CN102187871A - Thiacloprid microcapsule preparation and preparation method thereof - Google Patents
Thiacloprid microcapsule preparation and preparation method thereof Download PDFInfo
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Abstract
The invention provides a thiacloprid microcapsule preparation, which comprises the following components in part by weight: 0.1 to 5 parts of thiacloprid, 5 to 50 parts of solvent, 1 to 10 parts of urea formaldehyde resin, 2 to 10 parts of emulsifier, 3 to 10 parts of antifreeze agent, 0.05 to 0.3 part of viscosity regulator, 2 to 5 parts of dispersing agent, 0.1 to 100 parts of pH regulator and 0.1 to 100 parts of water. The preparation method comprises the following steps of: preparing a urea formaldehyde resin prepolymer from methyl aldehyde and urea by an in-situ polymerization method, dissolving the thiacloprid in the solvent, adding aqueous solution of a urea-methyl aldehyde resin prepolymer into thiacloprid solution with stirring at high speed, stirring and dispersing fully to form superfine particles, performing a reaction, curing, regulating the pH value, and adding the dispersing agent, the viscosity regulator and the antifreeze agent to obtain the thiacloprid microcapsule preparation. The medicine effect of the thiacloprid microcapsule preparation can last for a long time, the administration times can be reduced, the cost is reduced, and environmental pollution is relieved.
Description
Technical field
The present invention relates to a kind of pesticide micro capsule agent and preparation method thereof, be specifically related to a kind of thiophene worm quinoline microcapsule formulations and preparation method thereof.
Background technology
Thiophene worm quinoline (Thiacloprid)
Chemical name: 3-(6-chloro-3-picolyl)-1,3-thiazoles quinoline-2-base fork cyanamide.
Physicochemical property: former medicine is a light yellow crystalline powder, 136 ℃ of fusing points, relative density (20 ℃) 1.46, vapour pressure 23 * 10-12hPa (20 ℃), 8 * 10-12hPa (25 ℃), distribution coefficient (n-octyl alcohol/water, 20 ℃) is 18.0, solvability in the water (20 ℃) 185ug/L.In the time of 50 ℃, can stablize and store for 2 weeks.
Thiophene worm quinoline is novel chloro nicotinic insecticide.The mechanism of action and other conventional pesticides of thiophene worm quinoline are different.It mainly acts on the neural caudacoria that engages of insect, by combine interference insect nervous system normal conduction with nAChR, cause the obstruction of neural channel, cause a large amount of accumulation of acetylcholine, thereby make the insect exaltation, whole body spasm, paralysis and dead.Having stronger interior suction, tag and stomach poison function, do not have cross resistance with common insecticides such as pyrethroid, organic phosphates and carbamates, thereby can be used for resistance management, is one of efficient medicament of control pierce-suck type and pests with chewing mouthparts.Thiophene worm quinoline has good control efficiency to insects such as coleoptera, Lepidoptera, orthopteras.Japan promotes the use of thiophene worm quinoline control Monochamus alternatus Hope and has obtained very good control efficiency, makes pine nematode obtain effective control.
Control release technic is one of important development direction of pesticidal preparations and operation technique, also is present international state-of-the-art technique in using agriculture chemical, and the key technology of sustained release then is the medicament microencapsulation.The thiophene worm quinoline preparation of domestic production mainly contains micro-capsule suspension, microcapsule granule and three kinds of formulations of aqueous suspension agent.
The suspending agent of the tiny spherical shape microcapsules that micro-capsule suspension (CS) is made up of capsule-core that contains active substance and macromolecule cyst material, the capsule diameter of microcapsule suspending agent is generally 1～20 μ m.Active substance in the capsule-core slowly discharges under the condition of control, and to satisfy suitable preventive effect requirement, spraying is used behind the microcapsule suspending agent dilute with water.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of thiophene worm quinoline micro-capsule suspension that can sustained release, and the preparation method of this micro-capsule suspension is provided simultaneously.
Technical scheme of the present invention is, a kind of thiophene worm quinoline microcapsule formulation, described thiophene worm quinoline microcapsule formulation comprises: thiophene worm quinoline 0.1-5 weight portion, solvent 5-50 weight portion, Lauxite 1-10 weight portion, emulsifier 2-10 weight portion, antifreeze 3-10 weight portion, viscosity modifier 0.05-0.3 weight portion, dispersant 2-5 weight portion, the pH regulator agent, water 0.1-100 weight portion.
Cyst material of the present invention adopts Lauxite, is to be made by home position polymerization reaction by urea-formaldehyde resin performed polymer (Lauxite prepolymer).
Further, described thiophene worm quinoline microcapsule formulation also can comprise sterilization antiseptic, defoamer a kind of or two kinds.
According to thiophene worm quinoline microcapsule formulation of the present invention, be preferably, described solvent is selected from: toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, mineral oil, aromatic solvent naphtha, N-Methyl pyrrolidone, carrene, methyl-sulfoxide, benzinum, chloroform, cyclohexanone, cyclohexane.
More preferably be that described solvent is selected from chloroform and cyclohexanone.
According to thiophene worm quinoline microcapsule formulation of the present invention, be preferably, described emulsifier is selected from one or more of following composition: lauryl sodium sulfate, neopelex, NP series Nonyl pheno, alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphoric acid fat, AEO series fatty alcohol-polyoxyethylene ether, the polyoxyethylene nonylphenol ether phosphate, polycarboxylate, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, the dialkyl succinylsuccinate sulfonated ester, this coils SPAN, soil temperature TWEEN, phenylethylene-maleic anhydride copolymerization sodium salt.
Preferably, described antifreeze is selected from: ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, urea; Described viscosity modifier is selected from: xanthans, cellulose ether and derivative thereof, polyethylene glycol, polyvinyl alcohol, magnesium alumino metasilicate, bentonite, kaolin, diatomite, attapulgite.More preferably ethylene glycol of antifreeze wherein; Viscosity modifier is xanthans, cellulose ether and derivative thereof more preferably.
Described dispersant is selected from one or more of following composition: naphthalenesulfonic acid-formaldehyde condensate, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, the alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, the polymerization of carboxylic acid salt.
Employed pH regulator agent is a kind of in glacial acetic acid, hydrochloric acid, ammoniacal liquor, monoethanolamine, diethylenetriamine, sodium hydroxide, the potassium hydroxide in the above-mentioned prescription;
Sterilization antiseptic in the prescription is: a kind of in potassium sorbate, Sodium Benzoate, formaldehyde, the isothiazolinone.
Defoamer in the prescription is preferably silicone based, the low-carbon (LC) alcohols.
The water that is adopted in this production technology: be deionized water or distilled water.
The method of producing microcapsules at present is of a great variety, generally can be divided into chemical method, physical method and physico-chemical process on principle.Method the most commonly used in the industrial production has interfacial polymerization, situ aggregation method, phase separation method, orifice-coagulating bath method, dry bath method, wraps up in core exchange process, powder bed method, air suspension film forming method, spray drying process, vacuum vapor deposition, static combined techniques and bio-microcapsule method etc.
The situ aggregation method that the present invention adopts prepares microcapsules, and this method is to prepare the most frequently used method of pesticide micro capsule, the advantage that process stabilizing is convenient to control.This method adopts the in-situ polymerization process route, generally adopts urea-formaldehyde prepolymer solution encystation, and by regulating the pH scope, polycondensation forms the microcapsules of firm difficult infiltration under catalytic action.We can add sour speed by control, add technological parameters such as the speed control of the temperature of the mode of acid, slaking, solution stirring.The microcapsules that carry out polymerization formation with urea-formaldehyde prepolymer have good toughness, sealing and permeability resistance.The method generally can be carried out fast, and the cyst wall of formation is rule, homogeneous, and quality is hard.
The present invention also provides the preparation method of above-mentioned thiophene worm quinoline microcapsule formulation, this method may further comprise the steps: the preparation of (1) performed polymer: urea is dissolved in 30%～40% formalin, formaldehyde and urea are extremely clarified with magnetic stirrer by 1: 1～1: 2.5 mol ratio, regulate pH value 7～9,45 ℃～80 ℃ of reaction temperatures, generate thick liquid after 1～3 hour reaction time, dilute with water promptly gets the stable urea-formaldehyde resin performed polymer aqueous solution again;
(2) preparation of thiophene worm quinoline solution: the normal temperature state is powdery or the former medicine 0.1-5 of graininess thiophene worm quinoline weight portion is dissolved in the solvent of 5-50 weight portion, stir, up to the solvent usage amount so that former medicine dissolving or disperse till, the back adds emulsifier and fully disperses and emulsification;
(3) preparation of thiophene worm quinoline microcapsules: the urea-formaldehyde resin performed polymer aqueous solution is joined in the thiophene worm quinoline solution under high-speed stirred, and fully dispersed with stirring becomes the ultrafine particle shape.Reduce rotating speed and add pH regulator agent adjusting pH in the 1-5 scope, the rising reaction temperature, insulation is solidified Lauxite, and polycondensation forms the microcapsules of firm difficult infiltration under the acid catalysis effect; After treating into capsule material and solidifying encystation fully, add the pH regulator agent once more, regulate pH value, adding 2-5 weight portion dispersant, the viscosity modifier of 0.05-0.3 weight portion, the antifreeze of 3-10 weight portion to neutral.
In the above-mentioned steps (1), hydromining is with distilled water or deionized water, and the preferable amount of water is the 1.5-3 doubly (weight ratio) of formaldehyde consumption, more preferably the formaldehyde consumption twice.
In the above-mentioned steps (3), the rotating speed of thiophene worm quinoline solution high-speed stirred has no special requirements, as long as can make the abundant dispersed with stirring of solution become the ultrafine particle shape.In practical operation, the preferred rotating speed of 350-700r/min; The preferred 200-500r/min of scope behind the reduction rotating speed.
Technical process of the present invention is all implemented to finish under atmospheric pressure state.
In step (1), also can add an amount of emulsifier; After solidifying encystation, can add sterilization antiseptic and/or defoamer.
Preferably, described curing reaction temperature is at 20 ℃～80 ℃; The described heat preservation solidification time varied with temperature and respective change between 2 hours～24 hours.More preferably, curing reaction temperature is at 45 ℃, and the heat preservation solidification time was at 6 hours.
Preparation method according to thiophene worm quinoline microcapsule formulation of the present invention is preferably, the granularity control 1um～20um of thiophene worm quinoline microcapsules.Between the granularity of the resulting thiophene worm of the present invention quinoline micro-capsule suspension control 1um～20um, possessed the characteristics of pesticide suspension concentrate, can convert the water use of directly spraying.
Thiophene worm quinoline micro-capsule suspension content of the present invention can change between 1%～5%, formulates different content according to its different purposes.Thiophene worm quinoline microcapsules aqueous suspension agent of the present invention also is a kind of formulation of controlled active ingredient rate of release simultaneously, and therefore according to its purposes, the thickness of decision softgel shell comes sustained release speed, to reach required effect.
The present invention is with respect to other formulations, by selecting suitable microcapsule shell material, control the rate of release of core material with the size of the hierarchical structure of thickness, hardness and the softgel shell of regulating softgel shell and capsule, can prolong the action time of medicament, lasting period reaches 2-3 month, make Monochamus alternatus Hope can both obtain continuing control in its long emergence period, this just significantly reduces spraying times, saves the dispenser cost.By the thiacloprid microcapsule suspending agent of developing, effectively reduce the toxicity of preparation, thereby improve safety non-target biology.Owing to, thereby there is the long lasting period to the sustained release of active ingredient thiophene worm quinoline, reduce the number of times of dispenser, thereby reduce the usage amount of agricultural chemicals, Zhi Bei thiacloprid microcapsule suspending agent has good preventive and therapeutic effect to the target insect simultaneously.
Major technique starting point of the present invention:
1, by improving the stability of agricultural chemicals after the pesticide micro capsuleization.
Thiophene worm quinoline is easy to be decomposed in the presence of illumination and oxygen; In soil, half life period DT50=7-21 days; Form the medicine film in environment after, sunshine quickens its decomposition.Be wrapped in the suitable UV absorbers of capsule heartwood material neutralization interpolation by thiophene worm quinoline behind the microencapsulation and effectively reduce the decomposition of ultraviolet light thiophene worm quinoline.
2, by microencapsulation prolonged the lasting period of preparation.
Photodissociation, oxidation, hydrolysis then are the principal elements that influences the agricultural chemicals lasting period.Active ingredient can artificially be controlled by the permeability of cyst material behind the microencapsulation, and slow release speed can design in advance.Because the protection of capsule skin, the active ingredient degradation speed slows down, and the agricultural chemicals lasting period can prolong 2-8 doubly.Lasting period prolongs, and just can improve control efficiency, reduces spraying times, reduces agricultural cost.
3, environmental pollution fall cause minimum.
Behind the pesticide micro capsule, medium makes organic solvents such as water rather than dimethylbenzene, thereby effectively reaches the usage amount that reduces environmental pollution and reduce organic solvent.Microcapsule formulations with water is dispersion medium, and is nonflammable explosive, transportation safety.
Embodiment
Embodiment 1
In the carrene (commercial material) that the former medicine of thiophene worm quinoline of 0.5g is dissolved in 8g and the benzinum of 15g, the emulsifier Tween-20 that adds 1g then stir (oil phase); The 25% Lauxite prepolymer aqueous solution of the emulsifier neopelex of 3.0g, 15g is added in the deionized water of 34g and stir evenly (water); The oil phase that configures to going into water and opening the high speed homogenizing, is formed stable O/W emulsion; Open to stir (keeping 600 changes/min), adding 2% hydrochloric acid HCL regulation system pH value in the 30min in batches is 2.5, rotating speed is progressively reduced to 300 commentaries on classics/min, progressively be warming up to 35 ℃ and solidify cyst wall, kept stable cyst material solidification temperature 20 hours, to reaction end, it is neutral adding NaOH regulation system pH value, the back adds the dispersant 3.0g of wooden sodium sulfonate, ethylene glycol 5.0g, the xanthans of 10g (2%) aqueous solution, Magnesiumaluminumsilicate (2%) 5g, bactericide shredding 0.1g, silicone defoaming agent 0.3g stirs, and promptly makes 0.5% thiacloprid microcapsule suspending agent.
Embodiment 2
The former medicine of thiophene worm quinoline of 2g is dissolved in the benzinum, 8g cyclohexanone of the chloroform (commercial material) of 10g and 12g the emulsifier op-10 that adds 3g then stir (oil phase); The 25% Lauxite prepolymer aqueous solution of the emulsifier sodium lauryl sulfate of 5.0g, 25g is added in the deionized water of 20g and stir evenly (water); The oil phase that configures to going into water and opening the high speed homogenizing, is formed stable O/W emulsion; Open to stir (keeping 400 changes/min), adding 2% hydrochloric acid HCL regulation system pH value in the 40min in batches is 2.5, rotating speed is progressively reduced to 300 commentaries on classics/min, progressively be warming up to 45 ℃ and solidify cyst wall, kept stable cyst material solidification temperature 6 hours, to reaction end, it is neutral adding NaOH regulation system pH value, back adding phosphoric acid ester dispersant NP-P4.0g, xanthans (2%) aqueous solution of 7.5g, bactericide formaldehyde 0.3g, silicone defoaming agent 0.3g stir, and promptly make 2% thiacloprid microcapsule suspending agent.
Embodiment 3
The former medicine of thiophene worm quinoline of 5g is dissolved in the benzinum, 15g cyclohexanone of the chloroform (commercial material) of 15g and 10g the emulsifier NP-5 that adds 4g then stir (oil phase); With the emulsifier phenylethylene-maleic anhydride copolymerization sodium salt SMA of 6.0g, the 25% Lauxite prepolymer aqueous solution (water) of 35g; The oil phase that configures to going into water and opening the high speed homogenizing, is formed stable O/W emulsion; Open to stir (keeping 400 changes/min), adding 2% hydrochloric acid HCL regulation system pH value in the 40min in batches is 2.0, rotating speed is progressively reduced to 400 commentaries on classics/min, progressively be warming up to 80 ℃ and solidify cyst wall, kept stable cyst material solidification temperature 3 hours, to reaction end, it is neutral adding NaOH regulation system pH value, back adding metal carboxylate dispersant TERSPERSE 27002.0g, xanthans (2%) aqueous solution of 5.0g, bactericide Sodium Benzoate 0.1g, silicone defoaming agent 0.3g stir, and promptly make 5% thiacloprid microcapsule suspending agent.
The key technical indexes of the embodiment of the invention such as following table 1:
The key technical indexes of table 1 embodiment of the invention
Toxicity and drug effect
1 materials and methods
1.1 test material
Reagent agent is 2% thiophene worm quinoline micro-capsule suspension, 48% thiophene worm quinoline aqueous suspension agent (contrast).For the examination apparatus is sprayer-duster.For examination worm source, place in the dependent insect cage in selecting the big withered pine tree of Monochamus alternatus Hope larva insect density to be sawn into juggle by the end of March.After the longicorn adult eclosion portals, be placed in the dependent insect cage, feed, be equipped with test and use with fresh pine branch.
1.2 overview experimental field
Experimental field be Pinus massoniana forest, the age of tree 20～30 years, the height of tree 10～15m, the sylvan life vegetation is abundant.Select the experimental field about 30hm of control, and be divided into 8 test regions therein.
1.3 experimental scheme
Establish 8 processing altogether, be respectively: 2% thiophene worm quinoline 100 times of liquid of micro-capsule suspension (A), 200 times of liquid (B), 400 times of liquid (C), 600 times of liquid (D); 48% thiophene worm quinoline 1000 times of liquid of aqueous suspension agent (E), 2000 times of liquid (F), 3000 times of liquid (G); The spray clear water is contrast (CK).1 processing is in 1 test region, randomized arrangement.Each is handled at interval and keeps more than the 50m.
1.4 test method
Each test region selects 10 strains for the examination pine tree at random, and with red lacquer mark.Respectively behind the spray medicine 7,14,28d is connecting 12 of the Monochamus alternatus Hope adults (6 sufferings, 66) that are going strong for the examination pine tree, and shroud with ready worm.All indicate different area codes and cage number on the cage.Add up longicorn imago feeding and death condition every day.
2 results and analysis
Table 1 thiophene worm quinoline woodland control Monochamus alternatus Hope drug effect
As shown in Table 1, various formulations of thiophene worm quinoline and different extension rate thereof can reach more than the 28d in lasting drug effect on the branch.But it is variant that the different extension rates of 2% thiophene worm quinoline micro-capsule suspension are poisoned the speed of longicorn adult with poison.To spraying the pine branch behind 100 times of liquid 28d of 2% thiophene worm quinoline micro-capsule suspension, 5d is all dead behind the longicorn imago feeding, and drug effect is the strongest; 200 times of liquid drug effects are taken second place, and 6d is all dead; 400 times of liquid 9d are all dead; 600 times of liquid 10d are all dead.
Be equivalent to 48% thiophene worm quinoline 3000 times of liquid of suspending agent (G) by content comparative analysis 2% thiophene worm quinoline 600 times of liquid of micro-capsule suspension (D), under the equal insect killing effect prerequisite, the unit consumption of 2% thiophene worm woods microcapsule formulations suspending agent is starkly lower than 48% common thiophene worm quinoline suspending agent consumption, microcapsule formulations effectively lowers the consumption that makes medication, plays the effect of the low consumption of environmental protection.
Claims (10)
1. thiophene worm quinoline microcapsule formulation, it is characterized in that: described thiophene worm quinoline microcapsule formulation comprises: thiophene worm quinoline 0.1-5 weight portion, solvent 5-50 weight portion, Lauxite 1-10 weight portion, emulsifier 2-10 weight portion, antifreeze 3-10 weight portion, viscosity modifier 0.05-0.3 weight portion, dispersant 2-5 weight portion, pH regulator agent, water 0.1-100 weight portion.
2. thiophene worm quinoline microcapsule formulation according to claim 1 is characterized in that: described thiophene worm quinoline microcapsule formulation comprises sterilization antiseptic, defoamer a kind of or two kinds.
3. thiophene worm quinoline microcapsule formulation according to claim 1, it is characterized in that: described solvent is selected from: toluene, dimethylbenzene, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, mineral oil, aromatic solvent naphtha, N-Methyl pyrrolidone, carrene, methyl-sulfoxide, benzinum, chloroform, cyclohexanone, cyclohexane.
4. thiophene worm quinoline microcapsule formulation according to claim 1, it is characterized in that: described emulsifier is selected from one or more of following composition: lauryl sodium sulfate, neopelex, NP series Nonyl pheno, alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphoric acid fat, AEO series fatty alcohol-polyoxyethylene ether, the polyoxyethylene nonylphenol ether phosphate, polycarboxylate, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, the dialkyl succinylsuccinate sulfonated ester, this coils SPAN, soil temperature TWEEN, phenylethylene-maleic anhydride copolymerization sodium salt.
5. thiophene worm quinoline microcapsule formulation according to claim 1, it is characterized in that: described antifreeze is selected from: ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol, urea; Described viscosity modifier is selected from: xanthans, cellulose ether and derivative thereof, polyethylene glycol, polyvinyl alcohol, magnesium alumino metasilicate, bentonite, kaolin, diatomite, attapulgite.
6. thiophene worm quinoline microcapsule formulation according to claim 1, it is characterized in that: described dispersant is selected from one or more of following composition: naphthalenesulfonic acid-formaldehyde condensate, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, the alkylphenol polyoxyethylene class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, the alkyl naphthalene formaldehyde condensate sulfonates, macromolecule is dredged a dress copolymer of type, the polymerization of carboxylic acid salt.
7. the preparation method of the described thiophene worm of claim 1 quinoline microcapsule formulation, it is characterized in that: this method is carried out according to the following steps:
(1) preparation of performed polymer: urea is dissolved in 30%～40% formalin, formaldehyde and urea are extremely clarified with magnetic stirrer by 1: 1～1: 2.5 mol ratio, regulate pH value 7～9,45 ℃～80 ℃ of reaction temperatures, generate thick liquid after 1～3 hour reaction time, dilute with water promptly gets the stable urea-formaldehyde resin performed polymer aqueous solution again;
(2) preparation of thiophene worm quinoline solution: the normal temperature state is powdery or the former medicine 0.1-5 of graininess thiophene worm quinoline weight portion is dissolved in the solvent of 5-50 weight portion, stir, up to the solvent usage amount so that former medicine dissolving or disperse till, the back adds emulsifier and fully disperses and emulsification;
(3) preparation of thiophene worm quinoline microcapsules: the urea-formaldehyde resin performed polymer aqueous solution is joined in the thiophene worm quinoline solution under high-speed stirred, and fully dispersed with stirring becomes the ultrafine particle shape.Reduce rotating speed and add pH regulator agent adjusting pH in the 1-5 scope, the rising reaction temperature, insulation is solidified Lauxite, and polycondensation forms the microcapsules of firm difficult infiltration under the acid catalysis effect; After treating into capsule material and solidifying encystation fully, add the pH regulator agent once more, regulate pH value, adding 2-5 weight portion dispersant, the viscosity modifier of 0.05-0.3 weight portion, the antifreeze of 3-10 weight portion to neutral.
8. the preparation method of thiophene worm quinoline microcapsule formulation according to claim 7 is characterized in that: add an amount of emulsifier in step (1); After solidifying encystation, add sterilization antiseptic and/or defoamer.
9. the preparation method of thiophene worm quinoline microcapsule formulation according to claim 7 is characterized in that: described curing reaction temperature is at 20 ℃～80 ℃; The described heat preservation solidification time is between 2 hours～24 hours.
10. the preparation method of thiophene worm quinoline microcapsule formulation according to claim 7 is characterized in that: the granularity control 1um～20um of thiophene worm quinoline microcapsules.
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| CN102550551B (en) * | 2011-12-22 | 2013-11-06 | 广东中迅农科股份有限公司 | Spirodiclofen microcapsule suspension |
| CN102524251A (en) * | 2012-01-17 | 2012-07-04 | 广东中迅农科股份有限公司 | Benthiavalicarb-isopropyl microcapsule suspending agent and preparation method thereof |
| CN102626086A (en) * | 2012-03-16 | 2012-08-08 | 广东中迅农科股份有限公司 | Pyridaben microcapsule suspending agent and preparation method thereof |
| CN102669147A (en) * | 2012-06-05 | 2012-09-19 | 上海沪联生物药业（夏邑）有限公司 | Microcapsule suspension containing both difenoconazole and imidacloprid and preparation method thereof |
| CN103202298A (en) * | 2013-03-21 | 2013-07-17 | 江苏三迪化学有限公司 | Method for manufacturing 2-chlorine-6-nitrapyrin microcapsule suspending agents |
| CN105230613A (en) * | 2015-11-06 | 2016-01-13 | 河北师范大学 | Preparation method of wheat chemical male gametocide microcapsule preparation |
| CN105284827A (en) * | 2015-11-26 | 2016-02-03 | 山东潍坊润丰化工股份有限公司 | Clomazone-containing microcapsule suspending agent and preparation method thereof |
| CN105284827B (en) * | 2015-11-26 | 2018-03-30 | 山东潍坊润丰化工股份有限公司 | A kind of microcapsule suspending agent containing clomazone and preparation method thereof |
| CN113812416A (en) * | 2021-08-03 | 2021-12-21 | 惠州市银农科技股份有限公司 | Double-release preparation containing thiacloprid and preparation method thereof |
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Application publication date: 20110921 |