CN101869112A - Method for preparing controlled photodegradable nano avermectins microcapsules - Google Patents
Method for preparing controlled photodegradable nano avermectins microcapsules Download PDFInfo
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- CN101869112A CN101869112A CN200910071866A CN200910071866A CN101869112A CN 101869112 A CN101869112 A CN 101869112A CN 200910071866 A CN200910071866 A CN 200910071866A CN 200910071866 A CN200910071866 A CN 200910071866A CN 101869112 A CN101869112 A CN 101869112A
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- avermectin
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Abstract
The invention relates to a method for preparing controlled photodegradable nano avermectins microcapsules, which is characterized by (1) re-separating out the raw pesticide in the form of crystals and adjusting the particle size by a probe-type ultrasonic method or a vibration method, (2) using avermectins 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 imidacloprid, thus obtaining the avermectins microcapsules, and (3) using W and Ag+ to adjust the photodegradable activity of TiO2. An appropriate nano photocatalyst is selected according to the actual demand to prepare the photodegradable nano imidacloprid. 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 method for preparing controlled photodegradable nano avermectins microcapsules.
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 that a kind of selectivity is strong, efficient is high, free of contamination method for preparing controlled photodegradable nano avermectins microcapsules.
In order to achieve the above object, the technical solution used in the present invention is:
(1) the former medicine crystal recrystallization of Avermectin: the former medicine of 0.1-1g Avermectin 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 imidacloprid pesticide 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 Avermectin crystal
(2) adopting layer by layer, self-assembly method prepares nano-avermectin: the former medicine recrystallization of the AVM that obtains crystal 10mg-100mg is scattered in the 500 μ L deionized waters; Adding 1mL concentration is 0.5-5mg/mL cationic polyelectrolyte chitosan solution; 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 avermectins microcapsules of 5-10 layer nucleocapsid structure
(3) preparation of light degradation carrier: with the Ti (SO of concentration
4)
2Pass through hydrolysis, condense, add steps acquisition nano-TiOs such as crystal seed and roasting
2Regulate the pH value, at TiO
2In the aqueous solution, adding volumetric concentration is the AgNO of 0.01-0.05mol/L
3Solution feeds H
2Reduction Ag
+Ion makes Ag/TiO
2, nano-TiO
2Na with 2-4g
2WO
42H
2O mixes and adds in the 100mL distilled water, makes mixed solution, after magnetic stirrer stirs 0.1h-1h, and HIGH PRESSURE TREATMENT, drying sample obtains W/TiO
2Photochemical catalyst is mixed with nano-avermectin, and absorption obtains the light degradation nano-avermectin.
The described recrystallization organic reagent organic solvent that to be acetone, ethanol, 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 1-30 bilayer.
Advantage of the present invention is:
(1) envelop rate and the medicine carrying amount of avermectin microcapsule have been improved;
(2) the insect midgut location absorbs Avermectin;
(3) the Avermectin rate of release can be by the THICKNESS CONTROL of cyst wall;
(4) W, Ag decorated nanometer photochemical catalyst TiO
2Photocatalytic activity is strong;
(5) cyst material of microcapsules is a natural macromolecular material, cheap and environmental sound;
(6) 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;
(7) selectivity of the present invention is strong, efficient is high, cost is low, pollution-free, to the person poultry harmless.
Description of drawings
Fig. 1 the present invention coats the avermectin microcapsule laser co-focusing picture of 5 bilayers (CHI/ALG);
Fig. 2 is the avermectin microcapsule scanning electron microscope diagram sheet that invention coats 10 bilayers (CHI/ALG);
Fig. 3 is the potential change figure in the avermectin microcapsule preparation process of the present invention;
Fig. 4 is a slow release effect comparison diagram of the present invention;
Fig. 5 is TiO of the present invention
2The scanning electron microscope diagram sheet;
Fig. 6 is Ag of the present invention
+The TiO that modifies
2The scanning electron microscope diagram sheet;
Fig. 7 is the TiO that W of the present invention modifies
2The scanning electron microscope diagram sheet;
Fig. 8 is the different photochemical catalysts of the present invention degradation property comparison diagrams under ultraviolet light;
Fig. 9 is the different photochemical catalysts of the present invention degradation property comparison diagrams under natural daylight;
Figure 10 is 50%W/TiO of the present invention
2The scanning electron microscope diagram sheet of-Imidacloprid.
The surface characteristic of table 1 light degradation carrier.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described in further detail.
(1) the former medicine crystal recrystallization of Avermectin: the former medicine of 0.1g Avermectin 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 imidacloprid pesticide crystal particle diameter size, ultrasonic time is 3 minutes, and particle size is 0.1 micron, obtain the former medicine recrystallization of Avermectin crystal
(2) adopting layer by layer, self-assembly method prepares nano-avermectin: 10mg is scattered in the 500 μ L deionized waters with the former medicine recrystallization of the Avermectin 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, absorption 5min, repeat above-mentioned steps, successively adsorb shitosan and sodium alginate, promptly obtain the nano avermectins microcapsules of 5 layers of nucleocapsid structure
(3) preparation of light degradation carrier: with the Ti (SO of concentration
4)
2Pass through hydrolysis, condense, add steps acquisition nano-TiOs such as crystal seed and roasting
2Regulate the pH value, at TiO
2In the aqueous solution, adding volumetric concentration is the AgNO of 0.01mol/L
3Solution feeds H
2Reduction Ag
+Ion makes Ag/TiO
2, nano-TiO
2Na with 2-4g
2WO
42H
2O mixes and adds in the 100mL distilled water, makes mixed solution, after magnetic stirrer stirs 0.1h, and HIGH PRESSURE TREATMENT, drying sample obtains W/TiO
2Photochemical catalyst is mixed with nano-avermectin, and absorption obtains the light degradation nano-avermectin.
(1) the former medicine crystal recrystallization of Avermectin: the former medicine of 0.5g Avermectin is dissolved in the 50ml ethanol, 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 imidacloprid pesticide crystal particle diameter size, ultrasonic time is 5 minutes, and particle size is 0.5 micron, obtain the former medicine recrystallization of Avermectin crystal
(2) adopting layer by layer, self-assembly method prepares nano-avermectin: 0mg is scattered in the 500 μ L deionized waters with the former medicine recrystallization of the Avermectin that obtains crystal 2, 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, absorption 10min, repeat above-mentioned steps, successively adsorb shitosan and sodium alginate, promptly obtain the nano avermectins microcapsules of 7 layers of nucleocapsid structure
(3) preparation of light degradation carrier: with the Ti (SO of concentration
4)
2Pass through hydrolysis, condense, add steps acquisition nano-TiOs such as crystal seed and roasting
2Regulate the pH value, at TiO
2In the aqueous solution, adding volumetric concentration is the AgNO of 0.03mol/L
3Solution feeds H
2Reduction Ag
+Ion makes Ag/TiO
2, nano-TiO
2Na with 2-4g
2WO
42H
2O mixes and adds in the 100mL distilled water, makes mixed solution, after magnetic stirrer stirs 0.5h, and HIGH PRESSURE TREATMENT, drying sample obtains W/TiO
2Photochemical catalyst is mixed with nano-avermectin, and absorption obtains the light degradation nano-avermectin.
Embodiment 3,
(1) the former medicine crystal recrystallization of Avermectin: the former medicine of 1g Avermectin 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 imidacloprid pesticide crystal particle diameter size, ultrasonic time is 10 minutes, and particle size is 100 microns, obtain the former medicine recrystallization of Avermectin crystal
(2) adopting layer by layer, self-assembly method prepares nano-avermectin: the former medicine recrystallization of the AVM that obtains crystal 100mg is scattered in the 500 μ L deionized waters; Adding 1mL concentration is the 4.5mg/mL cation dextran; Ultrasonic absorption 15min; Through twice centrifugal-removal supernatant-washing-cycle of oscillation; Adding 1mL concentration is the 3mg/mL sodium carboxymethylcellulose; Absorption 15min; Repeat above-mentioned steps; Successively adsorb shitosan and sodium alginate; Namely obtain the nano avermectins microcapsules of 10 layers of nucleocapsid structure
(3) preparation of light degradation carrier: with the Ti (SO of concentration
4)
2Pass through hydrolysis, condense, add steps acquisition nano-TiOs such as crystal seed and roasting
2Regulate the pH value, at TiO
2In the aqueous solution, adding volumetric concentration is the AgNO of 0.05mol/L
3Solution feeds H
2Reduction Ag
+Ion makes Ag/TiO
2, nano-TiO
2Na with 2-4g
2WO
42H
2O mixes and adds in the 100mL distilled water, makes mixed solution, after magnetic stirrer stirs 1h, and HIGH PRESSURE TREATMENT, drying sample obtains W/TiO
2Photochemical catalyst is mixed with nano-avermectin, and absorption obtains the light degradation nano-avermectin.
Claims (5)
1. method for preparing controlled photodegradable nano avermectins microcapsules is characterized in that:
(1) the former medicine crystal recrystallization of Avermectin: the former medicine of 0.1-1g Avermectin 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 imidacloprid pesticide 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 Avermectin crystal
(2) adopting layer by layer, self-assembly method prepares nano-avermectin: the former medicine recrystallization of the AVM 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 avermectins microcapsules of 5-10 layer nucleocapsid structure
(3) preparation of light degradation carrier: with the Ti (SO of concentration
4)
2Pass through hydrolysis, condense, add steps acquisition nano-TiOs such as crystal seed and roasting
2Regulate the pH value, at TiO
2In the aqueous solution, adding volumetric concentration is the AgNO of 0.01-0.05mol/L
3Solution feeds H
2Reduction Ag
+Ion makes Ag/TiO
2, nano-TiO
2Na with 2-4g
2WO
42H
2O mixes and adds in the 100mL distilled water, makes mixed solution, after magnetic stirrer stirs 0.1h-1h, and HIGH PRESSURE TREATMENT, drying sample obtains W/TiO
2Photochemical catalyst is mixed with nano-avermectin, and absorption obtains the light degradation nano-avermectin.
2. method for preparing controlled photodegradable nano avermectins microcapsules according to claim 1 is characterized in that: the described recrystallization organic reagent organic solvent that to be acetone, ethanol, methyl alcohol etc. dissolve each other with water.
3. method for preparing controlled photodegradable nano avermectins microcapsules according to claim 1 is characterized in that: described polyanion is seaweeds sodium, dextran sulfate, sodium carboxymethylcellulose.
4. method for preparing controlled photodegradable nano avermectins microcapsules according to claim 1 is characterized in that: described polycation is shitosan, poly arginine, cation dextran.
5. method for preparing controlled photodegradable nano avermectins microcapsules according to claim 1 is characterized in that: the described polymer number of plies is the 1-30 bilayer.
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| CN200910071866A CN101869112A (en) | 2009-04-23 | 2009-04-23 | Method for preparing controlled photodegradable nano avermectins microcapsules |
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Cited By (15)
| 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 |
| CN105815327A (en) * | 2016-04-27 | 2016-08-03 | 贺州学院 | Nanometer titanium dioxide silver-doped composite abamectin pesticide and preparation method |
| CN105831156A (en) * | 2016-04-27 | 2016-08-10 | 贺州学院 | Nano titanium dioxide doped silver compound triazophos pesticide and preparation method thereof |
| CN105851051A (en) * | 2016-04-27 | 2016-08-17 | 贺州学院 | Nano titanium dioxide silver-doped compound chlorpyrifos pesticide and preparation method thereof |
| CN105918313A (en) * | 2016-04-27 | 2016-09-07 | 贺州学院 | Silver-doped nanometer titanium dioxide composite acetamiprid pesticide and preparation method thereof |
| CN105918342A (en) * | 2016-04-27 | 2016-09-07 | 贺州学院 | Silver-doped nanometer titanium dioxide composite cypermethrin pesticide and preparation method thereof |
| CN107114385A (en) * | 2017-07-03 | 2017-09-01 | 安徽省鸿鑫生物科技有限公司 | A kind of composition pesticide |
| CN108014790A (en) * | 2016-01-29 | 2018-05-11 | 孙雪妮 | Based on Ag/TiO2The real-time liquid phase adsorption sulfur method of photocatalysis |
| CN109769803A (en) * | 2017-11-14 | 2019-05-21 | 北京纳威克生物科技开发有限公司 | A kind of pesticide polyelectrolyte nano-micelle and preparation method thereof |
| CN109832266A (en) * | 2019-04-15 | 2019-06-04 | 连云港秀景园林绿化工程有限公司 | A kind of insecticide Nano capsule and its preparation process for preventing and treating insect pest of the fruit tree |
| CN110720454A (en) * | 2019-11-01 | 2020-01-24 | 江苏省农业科学院 | Photolysis-resistant nano pesticide and preparation method thereof |
| CN110907654A (en) * | 2019-12-10 | 2020-03-24 | 宁波奥丞生物科技有限公司 | Free estriol quantitative detection kit and preparation method thereof |
| CN111557907A (en) * | 2020-06-22 | 2020-08-21 | 济宁润物生物科技有限公司 | Method for preparing chitosan and abamectin suspension by using dispersion method |
| CN112826825A (en) * | 2021-02-09 | 2021-05-25 | 杭州市农业科学研究院 | Environment-friendly fishery avermectin sustained-release preparation and preparation method and application thereof |
| CN116869012A (en) * | 2022-06-24 | 2023-10-13 | 贵州大学 | Illumination controlled release avermectin microcapsule pesticide and preparation method thereof |
-
2009
- 2009-04-23 CN CN200910071866A patent/CN101869112A/en active Pending
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| CN104365595A (en) * | 2014-11-27 | 2015-02-25 | 江南大学 | Pesticide microcapsules produced by layer-by-layer self-assembly |
| CN108014790B (en) * | 2016-01-29 | 2020-11-17 | 孙雪妮 | Based on Ag/TiO2Photocatalytic real-time liquid phase adsorption desulfurization method |
| CN108014790A (en) * | 2016-01-29 | 2018-05-11 | 孙雪妮 | Based on Ag/TiO2The real-time liquid phase adsorption sulfur method of photocatalysis |
| CN105815327A (en) * | 2016-04-27 | 2016-08-03 | 贺州学院 | Nanometer titanium dioxide silver-doped composite abamectin pesticide and preparation method |
| CN105831156A (en) * | 2016-04-27 | 2016-08-10 | 贺州学院 | Nano titanium dioxide doped silver compound triazophos pesticide and preparation method thereof |
| CN105851051A (en) * | 2016-04-27 | 2016-08-17 | 贺州学院 | Nano titanium dioxide silver-doped compound chlorpyrifos pesticide and preparation method thereof |
| CN105918313A (en) * | 2016-04-27 | 2016-09-07 | 贺州学院 | Silver-doped nanometer titanium dioxide composite acetamiprid pesticide and preparation method thereof |
| CN105918342A (en) * | 2016-04-27 | 2016-09-07 | 贺州学院 | Silver-doped nanometer titanium dioxide composite cypermethrin pesticide and preparation method thereof |
| CN107114385A (en) * | 2017-07-03 | 2017-09-01 | 安徽省鸿鑫生物科技有限公司 | A kind of composition pesticide |
| CN109769803A (en) * | 2017-11-14 | 2019-05-21 | 北京纳威克生物科技开发有限公司 | A kind of pesticide polyelectrolyte nano-micelle and preparation method thereof |
| CN109832266A (en) * | 2019-04-15 | 2019-06-04 | 连云港秀景园林绿化工程有限公司 | A kind of insecticide Nano capsule and its preparation process for preventing and treating insect pest of the fruit tree |
| CN110720454A (en) * | 2019-11-01 | 2020-01-24 | 江苏省农业科学院 | Photolysis-resistant nano pesticide and preparation method thereof |
| CN110907654A (en) * | 2019-12-10 | 2020-03-24 | 宁波奥丞生物科技有限公司 | Free estriol quantitative detection kit and preparation method thereof |
| CN111557907A (en) * | 2020-06-22 | 2020-08-21 | 济宁润物生物科技有限公司 | Method for preparing chitosan and abamectin suspension by using dispersion method |
| CN112826825A (en) * | 2021-02-09 | 2021-05-25 | 杭州市农业科学研究院 | Environment-friendly fishery avermectin sustained-release preparation and preparation method and application thereof |
| CN116869012A (en) * | 2022-06-24 | 2023-10-13 | 贵州大学 | Illumination controlled release avermectin microcapsule pesticide and preparation method thereof |
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Application publication date: 20101027 |