CN109874785A - One-step shaping method is prepared using polyethers as the insecticide microcapsules and its continuous producing method of wall material - Google Patents
One-step shaping method is prepared using polyethers as the insecticide microcapsules and its continuous producing method of wall material Download PDFInfo
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- CN109874785A CN109874785A CN201811551135.1A CN201811551135A CN109874785A CN 109874785 A CN109874785 A CN 109874785A CN 201811551135 A CN201811551135 A CN 201811551135A CN 109874785 A CN109874785 A CN 109874785A
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Abstract
One-step shaping method is prepared using polyethers as the insecticide microcapsules and its continuous producing method of wall material, and microcapsules technology field is belonged to.By insecticide core material solution ultrasonic disperse into polyether solutions, separating treatment is after stirring reasonable time up to insecticide microcapsules, after the supplement polyethers of the waste liquid after insecticide microcapsules will be isolated, that is, the aqueous phase solution in the production cycle period as a new round can be recycled.Prepared insecticide microcapsules are verified by extracorporeal releasing experiment, have good slow release effect.
Description
Technical field:
The invention belongs to field of pesticides, and in particular to a kind of one-step shaping method preparation is micro- as the insecticide of wall material using polyethers
Capsule and its continuous producing method.
Background technique:
It is (pulvis, wettable using conventional dosage forms in order to reach ideal control efficiency in the pest control field of agriculture and forestry
Property pulvis, aqua, missible oil etc.) insecticide generally require largely and to be continually administered, so inefficient method of application not only can
The organic solvent in formulation of insecticides, raw medicine and its catabolite is caused to cause serious harm to the mankind and natural environment, and
And it can also accelerate development of the pest to the drug resistance of its effective component.
Microencapsulation technology is will to be used as capsule using natural or synthetic high molecular material as having semi-permeable cyst wall
The active material of core wraps up, and forms a kind of technology of microencapsulation with particular geometric configuration.By microencapsulation technology
Applied to formulation of insecticides field, i.e., preparing protodrug is prepared as insecticide microcapsules, the above conventional pesticides agent can be solved
The problem that type is faced passes through the slow releasing function of the core-shell structure of microcapsules, on the basis of guaranteeing its instant drug effect, Ke Yi great
Width reduces insecticide amount of application, improves the lasting effect of effective component, and by insecticide active ingredient and severe natural environment every
It opens, effectively slows down its degradation process, further decrease the further harm to the mankind and natural environment.
Insecticide microcapsules are developed rapidly in recent years, and become the main path that insecticide minimizing uses, but desinsection
Still there are many problems to need continuous improvement and innovation for agent microcapsule formulation.Formulation of insecticides belongs to inexpensive industry, desinsection
Although the conventional dosage forms production process of agent only needs such as to dissolve, crushes simple basic technology, performance is unable to meet demand.
And the preparation method with commercialized insecticide microcapsules has been delivered at present, mostly by chemistry or ionomer, Electrostatic Absorption
Etc. principles form microcapsules shell, such as sodium alginate and calcium ion crosslinking, melamine and formaldehyde crosslinking, chitosan and polypropylene
Mutual absorption of sour sodium etc., generally requires the items such as the temperature, pH value, ionic strength of strict control system in above-mentioned reaction process
Part, and the equipment for generally requiring special designing, and for these critical conditions and Complicated Flow in large-scale industrial production
Control can undoubtedly reduce production efficiency, improve production cost, thereby reduce business investor to these insecticide microcapsules
The confidence of preparation method market prospects.
The one-step shaping method preparation method of insecticide microcapsules of the present invention is built upon the super of chemistry subject forward position
On the Research foundation in molecular chemistry field, selected amphiphilic diblock copolymer, that is, polyether high molecular is since different blocks are molten
There are difference for solvability in liquid, and insecticide capsule-core table is deposited under the driving of resulting non-covalent bond effect power
Face, spontaneously forms with specific structure and certain thickness shell, and that can be formed after deposition after a period of time, cladding is good
Good insecticide microcapsules.Entire preparation flow is simple, does not need complicated reaction system parameter regulation or temperature-pressure etc..Institute
The polyether high molecular of selection is synthesis high molecular material, and cost is relatively low, quality controllable, steady chemical structure, as wall material institute
Quality and the performance for forming microcapsules are controllable.Prepared insecticide microcapsules are verified by extracorporeal releasing experiment, are had good
Slow release effect.
Summary of the invention:
The present invention provides a kind of preparations of one-step shaping method using polyethers as the insecticide microcapsules and its continuous production of wall material
Method, it is excessively complicated to solve current insecticide microcapsules preparation flow, and production devil liquor recovery Recycling.
In order to solve the above-mentioned technical problem, the technical scheme is that by insecticide core material solution ultrasonic disperse to poly-
In ethereal solution, separating treatment is useless after insecticide microcapsules by isolating up to insecticide microcapsules after stirring reasonable time
After liquid supplements polyethers, that is, the aqueous phase solution in the production cycle period as a new round can be recycled.
Optionally, the preparation method specifically includes the following steps:
Microcapsules preparation: step 1 under ultrasonic treatment and mechanical stirring, the organic solvent solution of insecticide core material is dripped
It is added in the aqueous solution of polyethers, after completion of dropwise addition, keeps the mechanical stirring of a period of time；Gained suspension is passed through into separation of solid and liquid
Obtain microcapsules；
Step 2 supplements raw material: carrying out quantitative analysis by the waste liquid after being separated by solid-liquid separation to step 1, obtains step 1 institute
The polyether quality percentage composition in waste liquid is obtained, and reaches the original concentration of step 1 by calculating the suitable polyethers of supplement；
Continuous production: step 3 repeats the production procedure of step 1, carries out the production cycle period of a new round.
Optionally, the polyethers, as amphiphilic polyether high molecular, the entitled polyoxyethylene polyoxypropylene three block of chemistry
Copolymer, molecular structural formula are H [CH2CH2O]m[CH2CH(CH3)O]n[CH2CH2O]mOH, molecular weight 30000-
2000Da (dalton), preferably 15000-3000Da (dalton)；Its HLB value be 10-60, physical behavior be solid (sheet,
Particle, powder etc.), viscous paste shape, liquid, solution etc.；Active constituent content is with physical behavior in above-mentioned each polyethers raw material
Different and different from；A kind of specifically used mixture for above-mentioned polyethers or a variety of polyethers.
Optionally, the insecticide is carbamate insecticides, dissolves in organic solvent, slightly soluble or not soluble in water,
Raw medicine physical behavior is the solids, preferably arprocarb, Ficam, Mobucin etc. such as sheet, particle, powder.
Optionally, the organic solvent, with water energy mutual phased soln, preferably ethyl alcohol, acetone, butanone etc. in any proportion.
Optionally, in the step 1, mechanical stirring rate is 100-1000rpm, preferably 200-500rpm.
Optionally, in the step 1, ultrasonic frequency is 30~40kHz in ultrasonic treatment.
Optionally, each group distribution ratio is as follows as mass fraction for the raw material of the insecticide microcapsules:
Polyether aqueous solution is that every 1-50 parts of polyethers corresponds to 500-5000 parts of water；The organic solvent solution of insecticide core material is every
1-20 parts of insecticides correspond to 5-300 parts of organic solvents.
Optionally, in the step 1, the volume ratio of the aqueous solution of the organic solvent solution and polyethers of insecticide core material is
1:5~1:30.
Optionally, the methods of centrifugation, filtering, precipitating can be used in the separation of solid and liquid in the step 1.
Optionally, spectrophotometry, efficient liquid phase chromatographic analysis, drying can be used in the quantitative analysis in the step 2
The methods of gravimetric analysis.
Preparation of the invention carries out at room temperature, and the room temperature referred to, this field generally refers to 25 ± 5 DEG C.
Optionally, the described one-step shaping method preparation using polyethers as the insecticide microcapsules of wall material, average grain diameter 1-
50 μm, preferably 1-30 μm.
Optionally, the described one-step shaping method preparation using polyethers as the insecticide microcapsules of wall material, drugloading rate 30%-
95%, preferably 60%-95%.
Optionally, the described one-step shaping method preparation using polyethers as the insecticide microcapsules of wall material, encapsulation rate 50-
95%, preferably 70%-95%.
Technical solution provided by the invention, mainly implements at room temperature, using water as medium, passes through one-step shaping method
Preparation is using polyethers as the insecticide microcapsules of wall material, and by being able to continuously to isolating supplement polyethers in the waste liquid after microcapsules
Production.Process flow overall simple does not need complicated reaction system parameter regulation or temperature-pressure etc..Selected polyethers can
Artificial synthesized according to performance requirement, cost is relatively low, quality controllable, steady chemical structure.Prepared insecticide microcapsules pass through
Extracorporeal releasing experiment verifying, has good slow release effect.Prepared insecticide microcapsules have amphiphilic shell, Ke Yijin
One step compounding is the common new type disinsection agent formulations such as aqueous micro-capsule suspension, wide market.
Specific embodiment
In order to make it easy to understand, illustrating the one-step shaping method preparation using polyethers as the insecticide of wall material below with reference to embodiment
Microcapsules and its continuous producing method, it should be appreciated that these embodiments are merely to illustrate the present invention rather than limitation is of the invention
Range.
Test method as used in the following examples is unless otherwise specified conventional method.Institute in following embodiments
Material, reagent etc., are commercially available unless otherwise specified.Following scores as described in the examples refer both to matter
Measure part.Pfpe molecule structural formula is H [CH2CH2O]m[CH2CH(CH3)O]n[CH2CH2O]mOH。
Embodiment 1:
Step 1, preparation: under 30kHz ultrasonic treatment and 300rpm mechanical stirring, the ethyl alcohol of the Mobucin of 40ml is molten
Liquid (0.1g/ml) is added drop-wise in polyethers (molecular weight 14600Da) aqueous solution (5g/L) of 600ml, after completion of dropwise addition, keeps one
The mechanical stirring of section time.Resulting suspension is obtained into microcapsules by precipitating, partial size is 8 μm, drugloading rate 74%, packet
Envelope rate is 92%, and (straight alcohol dissolution medium, 25 DEG C, 0.1g microcapsules are put into bag filter extracorporeal releasing experiment, are subsequently placed in
In the ethyl alcohol of 300ml, following embodiment is same) measure the t of the Mobucin microcapsules50(the time required to cumulative release amount reaches 50%)
About 2 times of Mobucin raw medicine, t90(the time required to cumulative release amount reaches 90%) is about 2.75 times of Mobucin raw medicine.
Step 2 supplements raw material: the quality by polyethers in the resulting precipitating supernatant of quantitative analysis step 1 is about
1.6g, and be about 1.4g by calculating supplement polyethers.
Continuous production: step 3 repeats the production procedure of step 1, carries out the production cycle period of a new round.
Embodiment 2:
Step 1, preparation: under 30kHz ultrasonic treatment and 400rpm mechanical stirring, the acetone of the Ficam of 30ml is molten
Liquid (0.05g/ml) is added drop-wise in polyethers (molecular weight 5000Da) aqueous solution (4g/L) of 200ml, after completion of dropwise addition, keeps one
The mechanical stirring fixed time.Resulting suspension is obtained into microcapsules by centrifugation, partial size is 15 μm, drugloading rate 93%,
Encapsulation rate is 94%, and extracorporeal releasing experiment (pure acetonitrile dissolution medium, 25 DEG C) measures the t of the Ficam microcapsules50(cumulative release
Amount reaches the time required to 50%) it is about 2.8 times of Ficam raw medicine, t90(the time required to cumulative release amount reaches 90%) about dislikes
2.9 times of worm prestige raw medicine.
Step 2 supplements raw material: the quality by polyethers in the resulting centrifugation waste liquid of quantitative analysis step 1 is about
0.65g, and be about 0.15g by calculating supplement polyethers.
Continuous production: step 3 repeats the production procedure of step 1, carries out the production cycle period of a new round.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment, or some or all of the technical features are equal
Replacement, and these modifications or substitutions, the model for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (10)
1. one-step shaping method is prepared using polyethers as the continuous producing method of the insecticide microcapsules of wall material, which is characterized in that including
Following steps:
Microcapsules preparation: step 1 under ultrasonic treatment and mechanical stirring, the organic solvent solution of insecticide core material is added drop-wise to
In the aqueous solution of polyethers, after completion of dropwise addition, the mechanical stirring of a period of time is kept；Gained suspension is obtained by being separated by solid-liquid separation
Microcapsules；
Step 2 supplements raw material: carrying out quantitative analysis by the waste liquid after being separated by solid-liquid separation to step 1, obtains useless obtained by step 1
Polyether quality percentage composition in liquid, and reach the original concentration of step 1 by calculating the suitable polyethers of supplement；
Continuous production: step 3 repeats the production procedure of step 1, carries out the production cycle period of a new round.
2. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that the polyethers, as amphiphilic polyether high molecular, the entitled polyoxyethylene polyoxypropylene three block of chemistry
Copolymer, molecular structural formula are H [CH2CH2O]m[CH2CH(CH3)O]n[CH2CH2O]mOH, molecular weight 30000-
2000Da (dalton), preferably 15000-3000Da (dalton)；Its HLB value is 10-60, specifically used to gather for above-mentioned one kind
The mixture of ether or a variety of polyethers.
3. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that the insecticide is carbamate insecticides；The insecticide is selected from arprocarb, Ficam, different
Third prestige.
4. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that the organic solvent, for water energy mutual phased soln, preferably ethyl alcohol, acetone, butanone etc. in any proportion.
5. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that in step 1, mechanical stirring rate is 100-1000rpm, preferably 200-500rpm；Surpass in ultrasonic treatment
Frequency of sound wave is 30~40kHz.
6. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that each group distribution ratio is as follows as mass fraction for the raw material of the insecticide microcapsules:
Polyether aqueous solution is that every 1-50 parts of polyethers corresponds to 500-5000 parts of water；The organic solvent solution of insecticide core material is every 1-20
Part insecticide corresponds to 5-300 parts of organic solvents.
7. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that in step 1, the volume ratio of the aqueous solution of the organic solvent solution and polyethers of insecticide core material be 1:5~
1:30。
8. one-step shaping method preparation described in accordance with the claim 1 is using polyethers as the continuous production side of the insecticide microcapsules of wall material
Method, which is characterized in that the separation of solid and liquid in the step 1, using centrifugation, filtering, precipitating method；In the step 2
Quantitative analysis, the method that spectrophotometry, efficient liquid phase chromatographic analysis, dry weight can be used to analyze；Preparation is in room temperature condition
Lower progress.
9. the insecticide microcapsules using polyethers as wall material are prepared according to the described in any item methods of claim 1-8.
10. according to the described in any item methods of claim 1-8 be prepared using polyethers as the insecticide microcapsules of wall material,
It is characterized in that, average grain diameter is 1-50 μm, preferably 1-30 μm；Drugloading rate is 30%-95%, preferably 60%-95%；Encapsulating
Rate is 50-95%, preferably 70%-95%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1957701A (en) * | 2006-10-27 | 2007-05-09 | 陕西上格之路生物科学有限公司 | Insecticide of ivermectin |
| CN101054674A (en) * | 2007-02-08 | 2007-10-17 | 河南师范大学 | Method of preparing hydroxyl nickel oxide by electrolysis and electrolysis bath used for the same |
| CN101732234A (en) * | 2010-01-19 | 2010-06-16 | 山东大学 | Method for preparing block polymer micelle freeze-drying preparation carrying docetaxel |
| CN102836437A (en) * | 2011-06-22 | 2012-12-26 | 中国科学院上海药物研究所 | Docetaxelpolyoxyethelene-polyoxypropylene-polyoxyethelene compound capable of self-assembling into micelle |
| CN103446040A (en) * | 2012-06-04 | 2013-12-18 | 复旦大学 | Docetaxel-coated polymeric micelle and preparation method thereof |
-
2018
- 2018-12-18 CN CN201811551135.1A patent/CN109874785A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1957701A (en) * | 2006-10-27 | 2007-05-09 | 陕西上格之路生物科学有限公司 | Insecticide of ivermectin |
| CN101054674A (en) * | 2007-02-08 | 2007-10-17 | 河南师范大学 | Method of preparing hydroxyl nickel oxide by electrolysis and electrolysis bath used for the same |
| CN101732234A (en) * | 2010-01-19 | 2010-06-16 | 山东大学 | Method for preparing block polymer micelle freeze-drying preparation carrying docetaxel |
| CN102836437A (en) * | 2011-06-22 | 2012-12-26 | 中国科学院上海药物研究所 | Docetaxelpolyoxyethelene-polyoxypropylene-polyoxyethelene compound capable of self-assembling into micelle |
| CN103446040A (en) * | 2012-06-04 | 2013-12-18 | 复旦大学 | Docetaxel-coated polymeric micelle and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 姚日生: "《药用高分子材料》", 31 August 2003 * |
| 梁向峰: "PEO-PPO-PEO嵌段共聚物在水溶液中的自组装行为及其应用", 《化工学报》 * |
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Application publication date: 20190614 |