and condensed product is adjusted to 6-8, and a fourth material is obtained; (5) a dispersing agent is added to the fourth material, and a fifth material is obtained; and (6) the fifth material is mixed with an etoxazole suspending agent uniformly, and the micro-capsule suspension-suspending agent is obtained. The micro-capsule suspension-suspending agent is long in duration of efficacy, and the dosage of a pesticide can be reduced effectively.
Description
Technical field
It relates to technical field of pesticide, in particular it relates to a kind of microcapsule suspension containing avilamycin and etoxazole-outstanding
Floating agent.
Background technology
Avilamycin is a kind of parasite killing widely used agricultural or for animals, sterilization, acaricide, by vast pesticide producing enterprise
Industry and the favor of peasant.But avilamycin photolysis are abnormal strong, in plant and soil surface due to the irradiation of ultraviolet light, medicament
Decomposition failure quickly, therefore reduce its preventive effect.In addition, on market avilamycin preparation based on cream, containing a large amount of organic molten
Agent, both waste of resource, polluted environment again.Therefore, by avermectin microcapsule it is one of important channel for solving the above problems.
But avermectin microcapsule suspending agent is prepared with traditional method such as interfacial polymerization, original flavor polymerization, not only technique is loaded down with trivial details, plus
Work high cost, and reunion, solidification phenomenon are susceptible to, cause to be difficult storage.Avilamycin can reach both with etoxazole compounding
Quick-acting purposes, reduces dosage, so as to reduce the pollution to environment.
But, there is number of drawbacks in existing avilamycin, such as wettable powder easily draws with the combination medicament of etoxazole
Product bonding is played, should not disperse to suspend in water, precipitation makes medicament sprinkling uneven in aerosol apparatus, and the storage of existing medicament
Deposit stability relatively low, synergy is not obvious enough.
Therefore, in the urgent need to developing a kind of novel agrochemical formulations containing avilamycin and etoxazole so as to which potentiation substantially, is held
The effect phase extends, and stores stable.
The content of the invention
The purpose of the disclosure is to provide a kind of novel agrochemical dosage form containing avilamycin and etoxazole, the novel agrochemical dosage form
The lasting period of avilamycin and etoxazole can be obviously prolonged.
To achieve these goals, the disclosure provides a kind of microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole
Preparation method, the preparation method may include steps of:(1) by the first solution and the second solution mix homogeneously, first is obtained
Material;Wherein described first solution contains benzoyl peroxide and methyl methacrylate;Second solution contains Avermectin
Plain cream;First solution is 1 with the weight ratio of second solution:(50-200);(2) first material and water are mixed
Close uniform, stirring and emulsifying obtains second material;The first material is 1 with the weight ratio of water:(0.5-5);(3) to described second
NaHSO is added in material3Solution, obtains 3 material after mix homogeneously;Benzoyl peroxide and NaHSO in the second material3
NaHSO in solution3Weight ratio be 1:(1-3);(4) 3 material is carried out into solidification bunching, obtains solidifying bunching product;
It is 6-8 to add pH adjusting agent to make the pH value of the solidification bunching product in the solidification bunching product, obtains 4 materials;
(5) dispersant is added in the 4 materials, obtains the 5th material;The 4 materials are with the weight ratio of the dispersant
1:(0.01-0.1);(6) the 5th material is mixed homogeneously with etoxazole suspending agent, is obtained containing avilamycin and etoxazole
Microcapsule suspension-suspendinagent agent;5th material is 1 with the weight ratio of etoxazole suspending agent:(0.5-20).
The invention provides a kind of microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole, the suspending agent is by above institute
The method stated is prepared.
By above-mentioned technical proposal, the microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole that the present invention is provided can
The preventing and treating crop pests of slow release long-acting, and with good quick-acting, dosage and times for spraying can be reduced, so as to save
The pollution of cost and reduction to environment.
Other feature and advantage of the disclosure will be described in detail in subsequent specific embodiment part.
Specific embodiment
Hereinafter specific embodiment of this disclosure is described in detail.It should be appreciated that described herein concrete
Embodiment is merely to illustrate and explains the disclosure, is not limited to the disclosure.
The disclosure provides a kind of preparation method containing avilamycin and the microcapsule suspension-suspendinagent agent of etoxazole, the preparation side
Method may include steps of:(1) by the first solution and the second solution mix homogeneously, first material is obtained;Wherein described first
Solution contains benzoyl peroxide and methyl methacrylate;Second solution contains abamectin emulsifiable concentrate;Described first is molten
Liquid is 1 with the weight ratio of second solution:(5-10);(2) first material is mixed homogeneously with water, stirring obtains second
Material;The first material is 1 with the weight ratio of water:(1-5);(3) NaHSO is added in the second material3Solution, mixing
3 material is obtained after uniform;Benzoyl peroxide and NaHSO in the second material3NaHSO in solution3Weight ratio be 1:
(1-3);(4) 3 material is carried out into solidification bunching, obtains solidifying bunching product;Add in the solidification bunching product
It is 6-8 that pH adjusting agent makes the pH value of the solidification bunching product, obtains 4 materials;(5) add in the 4 materials and divide
Powder, obtains the 5th material;The 4 materials are 1 with the weight ratio of the dispersant:(0.01-0.1);(6) by described
Five materials are mixed homogeneously with etoxazole suspending agent, obtain the microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole;Described 5th
Material is 1 with the weight ratio of etoxazole suspending agent:(0.5-20).
In the present invention, avilamycin (Abamectin), molecular formula C48H72O14(B1a)·C47H70O14(B1b), average molecular
Amount B1a:873.09,B1b:859.06, No. CAS:71751-41-2, structural formula is as follows:
Etoxazole (etoxazole), chemical name is (the RS) -5- tert-butyl group -2- [2- (2,6- difluorophenyl) -4,5- bis-
Hydrogen -1.3- oxazole -4- bases] ethoxybenzene.Molecular formula C21H23F2NO2, relative molecular weight 359.4, No. CAS:153233-91-1,
Structural formula is as follows:
According to the present invention, the microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole obtained by above-mentioned preparation method,
It is not susceptible to reunite and coacervation, is capable of the preventing and treating crop pests of slow release long-acting, and with good quick-acting, can drops
Low dosage and times for spraying, so as to pollution cost-effective and that reduction is to environment.
According to the first aspect of the invention, the composition pesticide can also be containing compositionss adjuvant.Wherein, aid in
The consumption of agent is known to those skilled in the art without particular/special requirement, for example, relative to the active component of 1 weight portion, compositionss
Can be 0.01-100 weight portions with the content of adjuvant;Preferably, relative to the active component of 1 weight portion, compositionss adjuvant
Content for can be with 0.2-50 weight portions.
According to the first aspect of the invention, can as needed to match this area normal for the adjuvant in the composition pesticide
Composition, for example, adjuvant can be selected from dispersant, wetting agent, antifreezing agent, preservative, thickening agent, emulsifying agent, You Jirong
At least one in agent and defoamer.In the present invention, for mentioned component is without particular/special requirement, can adopt commonly used in the art
Material, for example:
The dispersant can be dodecyl benzene sulfonate, di-2-ethylhexylphosphine oxide naphthalene sulfonate, 1- methyl naphthalene sulfonic acid sodium formaldehydes
Condensation substance, benzyl naphthalene sulfonic acid-formaldehyde condensation product, lignosulfonates, desaccharide lignosulfonates, desaccharide condensation lignin sulfonic acid
At least one in salt, succinate sulfonate, pull open powder, phosphoric acid ester, polycarboxylic acid salt and fatty alcohol-polyoxyethylene ether;
The wetting agent can for sodium lauryl sulphate, sodium laurylsulfate, pull open powder, dodecylbenzene sodium sulfonate,
At least one in diisobutyl sodium sulfonate, fatty alcohol-polyoxyethylene ether or alkylphenol polyoxyethylene;
The antifreezing agent can be ethylene glycol, 1,2-PD, glycerol, carbamide, Polyethylene Glycol, Sorbitol, Sodium Chloride
In at least one;
The preservative can be at least in formaldehyde, Kazon, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate
Kind;
The thickening agent can be Magnesiumaluminumsilicate, xanthan gum, polyvinyl alcohol, sodium alginate, guar gum, carboxymethyl cellulose
At least one in sodium, organobentonite, white carbon;
The emulsifying agent can include sodium lignin sulfonate, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, benzene second
Alkene-copolymer-maleic anhydride, fatty alcohol-polyoxyethylene ether, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, anhydrous sorbitol list
At least one in stearate polyoxyethylene ether, sodium laurylsulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate;
The organic solvent can be 200# solvent naphthas, N-Methyl pyrrolidone, petroleum ether, ethyl acetate, toluene, N, N-
At least one in dimethylformamide, chloroform, isopropanol, dimethylbenzene and solvent naphtha;
The defoamer can be at least one in silicone oil, higher alcohol, mineral oil or vegetable oil.
Wherein, in step (1), the system that the preparation method of the abamectin emulsifiable concentrate can be known to the skilled person
Preparation Method, the present invention has no particular limits to this.Under preferable case, the abamectin emulsifiable concentrate contains avilamycin, organic
Solvent and emulsifying agent;Preferably, avilamycin and the mass ratio of the organic solvent, the emulsifying agent can be 1:(14-19):
(1-4)。
Wherein, in order to further lift the clad ratio of microcapsule, in step (1), benzoyl peroxide first in first solution
The weight ratio of acyl and methyl methacrylate is 1:(200-1000).
Wherein, in step (3), the NaHSO3NaHSO in solution3Concentration be 0.01-0.1 weight %.
Wherein, in step (4), described pH adjusting agent can be the various materials that can adjust pH value;Under preferable case,
The pH adjusting agent can include hydrochloric acid, sulphuric acid, phosphoric acid, acetic acid, ammonium chloride and sodium hydroxide, sodium carbonate, potassium carbonate, citric acid
At least one in potassium, sodium citrate;The concentration of the pH adjusting agent can be 0.5-8 weight %.
Wherein, in order to further improve the particle diameter distribution and bin stability of avermectin microcapsule suspending agent, step (5)
In, can also be containing thickening agent and/or antifreezing agent in the 5th material;The 4 materials, the dispersant, the thickening
Agent, the weight ratio of the antifreezing agent can be 1:(0.01-0.1):(0.001-0.02):(0.02-0.15).
Wherein, the preparation method of the etoxazole suspending agent can be preparation method well known to those skilled in the art, this
Invention has no particular limits to it;In order to further lift the stability of etoxazole suspending agent, under preferable case, step (6)
In, the etoxazole suspending agent can be containing etoxazole microgranule of the particle diameter less than 5 μm, water and adjuvant;The etoxazole microgranule,
The weight ratio of adjuvant and water can be 1:(1-20):(0.5-50);Preferably, the adjuvant can include dispersant, disappear
Infusion, thickening agent, antifreezing agent and at least one of the preservatives;The etoxazole microgranule, the dispersant, the defoamer,
The weight ratio of the thickening agent, the antifreezing agent and the preservative is 1:(2-15):(2-15):(0.005-0.1):(2-
15):(2-15).
Wherein, in order to further lifted the bin stability of suspending agent with it is long-lasting, in step (6), the avilamycin
With also contain dispersant in the microcapsule suspension-suspendinagent agent of etoxazole;The avermectin microcapsule suspending agent, etoxazole suspending agent and
The weight ratio of dispersant is 1:(0.1-10):(0.01-2).
Wherein, in order to avoid there is the phenomenon such as microcapsule aggregation, precipitation, hardened, described mixing condition includes:Step (2)
In, described emulsification condition includes:3-10min is stirred under 50-200 rev/min of speed;In step (3), described mixing
Conditions Condition includes:Under 100-300 rev/min of stir speed (S.S.), with the speed addition dripped every 4-5 minutes Deca 1
NaHSO3Solution, and the time of Deca stirring is 60-90min;In step (4), described solidification bunching condition includes:
Be polymerized 1-8h under the conditions of 10-40 DEG C.
According to the present invention, the present invention also provides a kind of microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole, the suspension
Agent is obtained according to preparation method as above.
Be further elaborated by the following examples the present invention, but the present invention does not therefore suffer from any limit
System.
Avilamycin is purchased from Shandong Weifang Rainbow Chemical Co., Ltd.;Etoxazole is purchased from Jiangsu Province Nantong Thailand standing grain chemical industry
Company limited;Benzoyl peroxide (BPO) is purchased from Laiwu City Heng Tong Chemical Co., Ltd.;Methyl methacrylate (MMA) is purchased from
Shanghai Mai Ruier chemical technologies company limited;N-Methyl pyrrolidone is purchased from Jiangsu Kangheng Chemical Co., Ltd.;Detergent alkylate
Sulfoacid calcium, sorbitan monostearate polyoxyethylene ether are purchased from Cangzhou Hong Yuan agrochemical company limited;Sodium lignin sulfonate, wood
Quality sulfoacid calcium is purchased from Shandong Lv Cheng Chemical Co., Ltd.s;Ethylene glycol, NaHSO3Beijing Chemical Plant is purchased from carbamide;Xanthan gum is purchased
From Zibo Deosen Biochemical Ltd.;Sodium methylene bis-naphthalene sulfonate is purchased from Jinan City Licheng District Gaosheng chemical industry;Aluminium-magnesium silicate is purchased from
Hunan Peng Tai new high-tech materials company limited.
Embodiment 1
Benzoyl peroxide (BPO) is dissolved in methyl methacrylate (MMA), mix homogeneously, wherein BPO are with MMA's
Weight ratio is 1:1000.
By avilamycin, N-Methyl pyrrolidone, calcium dodecyl benzene sulfonate, sorbitan monostearate polyoxy second
Alkene ether mix homogeneously, obtains abamectin emulsifiable concentrate, wherein, the avilamycin and N-Methyl pyrrolidone, detergent alkylate sulphur
Sour calcium, the mass ratio of sorbitan monostearate polyoxyethylene ether are 1:8.5:1:1.5:0.4.
By gained BPO/MMA solution and abamectin emulsifiable concentrate mix homogeneously, first material is obtained, wherein the BPO/MMA
The weight ratio of solution and abamectin emulsifiable concentrate is 1:100;At ambient temperature, the first material is mixed with water, Jing 50r/
Min stirs 3min, obtains second material, and wherein first material and the weight ratio of water are 1:1;At ambient temperature, by 0.01 weight
The NaHSO of amount %3Solution is slowly added dropwise to the second material with the speed dripped every 4-5 minutes Deca 1, while with 100r/
The speed of min is stirred to it, obtains 3 material, wherein, BPO and NaHSO in the second material3NaHSO in solution3
Weight ratio be 1:1;Under conditions of room temperature, the 3 material is carried out into polycondensation 2h, obtain solidifying bunching product;To
1 weight %NH is added in the solidification bunching product4Cl, pH value is adjusted to 7, obtains 4 materials;To the 4 materials
Middle addition sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously, obtain the 5th material, i.e. avermectin microcapsule and suspend
Agent, wherein, the 4 materials are 1 with the mass ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.01:0.005:
0.05。
By the etoxazole (content is 96%) of 50 weight %, the sodium lauryl sulphate of 0.5 weight %, 3 weight % wood
Quality sodium sulfonate, the organic silicon defoamer of 2 weight %, the ethylene glycol of 5 weight %, the xanthan gum of 0.3 weight %, 0.2 weight %
Sodium benzoate be sufficiently mixed, disperse with the water of 40 weight %, sand mill is passed through after being uniformly dispersed carries out sand milling, and sand milling is to average
Suspension of the particle diameter less than 5 microns, obtains etoxazole suspending agent.
Finally, avermectin microcapsule suspending agent is mixed with etoxazole suspending agent, adds sodium lignin sulfonate, use water
Supply, stir, wherein, avermectin microcapsule suspending agent and etoxazole suspending agent, the ratio of sodium lignin sulfonate are 1:
0.3:0.02, obtain 13 weight % avilamycin etoxazole microcapsule suspension-suspendinagent agents.
Embodiment 2
Benzoyl peroxide (BPO) is dissolved in methyl methacrylate (MMA), mix homogeneously, wherein BPO are with MMA's
Weight ratio is 1:1000.
The preparation method of abamectin emulsifiable concentrate is same as Example 1.
By gained BPO/MMA solution and abamectin emulsifiable concentrate mix homogeneously, first material is obtained, wherein the BPO/MMA
The weight ratio of solution and abamectin emulsifiable concentrate is 1:200;At ambient temperature, the first material is mixed with water, Jing 100r/
Min stirs 3min, obtains second material;Wherein first material and the weight ratio of water are 1:0.8;At ambient temperature, by 0.01
The NaHSO of weight %3Solution is slowly added dropwise to the second material with the speed dripped every 4-5 minutes Deca 1, while with
The speed of 100r/min is stirred to it, obtains 3 material, wherein, BPO and NaHSO in the second material3In solution
NaHSO3Weight ratio be 1:1.5;Under conditions of room temperature, the 3 material is carried out into polycondensation 2h, obtain solidification poly-
Contracting product;1 weight %NH is added in the solidification bunching product4PH value is adjusted to 7 and obtains 4 materials by Cl;To described
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously are added in 4 materials, the micro- glue of the 5th material, i.e. avilamycin is obtained
Capsule suspending agent, wherein, the 4 materials are 1 with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.02:
0.005:0.05。
The preparation method of etoxazole suspension is same as Example 1.
Finally, avermectin microcapsule suspending agent is mixed with etoxazole suspending agent, adds sodium lignin sulfonate, use water
Supply, stir, wherein, avermectin microcapsule suspending agent and etoxazole suspending agent, the ratio of sodium lignin sulfonate are 1:
0.5:0.02, obtain 17.5 weight % avilamycin etoxazole microcapsule suspension-suspendinagent agents.
Embodiment 3
Benzoyl peroxide (BPO) is dissolved in methyl methacrylate (MMA), mix homogeneously, wherein BPO are with MMA's
Weight ratio is 1:1000.
The preparation method of abamectin emulsifiable concentrate is same as Example 1.
By gained BPO/MMA solution and abamectin emulsifiable concentrate mix homogeneously, first material is obtained, wherein the BPO/MMA
The weight ratio of solution and abamectin emulsifiable concentrate is 1:100;At ambient temperature, the first material is mixed with water, Jing 150r/
Min stirs 3min, obtains second material, and wherein first material and the weight ratio of water are 1:1.2;At ambient temperature, by 0.01
The NaHSO of weight %3Solution is slowly added dropwise to the second material with the speed dripped every 4-5 minutes Deca 1, while with
The speed of 100r/min is stirred to it, obtains 3 material, wherein, BPO and NaHSO in the second material3In solution
NaHSO3Weight ratio be 1:1.5;Under conditions of room temperature, the 3 material is carried out into polycondensation 2h, obtain solidification poly-
Contracting product;1 weight %NH is added in the solidification bunching product4PH value is adjusted to 7 and obtains 4 materials by Cl;To described
Sodium methylene bis-naphthalene sulfonate, xanthan gum and carbamide mix homogeneously are added in 4 materials, the micro- glue of the 5th material, i.e. avilamycin is obtained
Capsule suspending agent, wherein, the 4 materials are 1 with the weight ratio of sodium methylene bis-naphthalene sulfonate, xanthan gum and carbamide:0.01:
0.005:0.05。
The preparation method of etoxazole suspending agent is same as Example 1.
Finally, avermectin microcapsule suspending agent is mixed with etoxazole suspending agent, adds sodium methylene bis-naphthalene sulfonate,
Supplied with water, stirred, wherein, avermectin microcapsule suspending agent and etoxazole suspending agent, sodium methylene bis-naphthalene sulfonate
Ratio is 1:1:0.05, obtain 23.8 weight % avilamycin etoxazole microcapsule suspension-suspendinagent agents.
Embodiment 4
Benzoyl peroxide (BPO) is dissolved in methyl methacrylate (MMA), mix homogeneously, wherein BPO are with MMA's
Weight ratio is 1:200.
The preparation method of abamectin emulsifiable concentrate is same as Example 1.
By gained BPO/MMA solution and abamectin emulsifiable concentrate mix homogeneously, first material is obtained, wherein the BPO/MMA
The weight ratio of solution and abamectin emulsifiable concentrate is 1:100;At ambient temperature, the first material is mixed with water, Jing 200r/
Min stirs 3min, obtains second material;Wherein first material and the weight ratio of water are 1:1;At ambient temperature, by 0.01 weight
The NaHSO of amount %3Solution is slowly added dropwise to the second material with the speed dripped every 4-5 minutes Deca 1, while with 100r/
The speed of min is stirred to it, obtains 3 material, wherein, BPO and NaHSO in the second material3NaHSO in solution3
Weight ratio be 1:1;Under conditions of room temperature, the 3 material is carried out into polycondensation 2h, obtain solidifying bunching product;To
1 weight %NH is added in the solidification bunching product4PH value is adjusted to 6 and obtains 4 materials by Cl;To in the 4 materials
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously are added, the 5th material, i.e. avermectin microcapsule is obtained and is suspended
Agent, wherein, the 4 materials are 1 with the weight ratio of sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol:0.01:0.005:
0.05。
The preparation method of etoxazole suspending agent is same as Example 1.
Finally, avermectin microcapsule suspending agent is mixed with etoxazole suspending agent, adds sodium lignin sulfonate, use water
Supply, stir, wherein, avermectin microcapsule suspending agent and etoxazole suspending agent, the ratio of sodium lignin sulfonate are 1:
0.5:0.02, obtain 17.8 weight % avilamycin etoxazole microcapsule suspension-suspendinagent agents.
Embodiment 5
Benzoyl peroxide (BPO) is dissolved in methyl methacrylate (MMA), mix homogeneously, wherein BPO are with MMA's
Weight ratio is 1:800.
The preparation method of abamectin emulsifiable concentrate is same as Example 1.
By gained BPO/MMA solution and abamectin emulsifiable concentrate mix homogeneously, first material is obtained, wherein the BPO/MMA
The weight ratio of solution and abamectin emulsifiable concentrate is 1:200;At ambient temperature, the first material is mixed with water, Jing 150r/
Min stirring and emulsifyings 5min, obtain second material;At ambient temperature, by the NaHSO of 0.01 weight %3Solution is with every 4-5 point
The speed of the drop of clock Deca 1 is slowly added dropwise to the second material, while be stirred to it with the speed of 100r/min, obtains the
3 material, wherein, BPO and NaHSO in the second material3NaHSO in solution3Weight ratio be 1:1;Under conditions of room temperature,
The 3 material is carried out into polycondensation 8h, obtains solidifying bunching product;1 weight % is added in the solidification bunching product
NH4PH value is adjusted to 8 and obtains 4 materials by Cl;Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously are added, is obtained
5th material, i.e. avermectin microcapsule suspending agent, wherein, the 4 materials and sodium lignin sulfonate, Magnesiumaluminumsilicate and second
The weight ratio of glycol is 1:0.01:0.005:0.05.
The preparation method of etoxazole is same as Example 1.
Finally, avermectin microcapsule suspending agent is mixed with etoxazole suspending agent, adds sodium lignin sulfonate, use water
Supply, stir, wherein, avermectin microcapsule suspending agent and etoxazole suspending agent, the ratio of sodium lignin sulfonate are 1:
1:0.05, obtain 23.8 weight % avilamycin etoxazole microcapsule suspension-suspendinagent agents.
Comparative example 1
This comparative example is with the difference of embodiment 1:After obtaining first material, at ambient temperature, by NaHSO3
Solution is slowly added dropwise to the first material with the speed dripped every 4-5 minutes Deca 1, is then mixed with water again, is stirred, breast
Change, other are same as Example 1.
Comparative example 2
This comparative example is with the difference of embodiment 1:After obtaining second material, not Deca NaHSO3Solution, directly
By the second material polycondensation 2h, obtain solidifying bunching product, other are same as Example 1.
Comparative example 3
This comparative example is with the difference of embodiment 1:Obtain not carried out after 3 material solidifying bunching and directly adjust
PH value is 7, and other are same as Example 1
Comparative example 4
This comparative example is with the difference of embodiment 1:Obtain solidify bunching product after, do not adjust pH value, directly to
Sodium lignin sulfonate, Magnesiumaluminumsilicate and ethylene glycol mix homogeneously are added in the solidification bunching product, the micro- glue of avilamycin is obtained
Capsule suspending agent, other are same as Example 1.
Comparative example 5
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent, difference are prepared
The weight ratio for being BPO and MMA is 1:1500.
Comparative example 6
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent, difference are prepared
The weight ratio for being BPO and MMA is 1:100.
Comparative example 7
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent, difference are prepared
The weight ratio for being BPO/MMA solution and abamectin emulsifiable concentrate in the first material is 1:1.
Comparative example 8
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent, difference are prepared
The weight ratio for being BPO/MMA solution and abamectin emulsifiable concentrate in the first material is 1:15.
Comparative example 9
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent is prepared, difference is
NaHSO3The drop rate of solution is dripped for Deca 1 at intervals of two minutes.
Comparative example 10
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent is prepared, difference is
It is 5000r/min, time 1min to the stir speed (S.S.) of first material.
Comparative example 11
According to the preparation method in embodiment 1, avilamycin etoxazole microcapsule suspension-suspendinagent agent, difference are prepared
It is that BPO/MMA solution in the first solution replaces with melamine-formaldehyde resin solution.
The preparation method of the carbamide numerical value solution is included first that tripolycyanamide and concentration are 37 weight %
Aldehyde aqueous solution is uniform, is 8 in pH value, and temperature is to react 1.5h under the conditions of 70 DEG C;Add water dilution, obtain tripolycyanamide-
Formaldehyde resin performed polymer aqueous solution, wherein, formaldehyde is 1 with the mol ratio of tripolycyanamide:0.5, the volume of water and formalin
Than for 1:1.5.
Testing example 1
The measure of Microcapsules Size:The particle diameter of avermectin microcapsule suspending agent is determined using laser particle size analyzer.
The measure of microencapsulated rate:It is micro- with the avilamycin in comparative example using each embodiment of high-performance liquid chromatogram determination
The content of the avilamycin dissociated in capsule suspension, and its envelop rate is calculated, formula (1) is shown in the calculating of envelop rate.
Heat storage stability is determined:By the avilamycin etoxazole microcapsule suspension-suspendinagent agent in each embodiment and comparative example
During the constant temperature oven of (54 ± 2) DEG C in being fitted into container, is positioned over after sealing, take out after standing 14 days, according to GB/T14825-
2006 standards, determine the suspensibility of micro-capsule suspension.
Low-temperature stability is determined:The avilamycin etoxazole microcapsule obtained in embodiment 1-5 and comparative example 1-11 is hanged
Floating-suspending agent is fitted in container, during (0 ± 2) DEG C refrigerator is placed in after sealing, keeps 1h, stirs once at interval of 15min, often
Secondary 15s, observation outward appearance has unchanged, continues to place 7 days in (0 ± 2) DEG C, then takes out to be placed in be stood under room temperature condition and recovers
Afterwards, according to the suspensibility of GB/T14825-2006 standard test suspending agents.Envelop rate, particle diameter, shed storage test result are shown in
Table 1.
Table 1
As it can be seen from table 1 the avilamycin second demodicid mite that the preparation method provided according to the present invention in embodiment 1-5 is obtained
The avilamycin etoxazole microcapsule suspension-suspendinagent agent particle diameter that azole microcapsule suspension-suspending agent is prepared relative to additive method
Less, envelop rate is higher, and with good thermal storage stability and low tempertaure storage stability.The present invention utilizes emulsion polymerization
Method, with methyl methacrylate as monomer, under the conditions of the specific stepwise reaction such as catalyst, stir speed (S.S.), prepares
Avilamycin etoxazole microcapsule suspension-suspendinagent agent is preferable.
Testing example 2
This testing example is micro- for the avilamycin etoxazole that measure will be obtained in embodiment 1-5 and comparative example 1-11
Prevention effect of the capsule suspension-suspending agent to red spider on Fructus Mali pumilae.Before test by embodiment 1-5 and comparative example 1-11 obtained Ah
It is standby that dimension rhzomorph etoxazole microcapsule suspension-suspendinagent agent is diluted to 2000-3000 times of liquid.
Test site:Hebei Gaobeidian city Xin Li village Zhen Lijia village village, is Red Star for trying apple variety, and the age of tree is 10-
12 years, there is heavier, experimental plot middle fertility in red spider.
Concrete steps include, are 30kg/ mus according to formulation rate, by embodiment 1-5 and comparative example using knapsack sprayer
The avilamycin etoxazole microcapsule suspension-suspendinagent agent medicinal liquid prepared in 1-11 is carried out respectively to the Fructus Mali pumilae of each growing area
Spraying, blank control group is sprayed using equivalent clear water to the apple tree in growing area.The Fructus Mali pumilae of each treatment region after dispenser
The routinely production management in addition to insecticide.
After dispenser 1 day, 10 days, 30 days and 50 days investigation European red mite prevention effect, concrete test method according to《Agriculture
Medicine field control effectiveness test criterion》Carry out.Using random 5 points samplings, each processes cell and investigates 10 branches each treatment region, adjusts
Each treatment region European red mite prevention effect is looked into, mortality rate and preventive effect are calculated respectively according to formula (2) with method shown in formula (3), tool
Body the results are shown in Table 2:
Table 2
Testing example 3
This testing example be used for test obtained avilamycin etoxazole microcapsule suspension in each embodiment and comparative example-
Prevention effect of the suspending agent to Tetranychus urticae on Fructus Cucumidis sativi.By obtained avilamycin second in each embodiment and comparative example before test
It is standby that demodicid mite azole microcapsule suspension-suspending agent is diluted to 2000-3000 times of liquid.
Test site:Hebei province Baoding virtuous of area country worthy's platform village warmhouse booth all over the city.The booth hydroelectric facility is complete, soil
Earth fertility is higher, the routinely production management in addition to acaricide of each treatment region Fructus Cucumidis sativi after dispenser.
Concrete steps include, are 30kg/ mus according to spouting liquid, by embodiment 1-5 and comparative example using knapsack sprayer
The avilamycin etoxazole microcapsule suspension-suspendinagent agent medicinal liquid obtained in 1-11 uniformly sprays respectively the Fructus Cucumidis sativi in each growing area
On plant, blank control group is sprayed using equivalent clear water to the cucumber plant in growing area, during dispenser, is hidden with plastic sheeting
Gear neighbor cell, prevents medicament from interfering.
After dispenser 1 day, 10 days, 30 days and 50 days investigation Tetranychus urticae prevention effect, concrete test method according to《Agriculture
Medicine field control effectiveness test criterion》Carry out.Using random 5 points samplings, each processes cell and investigates 25 plants of Fructus Cucumidiss sativi plants each treatment region
Strain, prevention effect represents that mortality rate, the computational methods of preventive effect are with reference to testing example 2 with the mortality rate of Tetranychus urticae.Specifically
The results are shown in Table 3:
Table 3
In table 2 and table 3, Jing embodiments 1-5 can be seen that the present invention compared with comparative example 1-11 and utilize emulsion polymerization,
With methyl methacrylate as monomer, under the conditions of the specific stepwise reaction such as catalyst, stir speed (S.S.), the AVM hereinafter for preparing
Rhzomorph etoxazole microcapsule suspension-suspendinagent agent, is not susceptible to reunite and coacervation, is capable of the preventing and treating crops evil of slow release long-acting
Worm, and with good quick-acting, dosage and times for spraying can be reduced, so as to dirt cost-effective and that reduction is to environment
Dye.
The avilamycin etoxazole microcapsule suspension-suspendinagent agent of the present invention is relative to the outstanding of other avilamycin etoxazoles
Floating agent, with the lasting period it is long the characteristics of, it is cost-effective so as to times for spraying and dosage can be reduced;What is wherein contained is organic molten
Agent is few, can reduce the pollution to environment.
The preferred implementation of the disclosure described in detail above, but, the disclosure is not limited in above-mentioned embodiment
Detail, in the range of the technology design of the disclosure, various simple variants can be carried out with technical scheme of this disclosure, this
A little simple variants belong to the protection domain of the disclosure.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means.In order to avoid unnecessary repetition, the disclosure to it is various can
The compound mode of energy is no longer separately illustrated.
Additionally, combination in any can also be carried out between a variety of embodiments of the disclosure, as long as it is without prejudice to this
Disclosed thought, it should equally be considered as disclosure disclosure of that.
Claims (10)
1. a kind of preparation method containing avilamycin and the microcapsule suspension-suspendinagent agent of etoxazole, it is characterised in that the preparation method
Comprise the steps:
(1) by the first solution and the second solution mix homogeneously, first material is obtained;Wherein described first solution contains benzoyl peroxide
Formyl and methyl methacrylate;Second solution contains abamectin emulsifiable concentrate;First solution and second solution
Weight ratio be 1:(50-200);
(2) first material is mixed homogeneously with water, stirring and emulsifying obtains second material;The weight of the first material and water
Than for 1:(0.5-5);
(3) NaHSO is added in the second material3Solution, obtains 3 material after mix homogeneously;Mistake in the second material
BP and NaHSO3NaHSO in solution3Weight ratio be 1:(1-3);
(4) 3 material is carried out into solidification bunching, obtains solidifying bunching product;PH is added in the solidification bunching product
It is 6-8 that regulator makes the pH value of the solidification bunching product, obtains 4 materials;
(5) dispersant is added in the 4 materials, obtains the 5th material;The weight of the 4 materials and the dispersant
Than for 1:(0.01-0.1);
(6) the 5th material is mixed homogeneously with etoxazole suspending agent, obtain the microcapsule suspension containing avilamycin and etoxazole-
Suspending agent;5th material is 1 with the weight ratio of etoxazole suspending agent:(0.5-20).
2. preparation method according to claim 1, it is characterised in that in step (1), the abamectin emulsifiable concentrate contain Ah
Dimension rhzomorph, organic solvent and emulsifying agent;The organic solvent includes 200# solvent naphthas, N-Methyl pyrrolidone, petroleum ether, acetic acid
At least one in ethyl ester, toluene, N,N-dimethylformamide, chloroform, isopropanol, dimethylbenzene and solvent naphtha;The breast
Agent includes sodium lignin sulfonate, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, styrene-maleic anhydride copolymer, fat
Fat polyoxyethylenated alcohol, anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate polyoxyethylene ether, the moon
At least one in lauryl sulfate, polyvinyl alcohol, polycarboxylate and naphthalene sulfonate;Wherein, avilamycin is organic molten with described
Agent, the mass ratio of the emulsifying agent are 1:(5-20):(1-4).
3. preparation method according to claim 1, it is characterised in that in step (1), benzoyl peroxide in first solution
The weight ratio of formyl and methyl methacrylate is 1:(200-1000).
4. preparation method according to claim 1, it is characterised in that in step (3), the NaHSO3NaHSO in solution3
Concentration be 0.01-0.1 weight %.
5. preparation method according to claim 1, it is characterised in that in step (4), the pH adjusting agent include hydrochloric acid,
At least one in sulphuric acid, phosphoric acid, acetic acid, ammonium chloride and sodium hydroxide, sodium carbonate, potassium carbonate, potassium citrate, sodium citrate;
The concentration of the pH adjusting agent is 0.5-8 weight %.
6. preparation method according to claim 1, it is characterised in that in step (5), the dispersant includes dodecyl
It is benzene sulfonate, di-2-ethylhexylphosphine oxide naphthalene sulfonate, 1- methyl naphthalene sulfonate formaldehyde condensates, benzyl naphthalene sulfonic acid-formaldehyde condensation product, wooden
Plain sulfonate, desaccharide lignosulfonates, desaccharide condensation lignosulfonates, succinate sulfonate, pull open powder, phosphate ester
At least one in class, polycarboxylic acid salt and fatty alcohol-polyoxyethylene ether;Preferably, thickening agent is also contained in the 5th material
And/or antifreezing agent;The thickening agent includes Magnesiumaluminumsilicate, xanthan gum, Polyethylene Glycol, polyvinyl alcohol, carboxymethyl cellulose, swelling
At least one in soil, active hargil and white carbon;The antifreezing agent includes ethylene glycol, 1,2- Propylene Glycol, glycerol and carbamide
In at least one;The 4 materials, the dispersant, the thickening agent, the weight ratio of the antifreezing agent are 1:(0.01-
0.1):(0.001-0.02):(0.02-0.15).
7. preparation method according to claim 1, it is characterised in that in step (6), the etoxazole suspending agent contains grain
Etoxazole microgranule, water and adjuvant that footpath is less than 5 μm;The weight ratio of the etoxazole microgranule, adjuvant and water is 1:(1-20):
(0.5-50);Preferably, the adjuvant includes at least in dispersant, defoamer, thickening agent, antifreezing agent and preservative
Kind;The weight of the etoxazole microgranule, the dispersant, the defoamer, the thickening agent, the antifreezing agent and the preservative
Amount is than being 1:(2-15):(2-15):(0.005-0.1):(2-15):(2-15).
8. preparation method according to claim 1, it is characterised in that in step (6), it is described containing avilamycin and etoxazole
Microcapsule suspension-suspendinagent agent in also contain dispersant;The avermectin microcapsule suspending agent, etoxazole suspending agent and dispersant
Weight ratio is 1:(0.1-10):(0.01-2).
9. preparation method according to claim 1, it is characterised in that in step (2), described stirring and emulsifying condition bag
Include:3-10min is stirred under 50-200 rev/min of stir speed (S.S.);
In step (3), described mixing condition condition includes:Under 100-300 rev/min of stir speed (S.S.), with every 4-5 point
The speed addition NaHSO of the drop of clock Deca 13Solution, and the time of Deca stirring is 10-90min;
In step (4), described solidification bunching condition includes:Be polymerized 1-8h under the conditions of 10-40 DEG C.
10. a kind of microcapsule suspension-suspendinagent agent containing avilamycin and etoxazole, it is characterised in that the suspending agent is according to right
Require what the preparation method in 1-9 described in any one was obtained.
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CN115414865A (en) * | 2022-09-27 | 2022-12-02 | 溢通环保科技(莆田)有限公司 | Anti-settling polymerization inhibitor for diesel oil tail gas treatment fluid and production process thereof |
CN115414865B (en) * | 2022-09-27 | 2023-09-19 | 溢通环保科技(莆田)有限公司 | Anti-settling polymerization inhibitor for diesel exhaust treatment fluid and production process thereof |
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