CN104365595A - Pesticide microcapsules produced by layer-by-layer self-assembly - Google Patents
Pesticide microcapsules produced by layer-by-layer self-assembly Download PDFInfo
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- CN104365595A CN104365595A CN201410704961.0A CN201410704961A CN104365595A CN 104365595 A CN104365595 A CN 104365595A CN 201410704961 A CN201410704961 A CN 201410704961A CN 104365595 A CN104365595 A CN 104365595A
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Abstract
The invention relates to pesticide preparations and relates to water-soluble pesticide suspension concentrate of microcapsule type, in particular to pesticide microcapsules containing any one of abamectin, lime sulphur, triadimefon, streptomycin prochloraz, carbendazim, chlorothalonil, kresoxim-methyl, thiophanate methyl, astromicin, antimycoin, hymexazol, metalaxyl, myclobutanil, moroxydine hydrochloride, dioctyl divinyltriamino glycine acetate, pyrimethanil, myclobutanil, glyphosate, paraquat, acetochlor, imidacloprid, acetamiprid, pymetrozine, thiamethoxam and pyridaben. Each pesticide microcapsule comprises a wall and a core; the core is made of effective ingredients and solvent; the wall is made of polyester material of polyelectrolyte. The pesticide microcapsules have the advantages that application cost is lowered and less pesticide is applied.
Description
Technical field
The invention belongs to pesticidal preparations production field, be related specifically to pesticide micro capsule prepared by a kind of LBL self-assembly method.
[background technology]
Micro-capsule suspension agricultural chemicals refers to the small container utilizing the macromolecular material of natural or synthesis to form nucleocapsid structure, and agricultural chemicals is wherein coated, and is suspended in the formulations of pesticide in water.It comprises cyst wall and capsule heart two parts, and the capsule heart is pesticide active ingredient and solvent, and cyst wall is the macromolecular material of film forming.This formulation is divided into continuous phase and discontinuous phase, and continuous phase is water and auxiliary agent, and discontinuous phase is the agricultural chemicals tiny capsules be wrapped by.
Layer-by-layer has been widely used in the preparation of medical microcapsules, because its technology content is higher comparatively speaking, does not also popularize in the preparation of pesticide micro capsule.But because bottleneck period has been arrived in the research of the preparation method to existing pesticide micro capsule, this will introduce new method to prepare pesticide micro capsule with regard to being badly in need of.That studies layer-by-layer along with researcher deepens continuously, and continues to optimize technology path, the incomparable advantage had with this technology, will become a kind of new pesticide micro capsule preparation method in the near future.
Layer-by-layer utilizes supermolecule electrostatic self-assembled principle, adsorbed the polyelectrolyte of oppositely charged successively, thus form ultrathin membrane having multi-functions by the effect of electrostatic attraction.The selection of film is not by the impact of substrate, and different agricultural chemicals can have general cyst material.
[summary of the invention]
The invention provides the pesticide micro capsule made of layer-by-layer.
The agricultural chemicals that the present invention adopts LBL self-assembly method to prepare, has following advantage:
1. the thickness of adsorption layer is in nano-scale range, can regulate and control accurately;
2. different agricultural chemicals can have general base material;
3. obtained pesticide micro capsule, reduces use cost, reduces quantity and the frequency of dispenser, reduces agricultural chemicals and runs off and accelerate residue degraded.
[embodiment]
The present invention is intended to the obtained pesticide micro capsule product of protection LBL self-assembly method.
Can better understand the present invention below by good embodiment and embodiment, although give these embodiments, but method of the present invention also should comprise: do not departing under scope of the invention condition, the apparent various change of those skilled in the art is carried out to disclosed method.
The scheme of layer-by-layer that the present invention uses is: that (1) first adds in agricultural-chemical suspension liquid is excessive, with the opposite polarity polyelectrolyte of its surface charge, electrostatic attraction is utilized to act on adsorption one deck polyelectrolyte layer of agricultural chemicals particulate, the polyelectrolyte that centrifugal removing is unnecessary to spend deionized water clean, then the polyelectrolyte with opposite charges is added, electrostatic attraction effect is utilized to adsorb last layer polyelectrolyte layer again, centrifugal and washes clean.(2) repeat the operation of (1), make the polyelectrolyte of oppositely charged at agricultural chemicals microparticle surfaces alternating sorbent, form multilayer film, thus prepare with agricultural chemicals particulate for capsule-core, polyelectrolyte multilayer film is the microcapsules of Nang wall.
Concrete technology step of the present invention is:
The preparation of step 1, agricultural-chemical suspension liquid: take certain agricultural chemicals, dissolve in organic solvent, add the aqueous solution containing surfactant, then in agitator with 700-1250r/min rapid stirring 10-15 minute, obtain oil-in-water agricultural-chemical suspension liquid A; Consisting of of the percentage by weight of agricultural chemicals, organic solvent, surfactant and water: agricultural chemicals 1%-30%, organic solvent 40%, surfactant 1-5%, supplies 100% with water.
Step 2: add in solution A excessive, with the opposite polarity polyelectrolyte of its surface charge, the polyelectrolyte that centrifugal removing is unnecessary to spend deionized water clean.
Step 3: repeat step 2, make the polyelectrolyte of oppositely charged in the absorption of agricultural chemicals microparticle surfaces, form multilayer film, thus to prepare with colloidal particle be capsule-core, polyelectrolyte multilayer film is the microcapsules of Nang wall.
Embodiment 1:(1) the water stirring at low speed of the Avermectin of 10g, the acetone of 40g, the carboxylate adding 2g and 38g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 30g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain avermectin microcapsule.
Embodiment 2:(1) the water stirring at low speed of the lime sulfur of 10g, the acetone of 40g, the carboxylate adding 2g and 38g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 30g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain lime sulfur microcapsules.
Embodiment 3:(1) the water stirring at low speed of the triadimefon of 10g, the acetone of 40g, the carboxylate adding 2g and 38g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 30g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain triadimefon microcapsules.
Embodiment 4:(1) the water stirring at low speed of the lime sulfur of 10g, the methyl alcohol of 40g, the carboxylate adding 2g and 38g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 50g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain lime sulfur microcapsules.
Embodiment 5:(1) the water stirring at low speed of the lime sulfur of 5g, the dimethylbenzene of 40g, the carboxylate adding 2g and 43g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 50g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain lime sulfur microcapsules.
Embodiment 6:(1) the water stirring at low speed of the Astromicin of 10g, the methyl alcohol of 40g, the carboxylate adding 2g and 38g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 50g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain Astromicin microcapsules.
Embodiment 7:(1) the water stirring at low speed of the pymetrozine of 5g, the dimethylbenzene of 40g, the carboxylate adding 2g and 43g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 50g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain pymetrozine microcapsules.
Embodiment 8:(1) the water stirring at low speed of the Moroxydine Hydrochloride of 10g, the methyl alcohol of 40g, the carboxylate adding 2g and 38g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 50g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain Moroxydine Hydrochloride microcapsules.
Embodiment 9:(1) the water stirring at low speed of the pyridaben of 5g, the dimethylbenzene of 40g, the carboxylate adding 2g and 43g mixes 10 minutes, obtains agricultural-chemical suspension liquid A; (2) in A, 50g PAMC mix and blend 30 minutes are added, centrifugal removing polyelectrolyte to spend deionized water clean; (3) repeat (2) three times, obtain pyridaben microcapsules.
Claims (7)
1. with pesticide micro capsule prepared by LBL self-assembly method, it is characterized in that: the pesticide micro capsule prepared by LBL self-assembly method, its microcapsule size be 5-200 micron can be water-soluble agricultural chemicals suspension agent.
2. pesticide micro capsule according to claim 1, it is characterized in that: described pesticide micro capsule prepares gained by following method, (1) first add in agricultural-chemical suspension liquid excessive, with the opposite polarity polyelectrolyte of its surface charge, electrostatic attraction is utilized to act on adsorption one deck polyelectrolyte layer of agricultural chemicals particulate, the polyelectrolyte that centrifugal removing is unnecessary to spend deionized water clean, then the polyelectrolyte with opposite charges is added, electrostatic attraction effect is utilized to adsorb last layer polyelectrolyte layer again, centrifugal and washes clean; (2) repeat the operation of (1), make the polyelectrolyte of oppositely charged at agricultural chemicals microparticle surfaces alternating sorbent, form multilayer film, thus prepare with agricultural chemicals particulate for capsule-core, polyelectrolyte multilayer film is the microcapsules of Nang wall.
3. agricultural-chemical suspension liquid according to claim 2, it is characterized in that: with organic solvent, farm chemical ingredients is dissolved, add the aqueous solution containing surfactant, then in agitator with 700-1250r/min rapid stirring 10-15 minute, obtain oil-in-water milky mixed liquor; This milky mixed liquor is exactly agricultural-chemical suspension liquid, it is characterized in that being made up of the particulate of 30nm-800nm.Consisting of of the percentage by weight of agricultural chemicals, organic solvent, surfactant and water: agricultural chemicals 1%-30%, organic solvent 40%, surfactant 1-5%, supplies 100% with water.
4. agricultural chemicals according to claim 3, is characterized in that: described agricultural chemicals is one or more in following medicine: Avermectin, lime sulfur, triadimefon, streptomycin Prochloraz, carbendazim, tpn, kresoxim-methyl, thiophanate methyl, Astromicin, antimycoin, carbendazim, the mould spirit of evil, first frost, nitrile bacterium azoles, Moroxydine Hydrochloride, pungent bacterium amine acetate, phonetic mould amine, nitrile bacterium azoles, glyphosate, paraquat, Acetochlor, Imidacloprid, Acetamiprid, pymetrozine, Diacloden, pyridaben.
5. polyelectrolyte according to claim 2, is characterized in that: described polyelectrolyte belongs to any one in PAMC, PDDA, Chitosan (shitosan); The consumption of polyelectrolyte is 5-10 times of pesticide concentration.
6. surfactant according to claim 3, is characterized in that: described surfactant is any one in carboxylate, sulfuric acid, sulfonate, phosphate ester salt.
7. organic solvent according to claim 3, is characterized in that: described organic solvent is one or more in acetone, dimethylbenzene, toluene, benzene, methyl alcohol, ethanol, cyclohexanone, dimethyl formamide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105625038A (en) * | 2016-03-28 | 2016-06-01 | 西南大学 | Method for preparing functional cotton fabric by layer-by-layer assembly of phytic acid via cationic polyacrylamide |
| CN106035323A (en) * | 2016-05-25 | 2016-10-26 | 广西南宁农事帮农业科技服务有限公司 | Sustained-release pesticide granules and preparation method therefor |
| CN109511669A (en) * | 2018-11-22 | 2019-03-26 | 然晟(上海)实业发展有限公司 | A kind of self assembly legal system Ficam micro-capsule suspension and preparation method thereof |
| CN111068596A (en) * | 2019-12-26 | 2020-04-28 | 浙江大学 | Self-assembled nanosphere and preparation method and application thereof |
| CN113142228A (en) * | 2018-08-28 | 2021-07-23 | 侨昌现代农业有限公司 | Bactericide composition |
| US11382330B2 (en) | 2017-12-25 | 2022-07-12 | Dow Global Technologies Llc | Micro-encapsulation of an insecticide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070292464A1 (en) * | 2006-04-11 | 2007-12-20 | Raymond Mathis | Fibers and sheet-form textiles provided with insect-repellent finishes |
| CN101869112A (en) * | 2009-04-23 | 2010-10-27 | 迟德富 | Method for preparing controlled photodegradable nano avermectins microcapsules |
| CN101869115A (en) * | 2009-04-23 | 2010-10-27 | 迟德富 | Method for preparing nano diflubenzuron microcapsules |
-
2014
- 2014-11-27 CN CN201410704961.0A patent/CN104365595A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070292464A1 (en) * | 2006-04-11 | 2007-12-20 | Raymond Mathis | Fibers and sheet-form textiles provided with insect-repellent finishes |
| CN101869112A (en) * | 2009-04-23 | 2010-10-27 | 迟德富 | Method for preparing controlled photodegradable nano avermectins microcapsules |
| CN101869115A (en) * | 2009-04-23 | 2010-10-27 | 迟德富 | Method for preparing nano diflubenzuron microcapsules |
Non-Patent Citations (3)
| Title |
|---|
| 周斌 等: "层层自组装制备阿维菌素微胶囊及其释药行为", 《精细化工》, vol. 25, no. 7, 31 July 2008 (2008-07-31), pages 625 - 627 * |
| 廖科超 等: "丁烯氟虫腈缓释微胶囊的制备与性能", 《应用化学》, vol. 31, no. 9, 30 September 2014 (2014-09-30), pages 1037 - 1042 * |
| 贾进伟 等: "负载戊唑醇的壳聚糖纳米胶囊的制备与性能研究", 《农药学学报》, vol. 15, no. 5, 31 December 2013 (2013-12-31), pages 582 - 586 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105625038A (en) * | 2016-03-28 | 2016-06-01 | 西南大学 | Method for preparing functional cotton fabric by layer-by-layer assembly of phytic acid via cationic polyacrylamide |
| CN106035323A (en) * | 2016-05-25 | 2016-10-26 | 广西南宁农事帮农业科技服务有限公司 | Sustained-release pesticide granules and preparation method therefor |
| CN106035323B (en) * | 2016-05-25 | 2018-12-11 | 广西南宁农事帮农业科技服务有限公司 | A kind of sustained releasing pesticide granule and preparation method thereof |
| US11382330B2 (en) | 2017-12-25 | 2022-07-12 | Dow Global Technologies Llc | Micro-encapsulation of an insecticide |
| CN113142228A (en) * | 2018-08-28 | 2021-07-23 | 侨昌现代农业有限公司 | Bactericide composition |
| CN109511669A (en) * | 2018-11-22 | 2019-03-26 | 然晟(上海)实业发展有限公司 | A kind of self assembly legal system Ficam micro-capsule suspension and preparation method thereof |
| CN109511669B (en) * | 2018-11-22 | 2021-07-09 | 然晟(上海)实业发展有限公司 | Self-assembly method bendiocarb microcapsule suspension and preparation method thereof |
| CN111068596A (en) * | 2019-12-26 | 2020-04-28 | 浙江大学 | Self-assembled nanosphere and preparation method and application thereof |
| CN111068596B (en) * | 2019-12-26 | 2021-06-11 | 浙江大学 | Self-assembled nanosphere and preparation method and application thereof |
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Application publication date: 20150225 |