CN101869115A - Method for preparing nano diflubenzuron microcapsules - Google Patents
Method for preparing nano diflubenzuron microcapsules Download PDFInfo
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- CN101869115A CN101869115A CN200910071865A CN200910071865A CN101869115A CN 101869115 A CN101869115 A CN 101869115A CN 200910071865 A CN200910071865 A CN 200910071865A CN 200910071865 A CN200910071865 A CN 200910071865A CN 101869115 A CN101869115 A CN 101869115A
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Abstract
The invention relates to a method for preparing nano diflubenzuron microcapsules, which is characterized by (1) re-separating out the raw pesticides in the form of crystals and adjusting the particle size by adopting a probe type ultrasonic method or a vibration method, (2) using diflubenzuron as the template particles, using two biocompatible macromolecules with opposite charges as the wall materials and forming an extremely thin protective outer film on the surface of diflubenzuron, thus obtaining the diflubenzuron microcapsules. The method is simple in process, mild in reaction conditions, easy in operation and good in repeatability, provides material base and technical support for developing the efficient green pesticides and has good application prospect.
Description
Technical field
The invention belongs to the novel agrochemical formulations field, especially relate to a kind of preparation method of diflubenzuron slow-release microcapsule.
Background technology
At present, chemical pesticide is that the mankind develop, the active drug that is used for destroying plant diseases and insect pests.Since human use's chemical pesticide, all benefits that chemical pesticide brings to the mankind have been experienced, increasing crop yield, prevention and the control mankind's infectious disease, according to FAO's survey data introduction, the annual cereal that is seized by damage by disease and insect in the whole world accounts for the 20%-30% of harvest, thus, the economic loss that causes reaches 1,200 hundred million dollars, in order to tackle damage by disease and insect, to produce more than 200 ten thousand tons of various chemical pesticides every year, its sales volume every year is up to 10,000,000,000 dollars.
But, chemical pesticide brings human destruction and yet fades in and revealed to come, because a large amount of chemical pesticides that use, air, the water source, soil and food have been subjected to pollution, poisonous substance causes that intoxicating phenomenon takes place repeatedly in the middle of being accumulated in domestic animal and human body, the whole world has 2,000,000 people to poison because of using chemical pesticide every year approximately, wherein about 40,000 people's death, and, long-term some chemical pesticide that uses also can make insect develop immunity to drugs, and existing 417 kinds at present of drug-fast insects are arranged, and China has begun complete prohibition and used organo-chlorine pesticide in 1987, however, the agricultural chemicals of accumulation still plays a role in considerable time in the past.Having does not have a kind of novel agricultural chemicals only to tackle damage by disease and insect, and the mankind are had no side effect, in recent years, in agricultural production, applying biological agricultural chemicals substituting chemical pesticide becomes a kind of trend gradually, countries in the world are at all drawbacks of chemical pesticide, have developed that a series of selectivity are strong, efficient is high, cost is low, pollution-free, to person poultry harmless's biopesticide.
Summary of the invention
The object of the present invention is to provide a kind of agricultural chemicals that can prevent to be destroyed, make it the steadily strategy of release by various digestive ferments in the insect bodies, and have drug effect height, the wide advantage of easily degrading that reaches of insecticidal spectrum, thereby the method for preparing nano diflubenzuron microcapsules of the residual contamination of the killing rate of enhancing agricultural chemicals and minimizing agricultural chemicals
In order to achieve the above object, the technical solution used in the present invention is:
(1) the former medicine crystal recrystallization of diflubenzuron: the former medicine of 0.1-0.5g diflubenzuron is dissolved in the 50mL organic reagent, magnetic agitation 1h, wait to dissolve the complete instantaneous adding 200mL in back and contain 0.025%m/v hydroxypropyl methylcellulose (HPMC) deionized water, magnetic agitation, use the probe-type ultrasonic to regulate diflubenzuron agricultural chemicals crystal particle diameter size, ultrasonic time is 0～10 minute, and particle size is the 0.1-100 micron, obtain the former medicine recrystallization of diflubenzuron crystal
(2) adopting layer by layer, self-assembly method prepares nano diflubenzuron: the former medicine recrystallization of the diflubenzuron that obtains crystal 10mg-100mg is scattered in the 500 μ L deionized waters; Add 1mL cationic polyelectrolyte chitosan solution 0.5-5mg/mL; Ultrasonic absorption 5-15min; Through twice centrifugal-removal supernatant-washing-cycle of oscillation; Add 1mL anionic polyelectrolyte sodium alginate soln 0.5-5mg/mL; Absorption 5-15min; Repeat above-mentioned steps; Successively adsorb shitosan and sodium alginate; Namely obtain the nano diflubenzuron microcapsules of 5-10 layer nucleocapsid structure
The described recrystallization organic reagent organic solvent that to be isopropyl alcohol, acetone, b propanol, methyl alcohol etc. dissolve each other with water.
Described polyanion is seaweeds sodium, dextran sulfate, sodium carboxymethylcellulose.
Described polycation is shitosan, poly arginine, cation dextran.
The described polymer number of plies is the 1-20 bilayer.
Advantage of the present invention is:
(1) envelop rate and the medicine carrying amount of diflubenzuron microcapsules have been improved;
(2) the insect midgut location absorbs;
(3) the diflubenzuron rate of release can be by the THICKNESS CONTROL of cyst wall;
(4) cyst material of microcapsules is a natural macromolecular material, cheap and environmental sound;
(5) technology of the present invention is simple, and the reaction condition gentleness is easy to operate, favorable reproducibility, and environmental friendliness for the development of efficient green agricultural chemicals provides material base and technical guarantee, has a good application prospect.
Description of drawings
Fig. 1 is the diflubenzuron microcapsules scanning electron microscope diagram sheet that the present invention coats 5 bilayers (CHI/ALG);
Fig. 2 is the diflubenzuron microcapsules scanning electron microscope diagram sheet that the present invention coats 10 bilayers (CHI/ALG);
Fig. 3 is electromotive force potential change figure in the coating process of the present invention;
Fig. 4 is a slow release effect comparison diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described in further detail.
Embodiment 1,
(1) the former medicine crystal recrystallization of diflubenzuron: the former medicine of 0.1g diflubenzuron is dissolved in the 50mL acetone, magnetic agitation 1h, wait to dissolve the complete instantaneous adding 200mL in back and contain 0.025%m/v hydroxypropyl methylcellulose (HPMC) deionized water, magnetic agitation, use the probe-type ultrasonic to regulate diflubenzuron agricultural chemicals crystal particle diameter size, ultrasonic time is 3 minutes, and particle size is 0.1 micron, obtain the former medicine recrystallization of diflubenzuron crystal
(2) adopting layer by layer, self-assembly method prepares nano diflubenzuron: 10mg is scattered in the 500 μ L deionized waters with the former medicine recrystallization of the diflubenzuron that obtains crystal, adding 1mL concentration is the 1.6mg/mL shitosan, ultrasonic absorption 5min, through two times centrifugal-removal supernatant-washing-cycle of oscillation, adding 1mL concentration is the 1.5mg/mL sodium alginate, and absorption 5min repeats above-mentioned steps, successively adsorb shitosan and sodium alginate, promptly obtain the nano diflubenzuron microcapsules of 5 layers of nucleocapsid structure.
Embodiment 2,
(1) the former medicine crystal recrystallization of diflubenzuron: the former medicine of 0.3g diflubenzuron is dissolved in the 50ml isopropyl alcohol, magnetic agitation 1h, wait to dissolve the complete instantaneous adding 200mL in back and contain 0.025%m/v hydroxypropyl methylcellulose (HPMC) deionized water, magnetic agitation, use the probe-type ultrasonic to regulate diflubenzuron agricultural chemicals crystal particle diameter size, ultrasonic time is 6 minutes, and particle size is 20 microns, obtain the former medicine recrystallization of diflubenzuron crystal
(2) adopting layer by layer, self-assembly method prepares nano diflubenzuron: 0mg is scattered in the 500 μ L deionized waters with the former medicine recrystallization of the diflubenzuron that obtains crystal 3, adding 1mL concentration is the 1.8mg/mL poly arginine, ultrasonic absorption 10min, through two times centrifugal-removal supernatant-washing-cycle of oscillation, adding 1mL concentration is the 1mg/mL dextran sulfate, and absorption 10min repeats above-mentioned steps, successively adsorb shitosan and sodium alginate, promptly obtain the nano diflubenzuron microcapsules of 7 layers of nucleocapsid structure.
Embodiment 3,
(1) the former medicine crystal recrystallization of diflubenzuron: the former medicine of 0.5g diflubenzuron is dissolved in the 50ml methyl alcohol, magnetic agitation 1h, wait to dissolve the complete instantaneous adding 200mL in back and contain 0.025%m/v hydroxypropyl methylcellulose (HPMC) deionized water, magnetic agitation, use the probe-type ultrasonic to regulate diflubenzuron agricultural chemicals crystal particle diameter size, ultrasonic time is 10 minutes, and particle size is 100 microns, obtain the former medicine recrystallization of diflubenzuron crystal
(2) adopting layer by layer, self-assembly method prepares nano diflubenzuron: 100mg is scattered in the 500 μ L deionized waters with the former medicine recrystallization of the diflubenzuron that obtains crystal, adding 1mL concentration is the 4.5mg/mL cation dextran, ultrasonic absorption 15min, through two times centrifugal-removal supernatant-washing-cycle of oscillation, adding 1mL concentration is the 3mg/mL sodium carboxymethylcellulose, and absorption 15min repeats above-mentioned steps, successively adsorb shitosan and sodium alginate, promptly obtain the nano diflubenzuron microcapsules of 10 layers of nucleocapsid structure.
Claims (5)
1. method for preparing nano diflubenzuron microcapsules is characterized in that:
(1) the former medicine crystal recrystallization of diflubenzuron: the former medicine of 0.1-0.5g diflubenzuron is dissolved in the 50mL organic reagent, magnetic agitation 1h, wait to dissolve the complete instantaneous adding 200mL in back and contain 0.025%m/v hydroxypropyl methylcellulose (HPMC) deionized water, magnetic agitation, use the probe-type ultrasonic to regulate diflubenzuron agricultural chemicals crystal particle diameter size, ultrasonic time is 0～10 minute, and particle size is the 0.1-100 micron, obtain the former medicine recrystallization of diflubenzuron crystal
(2) adopting layer by layer, self-assembly method prepares nano diflubenzuron: 10mg-100mg is scattered in the 500 μ L deionized waters with the former medicine recrystallization of the diflubenzuron that obtains crystal, add 1mL cationic polyelectrolyte chitosan solution 0.5-5mg/mL, ultrasonic absorption 5-15min, through two times centrifugal-removal supernatant-washing-cycle of oscillation, add 1mL anionic polyelectrolyte sodium alginate soln 0.5-5mg/mL, absorption 5-15min, repeat above-mentioned steps, successively adsorb shitosan and sodium alginate, promptly obtain the nano diflubenzuron microcapsules of 5-10 layer nucleocapsid structure.
2. method for preparing nano diflubenzuron microcapsules according to claim 1 is characterized in that: the described recrystallization organic reagent organic solvent that to be isopropyl alcohol, acetone, b propanol, methyl alcohol etc. dissolve each other with water.
3. method for preparing nano diflubenzuron microcapsules according to claim 1 is characterized in that: described polyanion is seaweeds sodium, dextran sulfate, sodium carboxymethylcellulose.
4. method for preparing nano diflubenzuron microcapsules according to claim 1 is characterized in that: described polycation is shitosan, poly arginine, cation dextran.
5. method for preparing nano diflubenzuron microcapsules according to claim 1 is characterized in that: the described polymer number of plies is the 1-20 bilayer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104365595A (en) * | 2014-11-27 | 2015-02-25 | 江南大学 | Pesticide microcapsules produced by layer-by-layer self-assembly |
| CN105032309A (en) * | 2015-07-08 | 2015-11-11 | 北京理工大学 | Microcapsule and preparation method therefor |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0008207A2 (en) * | 1978-08-03 | 1980-02-20 | E.I. Du Pont De Nemours And Company | Insecticidal compositions, and preparation and use thereof |
| WO2000032043A1 (en) * | 1998-12-03 | 2000-06-08 | Ben Gurion University Of The Negev Research And Development Authority | Sustained release polymer-based water insoluble beads |
| CN1491541A (en) * | 2003-09-24 | 2004-04-28 | 河北科技大学 | Pesticide water suspending nano capsule prepn and its preparing method |
| CN1994284A (en) * | 2006-12-14 | 2007-07-11 | 东南大学 | Preparation process of nano drug-loaded biological micro-capsule |
| CN101156854A (en) * | 2007-09-19 | 2008-04-09 | 哈尔滨峰源高科技开发有限公司 | Method for preparing camptothecin medicine slow releasing microcapsule |
| CN101248789A (en) * | 2008-04-17 | 2008-08-27 | 中国农业科学院植物保护研究所 | Preparation of deinsectization carbamide controllable sustained-release nano grain and uses thereof |
-
2009
- 2009-04-23 CN CN200910071865A patent/CN101869115A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0008207A2 (en) * | 1978-08-03 | 1980-02-20 | E.I. Du Pont De Nemours And Company | Insecticidal compositions, and preparation and use thereof |
| WO2000032043A1 (en) * | 1998-12-03 | 2000-06-08 | Ben Gurion University Of The Negev Research And Development Authority | Sustained release polymer-based water insoluble beads |
| CN1491541A (en) * | 2003-09-24 | 2004-04-28 | 河北科技大学 | Pesticide water suspending nano capsule prepn and its preparing method |
| CN1994284A (en) * | 2006-12-14 | 2007-07-11 | 东南大学 | Preparation process of nano drug-loaded biological micro-capsule |
| CN101156854A (en) * | 2007-09-19 | 2008-04-09 | 哈尔滨峰源高科技开发有限公司 | Method for preparing camptothecin medicine slow releasing microcapsule |
| CN101248789A (en) * | 2008-04-17 | 2008-08-27 | 中国农业科学院植物保护研究所 | Preparation of deinsectization carbamide controllable sustained-release nano grain and uses thereof |
Non-Patent Citations (1)
| Title |
|---|
| 叶伟华等: "BU-PHBV纳米粒的制备、逐层自组装包覆及体外释放", 《华南理工大学学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104365595A (en) * | 2014-11-27 | 2015-02-25 | 江南大学 | Pesticide microcapsules produced by layer-by-layer self-assembly |
| CN105032309A (en) * | 2015-07-08 | 2015-11-11 | 北京理工大学 | Microcapsule and preparation method therefor |
| CN105032309B (en) * | 2015-07-08 | 2017-12-12 | 北京理工大学 | A kind of microcapsules and preparation method thereof |
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