CN1899038A - Method for producing pesticide micro capsule - Google Patents
Method for producing pesticide micro capsule Download PDFInfo
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- CN1899038A CN1899038A CN 200510084363 CN200510084363A CN1899038A CN 1899038 A CN1899038 A CN 1899038A CN 200510084363 CN200510084363 CN 200510084363 CN 200510084363 A CN200510084363 A CN 200510084363A CN 1899038 A CN1899038 A CN 1899038A
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Abstract
The present invention relates to one kind of pesticide microcapsule and its production process. The pesticide microcapsule has capsule shell material of degradable polymer material and organosilicon surfactant with high surface activity, so that it has environment friendship, lasting action and no bad smell.
Description
Technical field
The present invention relates to pesticide field, more specifically relate to a kind of manufacture method of novel agrochemical microcapsules and the pesticide micro capsule made from the method.
Background technology
Microcapsules are meant and utilize natural or synthetic macromolecule cyst material, with the small capsule nuclear matter coating formation diameter 1 μ m～semi permeability of 5000 μ m (being generally 5 μ m～400 μ m) or the microencapsulation of sealing cyst membrane of solid, liquid or even gas.Wherein the cyst material of microcapsules choose extremely important, required cyst material should form the film that one deck has adhesive force on the capsule-core material, again not with capsule-core material generation chemical reaction, also to consider permeability, stability, dissolubility, hygroscopicity and the clarity etc. of product simultaneously.Sometimes cyst material also needs to unite use so that product presents certain plasticity with surfactant, antioxidant etc.With respect to other formulation, the pesticide micro capsule agent has following advantage: (1) is owing to the sustained release of active substance has the long lasting period; (2) active substance is wrapped in safety is provided in the cyst wall; (3) provide environmental effect; (4) active substance resolution ratio of (as ultraviolet light) in environment reduces greatly; (5) some unhappy smells and can be by hidden to the material of skin irritation; (6) reduce because the loss that the steam volatilization brings active substance; (7) minimizing is to the poisoning of crop; (8) can improve stability etc. by forming the suspension compatibility that barrier makes multiple composition between the different activities material.Method for making microcapsules mainly contains interfacial polymerization, on-site polymerization, spraying capsule polymerization, poly emulsion polymerization, emulsification-propagate polymerization method etc. at present.
Wherein interfacial polymerization is a kind of novel microcapsule embedded technology.Its principle is exactly that two immiscible liquid phases are being carried out polymerisation at the interface, forms cyst material, at last this cyst material just be coated on the capsule-core material around, thereby form single profile semi permeability microcapsules spherical in shape.
Different medicaments, using method, controlling object need different-grain diameter, coat the microcapsule granule of intensity, rate of release, therefore control the importance that the capsule granularity is the preparation microcapsule formulations.In addition, the same with most of heterogeneous water base property suspending agents, the pesticide micro capsule agent must select suitable surfactant system and protection colloid system to prevent the layering and the knot end, forms otherwise can influence cyst wall, and choice of Solvent is also very important in addition.
Summary of the invention
[problem that invention solves]
Short with respect to the lasting period that traditional pesticidal preparations exists, active substance is easy to decompose, poor with the friendly of environment, shortcomings such as processing safety is low, the present invention adopts easy degraded macromolecular material to make cyst material, and select specific high surface organic silicon surfactant for use, and made a kind of novel pesticide micro capsule behind the high-shear emulsion machine forced emulsification by different rotating speeds.
[solving the means of problem]
The present invention utilizes interfacial polymerization manufactured microcapsule pesticide.Utilize the reason of interfacial polymerization to be among the present invention owing in preparation process, use harmless solvent, can make human body harmless substantially, the micro-fine capsule of different-grain diameter.
This interfacial polymerization is, contains easy degraded macromolecular and liquid medicine and mixes with the water that contains the different surfaces activating agent, by stirring the continuous phase of the solvent phase that exists, is formed on the equilibrium figure of the drop of aqueous phase.At this moment,, make the emulsification in water that solvent can not be spontaneous on the drop at newly-generated interface, must stir because the aforementioned stable agent adheres to.Should add a large amount of water if reach solvent consoluet degree in water,, can pass through the micro-fine capsule of the mobile manufacturing microcapsules of solute in water because thermodynamic (al) unstable solvent spreads.
The above-mentioned manufacture method of the microcapsule pesticide of the present invention of interfacial polymerization of utilizing comprises the steps:
1) the easy degraded macromolecular of 0.1～1.0 weight portion is dissolved in 5～20 weight portion organic solvents;
2) in the solution of the above-mentioned easy degraded macromolecular of dissolving, mix 0.01～1 weight portion pesticidal active substance;
3) 0.1～5 weight portion high surface surfactant and 0.1～10 weight portion stabilizing agent are dissolved in 20～500 weight parts waters.
4) with step 2) and the gained solution of step 3) mix;
5) mixed liquor that step 4) is obtained at first stirs in high-shear emulsion machine, removes solvent then in slow-speed of revolution stirred reactor, solidifies encystation.
Easy degraded macromolecular among the present invention is as the capsule agent cyst material, and it is preferably selected from a kind of or its combination in poly-hexylamine lactone, poly-allyl acetate, methylcellulose, the carboxymethyl cellulose.
The solvent of the easy degraded macromolecular of dissolving is harmless among the present invention, and physico chemical property are stable, with water base unmixing and the solvent big to the macromolecule dissolution degree.As solvent above-mentioned among the present invention, it is preferably selected from benzinum, ethyl acetate, carrene, the chloroform any.
Pesticidal active substance among the present invention can be organic phosphor, pyrethroid, macrolide, carbamate etc.Be preferably selected among Cyhalothrin, cypermethrin, beta-cypermethrin, chlopyrifos, diazinon, Avermectin, Affirm (Merck Co.), the furans pellet any.
For making easy degraded macromolecular and agricultural chemicals and water form stable interface, stabilizing agent can require to select in anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan mono-laurate, polypropylene glycol oxirane ether, NaLS, dodecyl sodium sulfate, the polyethylene glycol any according to different surfaces tension force.
The aforementioned stable agent normally mixes use with the organic silicon surfactant of high surface.Described organic silicon surfactant for example is " Boost " of Doro Elaneo company; " L-77 " of union carbide corporation; " Sylgard309 " of Doco Corning company etc.
In above-mentioned steps 5) manufacture method in, earlier with high-shear emulsion machine with the mixing speed forced emulsification of 1000～15000rpm 1～15 minute, in the stirring at low speed reactor of 300～1500rpm, remove solvent again, solidify encystation.
The temperature that solvent steams is preferably 20～80 ℃.After the curing, the elimination water.
[invention effect]
The present invention utilizes interfacial polymerization method, adopts different rotating speeds, shell material, combinations-of surfactants, the pesticide micro capsule agent that can prepare different-grain diameter.
Microcapsule pesticide constructed in accordance can reach sustained release, the continuation excellence of drug effect, and also usage amount is few, has very high economic worth.
Microcapsule pesticide of the present invention is that the polymer substance with easy degraded is a shell material, and it is little not have unhappy smell and environmental pollution.
Description of drawings
Fig. 1: the microphotograph of average grain diameter 5um microcapsules;
Fig. 2: the microphotograph of average grain diameter 50um microcapsules;
Embodiment
Following examples only are to exemplary illustration of the present invention, and limitation of the scope of the invention anything but.
Preparation embodiment 1
In the 100g benzinum, behind the dissolving 15g carboxymethyl cellulose, mix 1g beta-cypermethrin under the normal temperature as insecticide active substance.
Dissolving 20g sorbitan mono-laurate and 5gL-77 organic silicon surfactant in 500g water.
With above-mentioned two kinds of mixing.Stirred 1～15 minute with 1000～15000rpm in high-shear emulsion machine, 50 ℃ of removal solvents in the stirring at low speed reactor of 300～1500rpm solidify encystation and filtration drying again.
The gained microcapsules as shown in Figure 1.
The physical and chemical parameter of these microcapsules is as follows:
| Project | Index |
| Beta-cypermethrin content, % (m/m) 〉= | 5.0 |
| Average grain diameter, (um)≤ | 5 |
| The pH value | 5.0-7.0 |
| Moisture % ,≤ | 2.0 |
| Heat storage stability (54 ℃ ± 2 ℃, 14 days) | Qualified |
Rate of release is measured in the water:
Take by weighing the 1.0g sample, be accurate to 0.0001g, add in the tool plug triangular flask, add 100ml distilled water, put into 30 ℃ ± 2 ℃ water bath with thermostatic control shaking tables after jumping a queue and continue to shake, regularly filter, measure active constituent content in the clear filtrate,
| Time (hour) | Burst size (%) |
| 12 | 0.9 |
| 24 | 1.6 |
| 48 | 3.1 |
| 72 | 5.2 |
Hence one can see that, and these microcapsules have good physicochemical property and slow release effect.
Preparation embodiment 2
In the 100g ethyl acetate solvent, dissolve poly-hexylamine lactone of the easy degraded macromolecular of 5g and 5g chlopyrifos under the normal temperature.
Dissolving 15g dodecyl sodium sulfate and 1gL-77 organic silicon surfactant in 500g water.
With above-mentioned organic solution and aqueous solution.In high-shear emulsion machine to stir under 1000～15000rpm 1～15 minute., 70 ℃ of removal solvents in the stirring at low speed reactor of 300～1500rpm solidify encystation and filtration drying again.
The gained microcapsules as shown in Figure 2.
The same with embodiment 1, these embodiment gained microcapsules also have good physicochemical property and slow release effect.
Claims (8)
1. the manufacture method of pesticide micro capsule is characterized in that comprising following steps:
1) the easy degraded macromolecular of 0.1～1.0 weight portion is dissolved in 5～20 weight portion organic solvents;
2) in the solution of the above-mentioned easy degraded macromolecular of dissolving, mix 0.01～1 weight portion pesticidal active substance;
3) 0.1～5 weight portion high surface surfactant and 0.1～10 weight portion stabilizing agent are dissolved in 20～500 weight parts waters.
4) with step 2) and the gained solution of step 3) mix;
5) mixed liquor that step 4) is obtained at first stirs in high-shear emulsion machine, removes solvent then in slow-speed of revolution stirred reactor, solidifies encystation.
2. according to the manufacture method of the pesticide micro capsule of claim 1, it is characterized in that above-mentioned easy degraded macromolecular is selected from a kind of or its combination in poly-hexylamine lactone, poly-allyl acetate, methylcellulose, the carboxymethyl cellulose.
3. according to the manufacture method of the pesticide micro capsule of claim 1, it is characterized in that above-mentioned organic solvent is any or its combination that is selected among benzinum, ethyl acetate, carrene, the chloroform.
4. according to the manufacture method of the pesticide micro capsule of claim 1, it is characterized in that above-mentioned pesticidal active substance is selected from Cyhalothrin, cypermethrin, beta-cypermethrin, chlopyrifos, diazinon, Avermectin, Affirm (Merck Co.) or furans pellet.
5. according to the manufacture method of the pesticide micro capsule of claim 1, it is characterized in that the aforementioned stable agent is selected from anhydrous sorbitol polyoxyethylene poly-oxygen propylene aether, sorbitan mono-laurate, polypropylene glycol oxirane ether, NaLS, dodecyl sodium sulfate or polyethylene glycol.
6. according to the manufacture method of the pesticide micro capsule of claim 1, it is characterized in that above-mentioned high surface surfactant is an organic silicon surfactant.
7. according to the manufacture method of the pesticide micro capsule of claim 1, it is characterized in that in step 5) earlier with high-shear emulsion machine in the stirred reactor of 300～1500rpm, removing solvent again with the mixing speed forced emulsification of 1000～15000rpm 1～15 minute.
8. the pesticide micro capsule of making according to the manufacture method of arbitrary microcapsules of claim 1-7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100843639A CN100372461C (en) | 2005-07-20 | 2005-07-20 | Method for producing pesticide micro capsule |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100843639A CN100372461C (en) | 2005-07-20 | 2005-07-20 | Method for producing pesticide micro capsule |
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| Publication Number | Publication Date |
|---|---|
| CN1899038A true CN1899038A (en) | 2007-01-24 |
| CN100372461C CN100372461C (en) | 2008-03-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100843639A Active CN100372461C (en) | 2005-07-20 | 2005-07-20 | Method for producing pesticide micro capsule |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502266A (en) * | 2009-03-27 | 2009-08-12 | 郭正 | Liquid pesticide formulation containing avermectin pesticide and organosilicon surfactant and preparation method thereof |
| CN101642099A (en) * | 2009-08-31 | 2010-02-10 | 桂林集琦生化有限公司 | Pesticide suspension concentrate with organosilicon surfactant and preparation method thereof |
| CN102273447A (en) * | 2011-06-27 | 2011-12-14 | 上海师范大学 | Abamectin-blue green algae ultraviolet-resistant sustained-release microcapsule pesticide and preparation method thereof |
| CN101461359B (en) * | 2009-01-15 | 2012-07-04 | 中国农业大学 | Method for preparing controlled release type nano pesticide |
| CN101632355B (en) * | 2009-08-31 | 2012-11-21 | 桂林集琦生化有限公司 | Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof |
| CN101743960B (en) * | 2010-02-01 | 2012-12-05 | 吴学民 | Thiacloprid microcapsule powder agent, suspending agent and preparation method and application thereof |
| CN104012528A (en) * | 2014-06-16 | 2014-09-03 | 江西农业大学 | Preparation method of pesticide microcapsule containing organic silicon |
| CN105557741A (en) * | 2016-03-04 | 2016-05-11 | 扬州大学 | Beta-cypermethrin microcapsule and preparation method thereof |
| CN105685081A (en) * | 2016-02-29 | 2016-06-22 | 南通香佳纺织科技有限公司 | Preparation method of microcapsule pesticide seed dressing agent for controlling soil insects |
| CN105707069A (en) * | 2016-04-13 | 2016-06-29 | 南通清安健无水印染研究所（普通合伙） | Preparation method of microencapsulated pesticide for controlling sugarcane borers |
| CN105875600A (en) * | 2016-04-13 | 2016-08-24 | 南通清安健无水印染研究所（普通合伙） | Preparation method of trunk-injecting microcapsule pesticide for controlling longhorn beetles on poplars |
| CN106035327A (en) * | 2016-06-16 | 2016-10-26 | 周启新 | Preparation method of biological pesticide microcapsules |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100515064B1 (en) * | 2003-01-30 | 2005-09-14 | 이병희 | Preparation Method for Microcapsule Insecticides |
-
2005
- 2005-07-20 CN CNB2005100843639A patent/CN100372461C/en active Active
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101461359B (en) * | 2009-01-15 | 2012-07-04 | 中国农业大学 | Method for preparing controlled release type nano pesticide |
| CN101502266A (en) * | 2009-03-27 | 2009-08-12 | 郭正 | Liquid pesticide formulation containing avermectin pesticide and organosilicon surfactant and preparation method thereof |
| CN101502266B (en) * | 2009-03-27 | 2012-10-17 | 郭正 | Liquid pesticide formulation containing avermectin pesticide and organosilicon surfactant and preparation method thereof |
| CN101632355B (en) * | 2009-08-31 | 2012-11-21 | 桂林集琦生化有限公司 | Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof |
| CN101642099B (en) * | 2009-08-31 | 2012-10-17 | 桂林集琦生化有限公司 | Pesticide suspension concentrate with organosilicon surfactant and preparation method thereof |
| CN101642099A (en) * | 2009-08-31 | 2010-02-10 | 桂林集琦生化有限公司 | Pesticide suspension concentrate with organosilicon surfactant and preparation method thereof |
| CN101743960B (en) * | 2010-02-01 | 2012-12-05 | 吴学民 | Thiacloprid microcapsule powder agent, suspending agent and preparation method and application thereof |
| CN102273447A (en) * | 2011-06-27 | 2011-12-14 | 上海师范大学 | Abamectin-blue green algae ultraviolet-resistant sustained-release microcapsule pesticide and preparation method thereof |
| CN102273447B (en) * | 2011-06-27 | 2014-10-15 | 上海师范大学 | Abamectin-blue green algae ultraviolet-resistant sustained-release microcapsule pesticide and preparation method thereof |
| CN104012528A (en) * | 2014-06-16 | 2014-09-03 | 江西农业大学 | Preparation method of pesticide microcapsule containing organic silicon |
| CN105685081A (en) * | 2016-02-29 | 2016-06-22 | 南通香佳纺织科技有限公司 | Preparation method of microcapsule pesticide seed dressing agent for controlling soil insects |
| CN105557741A (en) * | 2016-03-04 | 2016-05-11 | 扬州大学 | Beta-cypermethrin microcapsule and preparation method thereof |
| CN105707069A (en) * | 2016-04-13 | 2016-06-29 | 南通清安健无水印染研究所（普通合伙） | Preparation method of microencapsulated pesticide for controlling sugarcane borers |
| CN105875600A (en) * | 2016-04-13 | 2016-08-24 | 南通清安健无水印染研究所（普通合伙） | Preparation method of trunk-injecting microcapsule pesticide for controlling longhorn beetles on poplars |
| CN106035327A (en) * | 2016-06-16 | 2016-10-26 | 周启新 | Preparation method of biological pesticide microcapsules |
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|---|---|
| CN100372461C (en) | 2008-03-05 |
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Owner name: JIANGXI TIANREN ECO-INDUSTRIAL CO., LTD. Free format text: FORMER OWNER: WU XUEMIN Effective date: 20080808 |
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Effective date of registration: 20080808 Address after: Hi tech Industrial Development Zone, Ji'an, Jiangxi Patentee after: Jiangxi Tianren Zoology Industrial Co., Ltd. Address before: Department of chemistry, School of science, China Agricultural University, 2 West Old Summer Palace Road, Beijing, Haidian District Patentee before: Wu Xuemin |
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Address after: 343100 Jinggangshan Jiangxi economic and Technological Development Zone Patentee after: Jiangxi Tianren Ecology Co., Ltd. Address before: 343100 hi tech Industrial Development Zone, Jiangxi, Ji'an Patentee before: Jiangxi Tianren Zoology Industrial Co., Ltd. |
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