CN106577722A - Dinotefuran suspending agent and preparation method thereof - Google Patents
Dinotefuran suspending agent and preparation method thereof Download PDFInfo
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- CN106577722A CN106577722A CN201510660213.1A CN201510660213A CN106577722A CN 106577722 A CN106577722 A CN 106577722A CN 201510660213 A CN201510660213 A CN 201510660213A CN 106577722 A CN106577722 A CN 106577722A
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Abstract
The invention discloses a dinotefuran suspending agent. The suspending agent comprises, by mass, 1-25 parts of dinotefuran, 2-15 parts of a dispersant and a wetting agent, 2-5 parts of an emulsifier, 10-20 parts of a stabilizer, 0.1-2 parts of a thickener, 0.1-2 parts of an antifoaming agent, 0.005-2 parts of an antiseptic, 0.1-1 part of an antifreeze agent, 0.1-1 part of a pH regulator, and the balance of water, wherein the mass part sum of all above raw materials is 100. The invention also discloses a preparation method of the dinotefuran suspending agent. The average 95% particle size of dinotefuran is less than 5 [mu]m, and the suspending agent has the advantages of uniform particle size distribution, good stability, high spreadability and stickiness on crop leaf surfaces and good rain wash resistance; the suspending rate reaches 96% or above, and the suspending rate has good fluidity, does not stick bottle walls, has good hot/cold storage stability, and is easy to pour.
Description
Technical field
The present invention relates to formulations of pesticide manufacture field, is related to the formulations of pesticide containing MTI-446, and in particular to a kind of agricultural chemicals suspension agent containing MTI-446 and preparation method thereof.
Background technology
21st century, the use of pesticide are still one of Main Means that the mankind struggle with disease pest and weed in agricultural production.With a large amount of uses of pesticide, substantial amounts of organic solvent causes pollution to environment, with the continuous enhancing of people's environmental consciousness and security knowledge, direction of the formulations of pesticide towards water baseization, spheroidizing, slow-releasing, multi-functional, Labor-saving and environment-friendly type is developed, and particularly the dosage form of suspended emulsion is increasingly by favour and the attention of people.Agricultural chemicals suspension agent (SC) is a kind of environment amenable environment-protection pesticide dosage form with water as medium, is the higher suspension shape system disperseed homogenizing in aqueous medium and formed by a kind of water-fast solid-state active compound and a kind of oily liquids active compound and various auxiliary agents.Suspending agent is a three-phase mixture, and discontinuous phase is scattered in water phase, i.e. oil/water row Emulsion and is thoroughly dispersed in the solid phase of water phase.There is suspending agent, emulsifiable concentrates for agricultural chemicals and wettable powder pollution and murder by poisoning because of organic solvent and dust to environment and operator is such as avoided, storing safety, with higher biological activity etc., is shown one's talent in water-based aerosol.
The physicochemical property of MTI-446:Appearance white powder, without special odor, molecular formula C7H14N4O3
Structural formula is:
Relative molecular mass:202.21 (based on calendar year 2001 world relative atomic masses)
Biological activity:Parasite killing
Fusing point (DEG C):107.5
Dissolubility (g/L, room temperature):Water 40, is insoluble in the organic solvents such as hexamethylene, dimethylbenzene.
Density:1.425g/cm3
Stability:It is chronically exposed to perishable under sky air and heat and wet environment
MTI-446 have tag, stomach toxicity and root absorbability is strong, quick-acting high, lasting period long 3-4 are all(Theoretical lasting effect 43 days), the features such as insecticidal spectrum is wide, and have excellent preventive effect to sucking insect, and show very high insecticidal activity in very low dosage.It is mainly used in preventing and treating aphid in Semen Tritici aestivi, Oryza sativa L., Cotton Gossypii, vegetable, fruit tree, the various crop such as Nicotiana tabacum L., leafhopper, plant hopper, thrips, aleyrodid and its resistant strain, simultaneously coleoptera, Diptera and Lepidoptera, Diptera, beetle mesh and total wing mesh insect are had efficiently, and the sanitary insect pests such as cockroach, Coptotermes formosanus Shtrari., housefly are had efficiently.Which, was registered in the countries in Asia with Korea as representative, this country and European Countries in Japan's introduction later in 1993.
Suspending agent is the higher suspension shape system disperseed homogenizing in aqueous medium and formed by a kind of various auxiliary agents of water-fast solid-state active compound.The dispersion effect of the suspension emulsion of foreign study exploitation is substantially better than the country, but price is high, and the country technically needs to be broken through.
The main Hefei Xingyu Chemical Co., Ltd at home of the domestic research with regard to MTI-446 at present has made with regard to a kind of guadipyr and dinotefuran and its preparation and applied research, and has applied for patent, and number of patent application is 201210499882;A kind of imidaclothiz and MTI-446 compounded pesticides, number of patent application 201310166119 are reported in patent;Report that the dinotefuran insecticide of compounding has good potentiation in this two parts of patents.
It is an advantage of the current invention that:MTI-446 is prepared into environment-friendly pesticide novel form suspending agent as efficient pesticides of new generation(SC), reduce the organic solvent used by traditional cream preparation, it is possible to reduce environmental pollution, reduce the toxicity to operator.
The technical problem to be solved in the present invention is to provide the MTI-446 suspending agent that a kind of stable in properties, crystal is not grown up, the invention solves the problems that another technical problem be to provide the preparation method of MTI-446 suspending agent.The present invention has screened a kind phosphate ester class dispersant, improves adhesive force of the effective ingredient MTI-446 to Target crops, while preparing stable suspension system.The even particle size distribution of the MTI-446 suspending agent of the present invention, between 3-5um, suspending agent has good stability mean diameter, and suspensibility all reaches more than 96%, medicine show on crop blade face it is high open up and cohesiveness, anti-rain drop erosion;Good fluidity, hot/cold storage have good stability, and after heat storage, suspensibility is more than 95%;Easily topple over, do not stick bottle wall, room temperature topples over rear residue<0.8%, residue is toppled in heat storage<1.0%.And obtained MTI-446 suspending agent keeps stable in production and product storage period and does not separate out crystal.
The present invention innovative point be:
1st, with the suspension emulsion that new dispersant and active compound combination forming properties are more prominent.Flash-point is high, and suspensibility is high, reaches more than 96% suspensibility, and nonflammable explosive, environmentally friendly, product stability is good, and crystal is not separated out during storing.
2nd, phosphate ester surfactant has protective effect to MTI-446, and obtained suspending agent is good to the selectivity of crop target, and killing rate is high.3rd, the polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant is hydrophilic high polymers, there is between polymer and plant leaf surface certain cementation, so that the anti-rain drop erosion of pesticide, while extend the time of staying of the effective ingredient MTI-446 on crop, so as to notable potentiation.
4th, the polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant is water miscible, so good penetrability, product cost is low, and easy to package, the market competitiveness is strong.
5th, it is inclusion property colloidal suspending agent that the phosphate terpolymer is formed, so pesticide animal migration in soil is little, subsoil water is not polluted, production and application safety, without dust, environmentally friendly.
6th, application of the invention will bring good economic benefit to enterprise.
The content of the invention
It is an object of the invention to provide the preparation method of a kind of MTI-446 suspending agent do not grown up of stable in properties, crystal and this suspending agent.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of suspending agent containing MTI-446, the suspending agent include:
MTI-446,1~25 part;Dispersant, wetting agent, 2~15 parts;Emulsifying agent, 2 ~ 5 parts;Stabilizer, 1~40 part;Thickening agent, 0.1~2 part;Defoamer, 0.1~2 part;Preservative, 0.005 ~ 2 part;Antifreezing agent, 0.1~1 part;PH regulators, 0.1 ~ 1 part;Water, complements to 100 parts.
The dispersant of described MTI-446 suspending agent is selected from a kind of polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant, and this dispersant comes from patent《One class new type of phosphate dipersant and its synthesis technique》, the patent No. 2014100824497.
Described phosphoric acid ester dispersant, it is characterised in that the monomer ratio of the polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant is as follows:
(a)Certain herbaceous plants with big flowers base polyoxyethylene ether
Alkylpolyoxyethylene
1-3 parts
Myristyl polyoxyethylene ether
1-3 parts
Ceteth
1-3 parts
Steareth
1-3 parts
NPE
1-3 parts
OPEO
1-3 parts
Dodecyl phenol polyethenoxy ether
1-3 parts
Tristyrylphenyl polyoxyethylene ether
1-3 parts
(b)Epoxychloropropane
2-20 parts
(c)Tetrabutyl ammonium bromide
0.01-0.1 parts
(d)Sodium hydroxide
5-10 parts
(e)Phosphoric acid
6-20 parts
(f)Triethanolamine
6-20 parts
(g)Ether
100-300 parts
(f)Ethanol
100-300 parts
Polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant preparation technology, comprises the following steps that:(1)Material a described in claim 3 is measured into portion, is placed in constant pressure funnel.
(2)2 parts of epoxychloropropane is taken in there-necked flask, 2 parts of sodium hydrate solids instill 5ml water, 0.2 part of tetrabutyl ammonium bromide, stirring at normal temperature 10 minutes in there-necked flask.
(3)Material in constant pressure funnel is added drop-wise in there-necked flask, about half an hour adds.
(4)After normal-temperature reaction about three hours, 100 parts of dichloromethane washings are taken, is filtered, is collected filtrate, reduce pressure steaming vibrating dichloromethane at normal temperatures, is warmed up to 85 DEG C, boils off unreacted epoxychloropropane, collects in constant pressure funnel after having steamed.
(5)3 parts of phosphoric acid are taken in there-necked flask, with 100 parts of ether dissolutions.Material in constant pressure funnel is added dropwise in there-necked flask, is reacted 5 hours at 45 DEG C.Boil off ether.
(6)Gained material is dissolved in the middle of the beaker of 100 parts of ethanol, three parts of triethanolamine is taken and is added dropwise in beaker, have solid matter to separate out, after sucking filtration, collected filtrate, boil off methanol, that is, obtain the destination scatter agent.
One or more kinds of combinations of the described emulsifying agent in NP series NPEs, AEO series fatty alcohol-polyoxyethylene ether, macromolecule EO-PO block copolymers, alkylphenol polyoxyethylene and its sulfate, alkylphenol polyoxyethylene phosphate ester salt, styryl phenol polyethenoxy polyethenoxy ether.
Described thickening agent is selected from sodium carboxymethyl cellulose, aluminium-magnesium silicate, hydroxymethyl cellulose, hydroxyethyl cellulose, methylcellulose or polyvinyl alcohol, one or more in xanthan gum XG, WJ2-04.
Described defoamer is selected from silicone oil, silicone compound, Cl0-20 saturated fat acids compounds, wherein C8-10 aliphatic alcohols compounds, silicone compound such as organosilicon etc., C10-20 saturated fat acid compounds such as hendecanoic acid, tridecanoic acid, pentadecanoic acid etc., one or more in C8-10 aliphatic alcohols compound such as certain herbaceous plants with big flowers alcohol, ten alkanols.
Described antifreezing agent is selected from one or more in ethylene glycol, glycerol, Propylene Glycol, Polyethylene Glycol, Sorbitol or urea.
Described pH adjusting agent is selected from one or more in triethylamine, sodium hydroxide, ammonia, acetic acid, citric acid or phosphoric acid.
The consumption of described pH adjusting agent be make suspending agent pH value be 5~9.
Described stabilizer is selected from one or more in catechol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, polyethylene glycol diglycidyl ether, epichlorohydrin, sodium sorbate, sodium benzoate, epoxidised soybean oil, oleum lini, hydroquinone, anthraquinone, eugenol, citric acid, hydroxy benzoate or propyl parabene.
Present invention also offers above-mentioned preparation method the method containing MTI-446 suspending agent is comprised the following steps:
(1)By water in wetting dispersing agent, stabilizer, defoamer mix homogeneously, after input MTI-446 active compound is uniformly dispersed, serialization sand milling is carried out by sand mill, the suspension of MTI-446 is obtained;
(2)Emulsifying agent is dissolved in antifreezing agent, oil phase after mix homogeneously, is obtained.Emulsifying agent and water are mixed and made into into water phase, the oil phase for having configured is poured into water phase and high speed homogenization mulser is opened, form stable O/W emulsions;
(3)Step is added in the MTI-446 suspension for having configured(2)The emulsion for obtaining, mix homogeneously obtain MTI-446 suspending agent;
Preferably, the sand milling temperature is 0-30 DEG C;The particle diameter of the MTI-446 after the sand milling is 1-5um.
Further, the step(3)In can be with thickening agent 0.005-2 part weight portions, preservative 0.005-2 weight portions.
Specific embodiment
Embodiment 1
5% MTI-446 suspending agent
Each component content(By weight)For MTI-446 active compound 5%, polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant 5%;Macromolecule Pluronic PE 6800 emulsifying agent 6%, thickening agent xanthan gum XG2%, stabilizer phenyl glycidyl ether 10%, defoamer organosilicon 6%, antifreeze glycol 4%, it is 8 that pH adjusting agent makes suspending agent pH value in right amount.Plus deionized water is to l00%.
The first step:By above-mentioned formula by water in wetting dispersing agent, stabilizer, defoamer mix homogeneously, after input MTI-446 active compound is uniformly dispersed, continuous sand milling temperature control is carried out below 40 degree, after mean diameter reaches 5um ± 3um by sand mill, stop sand milling, obtain the suspension of MTI-446;
Second step:Emulsifying agent is dissolved in antifreezing agent, oil phase after mix homogeneously, is obtained.Emulsifying agent and water are mixed and made into into water phase, the oil phase for having configured is poured into water phase and high speed homogenization mulser is opened, form stable O/W emulsions;
3rd step:In the MTI-446 suspension for having configured, add second emulsion for obtaining, mix homogeneously to obtain MTI-446 suspending agent SC;
4th step:Open stirring(200r/min), thickening agent is subsequently adding, preservative stirs, and obtains final product MTI-446 suspending agent SC.
The key technical indexes is as follows:
Outward appearance:White uniformity liquid;Mean diameter, 3.55;Stability of emulsion is qualified;
Suspensibility is 97.40%, favorable dispersibility.
2 10% MTI-446 suspending agent of embodiment
Each component MTI-446 active compound 10% by weight, dispersant polyoxyethylene ether glycidyl ether phosphoric acid salt 10%;Macromolecule Pluronic PE 6800 emulsifying agent 6%, thickening agent hydroxymethyl cellulose 3%, stabilizer butyl glycidyl ether 2.5%, defoamer tridecanoic acid 1%, antifreezing agent glycerol 3%, pH adjusting agent make suspending agent pH value in right amount for 7, plus deionized water is to 100%.Concrete preparation is carried out by embodiment 1.
Outward appearance:White uniformity liquid;Mean diameter, 2.35um;Stability of emulsion is qualified;
Suspending agent suspensibility obtained in the formula is 97.80%, favorable dispersibility.
3 15% MTI-446 suspending agent of embodiment
Each component MTI-446 active compound 15% by weight, dispersant polyoxyethylene ether glycidyl ether phosphoric acid salt 15%;6% thickening agent methylcellulose 3% of macromolecule Pluronic PE 6800 emulsifying agent, stabilizer phenyl glycidyl ether 2.5%, defoamer Cl0-20 saturated fat acids compound 1%, antifreezing agent glycerol 3%, pH adjusting agent makes suspending agent pH value in right amount for 7, plus deionized water is to 100%.Concrete preparation is carried out by embodiment 1.
Outward appearance:White uniformity liquid;Mean diameter, 3.52um;Stability of emulsion is qualified;
Suspensibility is 97.50%, favorable dispersibility.
4 20% MTI-446 suspending agent of embodiment
Each component content(By weight)For MTI-446 active compound 20%, dispersant polyoxyethylene ether glycidyl ether phosphoric acid salt 12%, stabilizer Catechol 2 %;Macromolecule Pluronic PE 6800 emulsifying agent 8%;Thickening agent aluminium-magnesium silicate 3%, stabilizer catechol 5%, defoamer silicone oil 1%, antifreeze glycol 1%, pH adjusting agent make suspending agent pH value in right amount for 6, plus deionized water is to l00%.Concrete preparation is carried out by embodiment 1.
Outward appearance:White uniformity liquid;Mean diameter, 3.68um;Stability of emulsion is qualified;
Suspensibility is 98.40%, favorable dispersibility,.
5 25% MTI-446 suspending agent of embodiment
Each component content(By weight)For MTI-446 active compound 25%, dispersant polyoxyethylene ether glycidyl ether phosphoric acid salt 15%, stabilizer are selected from catechol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether;Macromolecule Pluronic PE 6800 emulsifying agent 8%, thickening agent xanthan gum WJ2-04 4%, stabilizer polyethylene glycol diglycidyl ether 5%, defoamer certain herbaceous plants with big flowers alcohol 2%, antifreeze glycol 1%, pH adjusting agent make suspending agent pH value in right amount for 6, plus deionized water is to l00%.Be mixed ball milling 2~3 hours in ball mill, make particle diameter all in below 3um.Concrete preparation is carried out by embodiment 1.
Outward appearance:White uniformity liquid;Mean diameter, 3.54um;Stability of emulsion is qualified;
98.60%, favorable dispersibility.
Claims (7)
1. a kind of suspending agent containing MTI-446, it is characterised in that:The suspending agent includes:
MTI-446
1~25 part
Dispersant, wetting agent
2~15 parts
Emulsifying agent
2 ~ 10 parts
Stabilizer
10~20 parts
Thickening agent
0.1~2 part
Defoamer
0.1~2 part
Preservative
0.005 ~ 2 part
Antifreezing agent
0.1~10 part
PH regulators
0.1 ~ 1 part
Water
Complement to 100 parts.
2. the dispersant of MTI-446 suspending agent according to claim 1 is selected from a kind of polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant, and this dispersant comes from patent《One class new type of phosphate dipersant and its synthesis technique》, the patent No. 2014100824497.
3. dispersant according to claim 2, it is characterised in that the monomer ratio of the polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant is as follows:
(a)Certain herbaceous plants with big flowers base polyoxyethylene ether
Alkylpolyoxyethylene
1-3 parts
Myristyl polyoxyethylene ether
1-3 parts
Ceteth
1-3 parts
Steareth
1-3 parts
NPE
1-3 parts
OPEO
1-3 parts
Dodecyl phenol polyethenoxy ether
1-3 parts
Tristyrylphenyl polyoxyethylene ether
1-3 parts
(b)Epoxychloropropane
2-20 parts
(c)Tetrabutyl ammonium bromide
0.01-0.1 parts
(d)Sodium hydroxide
5-10 parts
(e)Phosphoric acid
6-20 parts
(f)Triethanolamine
6-20 parts
(g)Ether
100-300 parts
(f)Ethanol
100-300 parts
Polyoxyethylene ether glycidyl ether phosphoric acid salt dispersant preparation technology, comprises the following steps that:
(1)Material a described in claim 3 is measured into portion, is placed in constant pressure funnel;
(2)2 parts of epoxychloropropane is taken in there-necked flask, 2 parts of sodium hydrate solids instill 5ml water, 0.2 part of tetrabutyl ammonium bromide, stirring at normal temperature 10 minutes in there-necked flask;
(3)Material in constant pressure funnel is added drop-wise in there-necked flask, about half an hour adds;
(4)After normal-temperature reaction about three hours, 100 parts of dichloromethane washings are taken, is filtered, is collected filtrate, reduce pressure steaming vibrating dichloromethane at normal temperatures, is warmed up to 85 DEG C, boils off unreacted epoxychloropropane, collects in constant pressure funnel after having steamed;
(5)3 parts of phosphoric acid are taken in there-necked flask, with 100 parts of ether dissolutions, the material in constant pressure funnel is added dropwise in there-necked flask, reacted 5 hours at 45 DEG C, boil off ether;
(6)Gained material is dissolved in the middle of the beaker of 100 parts of ethanol, three parts of triethanolamine is taken and is added dropwise in beaker, have solid matter to separate out, after sucking filtration, collected filtrate, boil off methanol, that is, obtain destination scatter agent described in claim 2.
4. one or more kinds of combinations of the emulsifying agent according to claim 1 in NP series NPEs, AEO series fatty alcohol-polyoxyethylene ether, macromolecule EO-PO block copolymers, alkylphenol polyoxyethylene and its sulfate, alkylphenol polyoxyethylene phosphate ester salt, styryl phenol polyethenoxy polyoxypropylene propylene ether.
5. the preparation method of MTI-446 suspending agent is contained according to claim 1-10, it is characterised in that:The method is comprised the following steps:
(1)By water in wetting dispersing agent, stabilizer, defoamer mix homogeneously, after input MTI-446 active compound is uniformly dispersed, serialization sand milling is carried out by sand mill, the suspension of MTI-446 is obtained;
(2)Emulsifying agent is dissolved in antifreezing agent, oil phase after mix homogeneously, is obtained, emulsifying agent and water are mixed and made into into water phase, the oil phase for having configured is poured into water phase and high speed homogenization mulser is opened, form stable O/W emulsions;
(3)Step is added in the MTI-446 suspension for having configured(2)The emulsion for obtaining, mix homogeneously obtain MTI-446 suspending agent.
6. the preparation method of MTI-446 according to claim 11, it is characterised in that:The sand milling temperature is 0-30 DEG C;The particle diameter of the MTI-446 after the sand milling is 1-5um.
7. the preparation method containing MTI-446 according to claim 12, it is characterised in that:The step(3)In can also add 0.1 ~ 10 weight portion of antifreezing agent, thickening agent 0.005-2 part weight portions, preservative 0.005-2 weight portions.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106577686A (en) * | 2015-10-14 | 2017-04-26 | 上海师范大学 | Pymetrozine suspension and preparation method thereof |
CN107593695A (en) * | 2017-06-25 | 2018-01-19 | 广东中迅农科股份有限公司 | A kind of application technology of stabilizer in suspending agent |
CN109221225A (en) * | 2018-09-28 | 2019-01-18 | 绩溪农华生物科技有限公司 | A kind of dinotefuran synergy suspending agent and preparation method thereof |
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CN102239829A (en) * | 2011-07-13 | 2011-11-16 | 南京扬子鸿利源化学品有限责任公司 | Dinotefuran aqueous suspension agent and its preparation method |
CN103120157A (en) * | 2013-01-24 | 2013-05-29 | 清远市顾地丰生物科技有限公司 | Insecticidal suspending agent containing dinotefuran and preparation method of insecticidal suspending agent |
CN106577686A (en) * | 2015-10-14 | 2017-04-26 | 上海师范大学 | Pymetrozine suspension and preparation method thereof |
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US4510070A (en) * | 1982-03-29 | 1985-04-09 | Kao Corporation | Emulsifying composition |
CN102239829A (en) * | 2011-07-13 | 2011-11-16 | 南京扬子鸿利源化学品有限责任公司 | Dinotefuran aqueous suspension agent and its preparation method |
CN103120157A (en) * | 2013-01-24 | 2013-05-29 | 清远市顾地丰生物科技有限公司 | Insecticidal suspending agent containing dinotefuran and preparation method of insecticidal suspending agent |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106577686A (en) * | 2015-10-14 | 2017-04-26 | 上海师范大学 | Pymetrozine suspension and preparation method thereof |
CN107593695A (en) * | 2017-06-25 | 2018-01-19 | 广东中迅农科股份有限公司 | A kind of application technology of stabilizer in suspending agent |
CN109221225A (en) * | 2018-09-28 | 2019-01-18 | 绩溪农华生物科技有限公司 | A kind of dinotefuran synergy suspending agent and preparation method thereof |
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Application publication date: 20170426 |