CN105052923A - Agricultural chemical slow release microspheres based on electrostatic spraying method and preparation method of agricultural chemical slow release microspheres - Google Patents
Agricultural chemical slow release microspheres based on electrostatic spraying method and preparation method of agricultural chemical slow release microspheres Download PDFInfo
- Publication number
- CN105052923A CN105052923A CN201510481181.9A CN201510481181A CN105052923A CN 105052923 A CN105052923 A CN 105052923A CN 201510481181 A CN201510481181 A CN 201510481181A CN 105052923 A CN105052923 A CN 105052923A
- Authority
- CN
- China
- Prior art keywords
- electrostatic spraying
- preparation
- slow release
- microspheres
- agricultural chemical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses agricultural chemical slow release microspheres based on an electrostatic spraying method and a preparation method of the agricultural chemical slow release microspheres. The method comprises the following steps of: (1) adding cellulose acetate (CA) in a mixed solvent of acetone and dimethyl formamide until the cellulose acetate is completely dissolved under the condition of water bath; and (2) adding effective ingredients of agricultural chemicals to a mixed system obtained in the step (1), stirring the effective ingredients and the mixed system until the effective ingredients and the mixed system are dissolved, and then performing electrostatic spraying so as to prepare drug loading microspheres. The agricultural chemical slow release microspheres and the preparation method thereof disclosed by the invention have the following advantages that the drug loading capacity of the microspheres is high, drugs do not loss basically, and the agricultural chemical slow release microspheres are economical and environment-friendly. The carrier of the microspheres is CA rather than a polymeric material with a long degrading period, so that the environmentally friendly performance of a pesticide formulation is improved; the preparation method of the microspheres is simple, the yield is high, the operation process is simple, requirements for equipment are low, and the method is wide in applicable range. The preparation method is suitable for all oil soluble drugs except tebuconazole used as a model drug mentioned in the method.
Description
Technical field
The invention belongs to technical field of pesticide, be specifically related to a kind of pesticide slow-release microballoon based on method of electrostatic spraying and preparation method thereof.
Background technology
Chemical control is the main method of crop diseases and pest prevention and control of weeds, plays an important role in agricultural production, but agricultural chemicals use problems such as also bringing such as residue of pesticide, environmental pollution and pesticide resistance in a large number.In the today greatly developing pollution-less agriculture, and do not mean that the use repelling agricultural chemicals, but agricultural chemicals is had higher requirement.The shortcomings such as the active ingredient rate of release of agricultural chemicals regular dosage form is too fast, duration of efficacy is short, accumulative dosage is large, not only cause waste economically, and cause great pollution to environment.Therefore, need to develop low toxicity, efficient, lasting sustained-release pesticides preparation as early as possible, overcome the shortcoming of traditional pesticidal preparations, improve the availability of agricultural chemicals, reach the object of economy, safety, effectively control pest.
Agricultural chemicals drug bearing microsphere is that former medicine is mixed in the complex microsphere formed in carrier macromolecular material network, and drug bearing microsphere not only can strengthen the duration of efficacy being wrapped medicine, and can strengthen the stability of medicine.Slow releasing carrier material can select synthetic material or natural macromolecular material.Cellulose acetate (CA) is as the representative in natural macromolecular material-cellulose material, have pliable and tough, transparent, good luster, melt fluidity are good, easy-formation processing and the feature such as thermoplasticity, therefore have broad application prospects, become an extremely potential branch in biodegradation material.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of pesticide slow-release microballoon based on method of electrostatic spraying and preparation method thereof.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
Based on a preparation method for the pesticide slow-release microballoon of method of electrostatic spraying, it comprises the steps:
(1) added by cellulose acetate in the mixed solvent of acetone and dimethyl formamide, water bath condition is dissolved completely down to cellulose acetate;
(2) pesticide active ingredient being added step (1) obtains in mixed system, carries out electrostatic spraying and obtain drug bearing microsphere after stirring and dissolving.
In step (1), the volume ratio of acetone and dimethyl formamide is 1:1 ~ 2:1, preferred 2:1.
In step (1), add that quality is mixed solvent gross mass 2 ~ 4% of cellulose acetate, preferably 4%.
In step (1), bath temperature is 50 ~ 60 DEG C, preferably 60 DEG C, and water bath time is 2 ~ 4 hours, preferably 2 hours.
In step (2), described pesticide active ingredient is Tebuconazole.
In step (2), the addition of Tebuconazole is 20 ~ 50% of cellulose acetate quality.
In step (2), electrostatic spraying condition is: solution being sucked internal diameter is in the syringe of 1 ~ 1.5mm (preferred 1.07mm) syringe needle, voltage is 20 ~ 25kV (preferred 25kV), masking foil makees receiver, distance between needle point and receiver is 10 ~ 15cm (preferred 15cm), syringe pump coutroi velocity, at 1 ~ 1.5ml/h (preferred 1ml/h), carries out electrostatic spraying.
The pesticide slow-release microballoon prepared by said method is also within protection scope of the present invention.Sustained-release micro-spheres structure is characterized by SEM, and by simulation release experiment and bacteriostatic experiment, the slow-release function that checking drug bearing microsphere is good and antibacterial effect.
Beneficial effect: the present invention compared with prior art has following advantage:
(1) microballoon drugloading rate is higher, can reach 50%, and medicine does not run off substantially, economic environmental protection.
(2) carrier of microballoon is CA, but not the polymeric material that degradation cycle is longer, improve the environment friendly of pesticidal preparations.
(3) method for preparing microsphere is simple, output is high, and operating process is simple, low for equipment requirements.
(4) to be applicable to scope wide for method.Be except model drug with Tebuconazole except what mention in patent of the present invention, all applicable to this method of other oil-soluble medicine.
Accompanying drawing explanation
Fig. 1 is drugloading rate is that 20% (mass content) Tebuconazole/CA complex microsphere SEM schemes.
Fig. 2 is the drug release patterns figure of drugloading rate 20% (mass content) Tebuconazole/CA complex microsphere.
Fig. 3 is the antibacterial experiment figure of drugloading rate 20% (mass content) Tebuconazole/CA complex microsphere.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Following examples reagent and source: 95% Original Tebuconazole (tebuconazole), Jiangsu Qi Zhou green chemical industry limited company, absolute ethyl alcohol (reagent Co., Ltd of traditional Chinese medicines group), cellulose acetate CA (in conjunction with acetic acid 54.5-56%), Chemical Reagent Co., Ltd., Sinopharm Group; Acetone, DMF (DMF) (Nanjing Chemistry Reagent Co., Ltd.).SEM (SEM) (JSM-7600F), Jeol Ltd., ultraviolet-visible spectrophotometer (UV-2450, Shimadzu), thermogravimetric analysis (German Nai Chi instrument company).
Embodiment 1:
Using Tebuconazole as model drug, measure 10ml acetone and 5mlDMF reagent, weigh after mixing, add the 4%CA of mixed solution gross mass again, water-bath 60 DEG C of 2h add Tebuconazole (20% of CA quality) after dissolving completely, electrostatic spraying is carried out after stirring and dissolving, solution being sucked internal diameter is in the syringe of 1.07mm syringe needle, voltage is 25kV, masking foil makees receiver, distance between needle point and receiver is 15cm, and syringe pump coutroi velocity, at 1ml/h, carries out electrostatic spraying and obtains drug bearing microsphere.
Embodiment 2:
Using Tebuconazole as model drug, measure 10ml acetone and 5mlDMF reagent, weigh after mixing, add the 4%CA of mixed solution gross mass again, water-bath 60 DEG C of 2h add Tebuconazole (50% of CA quality) after dissolving completely, electrostatic spraying is carried out after stirring and dissolving, solution being sucked internal diameter is in the syringe of 1.07mm syringe needle, voltage is 25kV, masking foil makees receiver, distance between needle point and receiver is 15cm, and syringe pump coutroi velocity, at 1ml/h, carries out electrostatic spraying and obtains drug bearing microsphere.
Embodiment 3:
Slowly-releasing assay method:
Take 0.1000g and carry Tebuconazole microballoon, put in tubular bag filter, two ends are lived with dialysis clamp sub-folder, be suspended in that to contain volume fraction containing 400mL be in the wide-mouth bottle of the ethanol water of 50%, magnetic agitation is carried out under room temperature, 5ml liquid is taken out in timing, and supplements with same amount liquid, and total liquid volume is remained unchanged.Measure the content of Tebuconazole in solution with ultraviolet-visible spectrophotometer, draw Tebuconazole change curve in time, and compared with the stripping curve of Original Tebuconazole, characterize slow release effect.
Test result analysis:
Tebuconazole/CA complex microsphere the SEM of Fig. 1 to be drugloading rate be 20% (mass content) schemes, and as can be seen from the figure Microsphere Size is homogeneous, and structure is obvious.Outer surface has some collapsed configuration, mainly due in electrostatic spray process, the evaporation rate of solvent quickly, and the migration velocity of polymer segment is relatively slow, therefore after the volatilization of microparticle surfaces solvent, a relatively fine and close shell will be formed, after the solvent volatilization of interparticle, interparticle forms hole, shrink after polymer segment is desolvated and form random coil closely, macroscopically just show as the microballoon subsided, this phenomenon can weaken along with the increase of polymer concentration in solution.
The release profiles of Tebuconazole/CA complex microsphere in 50% (v/v) ethanol/water solution of Fig. 2 to be drugloading rate be 20% (mass content).Can find out, former medicine and sustained release agent in the release of beginning a period of time comparatively rapidly, become slow afterwards, finally reach balance.Carry Tebuconazole microballoon close balance in delivery systme after 24h, calculate according to theoretical drugloading rate, release rate reaches 40%, and the visible Tebuconazole microballoon that carries has good slow release effect.
The antibacterial experiment of Fig. 3 to be drugloading rate be Tebuconazole/CA complex microsphere of 20% (mass content).What experiment adopted is Candida albicans, by containing the microballoon EFI of 0%, 20% Tebuconazole at diameter be respectively 1cm circular filter paper on, 37 DEG C cultivate 24h after observe.As can be seen from Fig., carry Tebuconazole microballoon and have obvious fungistatic effect.
Claims (8)
1., based on a preparation method for the pesticide slow-release microballoon of method of electrostatic spraying, it is characterized in that, it comprises the steps:
(1) added by cellulose acetate in the mixed solvent of acetone and dimethyl formamide, water bath condition is dissolved completely down to cellulose acetate;
(2) pesticide active ingredient being added step (1) obtains in mixed system, carries out electrostatic spraying and obtain drug bearing microsphere after stirring and dissolving.
2. the preparation method of the pesticide slow-release microballoon based on method of electrostatic spraying according to claim 1, is characterized in that, in step (1), the volume ratio of acetone and dimethyl formamide is 1:1 ~ 2:1.
3. the preparation method of the pesticide slow-release microballoon based on method of electrostatic spraying according to claim 1, is characterized in that, in step (1), and add that quality is mixed solvent gross mass 2 ~ 4% of cellulose acetate.
4. the preparation method of the pesticide slow-release microballoon based on method of electrostatic spraying according to claim 1, is characterized in that, in step (1), bath temperature is 50 ~ 60 DEG C, and water bath time is 2 ~ 4 hours.
5. the preparation method of the pesticide slow-release microballoon based on method of electrostatic spraying according to claim 1, is characterized in that, in step (2), described pesticide active ingredient is Tebuconazole.
6. the preparation method of the pesticide slow-release microballoon based on method of electrostatic spraying according to claim 1, is characterized in that, in step (2), the addition of Tebuconazole is 20 ~ 50% of cellulose acetate quality.
7. the preparation method of the pesticide slow-release microballoon based on method of electrostatic spraying according to claim 1, it is characterized in that, in step (2), electrostatic spraying condition is: solution being sucked internal diameter is in the syringe of 1 ~ 1.5mm syringe needle, voltage is 20 ~ 25kV, and masking foil makees receiver, and the distance between needle point and receiver is 10 ~ 15cm, syringe pump coutroi velocity, at 1 ~ 1.5mL/h, carries out electrostatic spraying.
8. the pesticide slow-release microballoon that in claim 1 ~ 7, any one method prepares.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510481181.9A CN105052923A (en) | 2015-08-07 | 2015-08-07 | Agricultural chemical slow release microspheres based on electrostatic spraying method and preparation method of agricultural chemical slow release microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510481181.9A CN105052923A (en) | 2015-08-07 | 2015-08-07 | Agricultural chemical slow release microspheres based on electrostatic spraying method and preparation method of agricultural chemical slow release microspheres |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105052923A true CN105052923A (en) | 2015-11-18 |
Family
ID=54482659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510481181.9A Pending CN105052923A (en) | 2015-08-07 | 2015-08-07 | Agricultural chemical slow release microspheres based on electrostatic spraying method and preparation method of agricultural chemical slow release microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105052923A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114271267A (en) * | 2021-12-06 | 2022-04-05 | 盐城工学院 | Pesticide delivery system and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921410A (en) * | 2010-09-16 | 2010-12-22 | 武汉工程大学 | Method for preparing cellulose microspheres |
| CN102226301A (en) * | 2011-04-28 | 2011-10-26 | 东北林业大学 | Preparation method of pesticide supported superfine fiber |
| CN102335144A (en) * | 2011-09-28 | 2012-02-01 | 广东榕泰实业股份有限公司 | Preparation method of poly (phenoxy) phosphazene microspheres |
| CN103636598A (en) * | 2013-12-18 | 2014-03-19 | 南京林业大学 | Tebuconazole nano controlled release preparation and preparation method thereof |
-
2015
- 2015-08-07 CN CN201510481181.9A patent/CN105052923A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921410A (en) * | 2010-09-16 | 2010-12-22 | 武汉工程大学 | Method for preparing cellulose microspheres |
| CN102226301A (en) * | 2011-04-28 | 2011-10-26 | 东北林业大学 | Preparation method of pesticide supported superfine fiber |
| CN102335144A (en) * | 2011-09-28 | 2012-02-01 | 广东榕泰实业股份有限公司 | Preparation method of poly (phenoxy) phosphazene microspheres |
| CN103636598A (en) * | 2013-12-18 | 2014-03-19 | 南京林业大学 | Tebuconazole nano controlled release preparation and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 于宾等: "静电纺醋酸纳米纤维及其应用研究现状", 《产业用纺织品总》 * |
| 吴海燕等: "可生物降解型载药微球的研究进展", 《国外丝绸》 * |
| 张春雪等: "静电喷射法制备聚合物微球和微粒", 《材料导报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114271267A (en) * | 2021-12-06 | 2022-04-05 | 盐城工学院 | Pesticide delivery system and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Construction of a controlled-release delivery system for pesticides using biodegradable PLA-based microcapsules | |
| Horuz et al. | Nanoencapsulation of carotenoids extracted from tomato peels into zein fibers by electrospinning | |
| Rai et al. | Eudragit-coated dextran microspheres of 5-fluorouracil for site-specific delivery to colon | |
| CN102070895B (en) | Core-shell microcapsule and preparation method thereof | |
| CN107279174B (en) | Preparation method of efficient cyhalothrin nano pesticide | |
| CN103599090A (en) | Multi-layer drug sustain-release nano fiber membrane and preparation method thereof | |
| CN104273522A (en) | Curcumin nanor compound and preparation method thereof | |
| CN102232921A (en) | Technique for preparing rod-like sustained-release preparation by using blending-modified corn zein as skeleton material and preparation prepared by technique | |
| CN101416631A (en) | Functional slow-release suspension seed-coating agents | |
| CN110973152A (en) | High-efficiency cypermethrin nano water aqua and preparation method and application thereof | |
| CN110476967A (en) | A kind of pesticide slow-release granule prevention and treatment Spodopterafrugiperda new method | |
| CN102961368B (en) | Curcumin nanosuspension and preparation method thereof | |
| CN102870771A (en) | Imidacloprid missible oil pesticide | |
| CN105052923A (en) | Agricultural chemical slow release microspheres based on electrostatic spraying method and preparation method of agricultural chemical slow release microspheres | |
| CN103081939A (en) | Methylamino abamectin benzoate/indoxacarb oil suspension and preparation method thereof | |
| CN101194616A (en) | Preparation of avermectin medicament sustained-release nano microsphere preparations and uses thereof | |
| CN103907643B (en) | A kind of Multifunctional environment friendly Acetamiprid water preparation and preparation method thereof | |
| CN103238590A (en) | Solvent composition for preparing neonicotinoid pesticide liquid preparation | |
| CN107484756A (en) | Aviation plant protection special assistant and preparation method and application | |
| CN105284827A (en) | Clomazone-containing microcapsule suspending agent and preparation method thereof | |
| CN107027746A (en) | A kind of slow-release pesticide microemulsion and preparation method thereof | |
| CN104083324B (en) | Veterinary suspoemulsion containing rifaximin as well as preparation method and application thereof | |
| CN105250236A (en) | Preparation method for catechin preparation for fish | |
| CN105230612A (en) | Chlorpyrifos composite microsphere | |
| CN104264372A (en) | Method for preparing PNIPAAm (poly(N-isopropylacrylamide)) and EC (ethyecellulose) blended nano-fiber membrane by electrostatic spinning |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination |