CN106496609A - The preparation method of polyvinyl alcohol microparticles - Google Patents
The preparation method of polyvinyl alcohol microparticles Download PDFInfo
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- CN106496609A CN106496609A CN201611064644.2A CN201611064644A CN106496609A CN 106496609 A CN106496609 A CN 106496609A CN 201611064644 A CN201611064644 A CN 201611064644A CN 106496609 A CN106496609 A CN 106496609A
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- polyvinyl alcohol
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- 30min
- stirring
- alcohol microparticles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/14—Powdering or granulating by precipitation from solutions
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/242—Applying crosslinking or accelerating agent onto compounding ingredients such as fillers, reinforcements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention discloses a kind of preparation method of polyvinyl alcohol microparticles, comprises the steps of：Polyvinyl alcohol is dissolved in deionized water, stands 30min, then heat to 80 DEG C, stir 30min；Add in the vegetable oil containing sorbitan trioleate, 30min is stirred at 60 80 DEG C；Add glutaraldehyde, after stirring 10 min, add Arlacel-80, persistently after stirring 1h, ultrasonically treated, centrifugation is precipitated, and 3 times are respectively washed with acetone, deionized water water, finally cleaned with acetone again 3 times, and products therefrom is vacuum dried, obtain white powder and be polyvinyl alcohol microparticles.The present invention is simple to operate, and the microspherulite diameter distribution for preparing is homogeneous, and, at 15 45 μm, form is completely smooth for average grain diameter, good dispersion.
Description
Technical field
The invention belongs to the preparation field of biomaterial, and in particular to a kind of preparation method of polyvinyl alcohol microparticles.
Background technology
Polyvinyl alcohol (PVA) is a kind of water soluble polymer of people T synthesis, because of good forming ability, nontoxic, biocompatibility
Good, biodegradable and be used for the biomedical sector mouth such as cartilage, artificial cornea, medicament slow release.However, grinding from both domestic and external
From the point of view of studying carefully present situation, at present for the research of the material is confined to form that PVA is made aquagel membrane mostly, then evaluating
Its feasibility as artificial articular cartilage material.Conversely, for the research of the PVA materials of other forms relatively fewer, this
Material application in biomedical sector is limited significantly certainly will.
Compared with the material of the forms such as hydrogel, porous support, film, fiber, coating, micro-sphere material have granularity little,
Unique advantages such as specific surface area is big, good fluidity, if distribute it to can be made into the artificial Bone Defect Repari of injection-type in cushioning liquid
Material.In addition, microballoon have in terms of insoluble drug release low toxicity, efficiently, sustained release, the characteristic such as long-acting, become at present growth factor,
The ideal carrier of antibiotic, cancer therapy drug etc..But, the preparation method of current polyvinyl alcohol microparticles is complicated, the framboid for obtaining
Footpath is larger, size heterogeneity.
Content of the invention
For the defect of prior art, the present invention is intended to provide a kind of preparation method of polyvinyl alcohol microparticles.
The present invention is achieved by the following technical solutions.
The preparation method of polyvinyl alcohol microparticles, comprises the steps of：
（1）According to mass concentration 2.5%-10%, polyvinyl alcohol is weighed, be dissolved in deionized water, stood 30min, then heat up
To 80 DEG C, 30min is stirred；
（2）According to volume ratio 2:1, by step（1）Solution add the vegetable oil containing sorbitan trioleate in,
30min is stirred at 60-80 DEG C；
（3）In step（2）Product in add glutaraldehyde, wherein, the mass ratio of glutaraldehyde and polyvinyl alcohol is 1:9, stirring
After 10min, Arlacel-80 is added, persistently after stirring 1h, then ultrasonic under conditions of ultrasonic power is 200W
Process 1h；
（4）By step（3）Product be centrifuged 50min under the rotating speed of 2000rpm, isolate precipitation, by precipitation acetone, go from
Sub- water is respectively washed 3 times, is finally cleaned with acetone again 3 times, and products therefrom is vacuum dried, and obtains white powder and is poly- second
Enol microballoon.
Preferably, step（1）Middle heating rate is 10 DEG C/min.
Preferably, step（2）Middle sorbitan trioleate is 1 with the mass ratio of vegetable oil:60.
Preferably, step（3）0.03 times for polyvinyl alcohol quality of the middle quality for adding Arlacel-80.
Preferably, step（4）In vacuum drying condition be 80 DEG C at dry 4h.
Advantages of the present invention：
The present invention prepares polyvinyl alcohol microparticles by emulsion-crosslinking method, simple to operate, the microspherulite diameter distribution for preparing
Homogeneous, at 15-45 μm, form is completely smooth for average grain diameter, good dispersion.
Specific embodiment
Embodiment 1
The preparation method of polyvinyl alcohol microparticles, comprises the steps of：
（1）According to mass concentration 2.5%, polyvinyl alcohol is weighed, be dissolved in deionized water, stood 30min, then heat to 80
DEG C, stir 30min；
（2）According to volume ratio 2:1, by step（1）Solution add the vegetable oil containing sorbitan trioleate in, 60
30min is stirred at DEG C；
（3）In step（2）Product in add glutaraldehyde, wherein, the mass ratio of glutaraldehyde and polyvinyl alcohol is 1:9, stirring
After 10min, Arlacel-80 is added, persistently after stirring 1h, then ultrasonic under conditions of ultrasonic power is 200W
Process 1h；
（4）By step（3）Product be centrifuged 50min under the rotating speed of 2000rpm, isolate precipitation, by precipitation acetone, go from
Sub- water is respectively washed 3 times, is finally cleaned with acetone again 3 times, and products therefrom is vacuum dried, and obtains white powder and is poly- second
Enol microballoon.
Embodiment 2
The preparation method of polyvinyl alcohol microparticles, comprises the steps of：
（1）According to mass concentration 10%, polyvinyl alcohol is weighed, be dissolved in deionized water, stand 30min, then with heating rate
For 10 DEG C/min, 80 DEG C are warming up to, stir 30min；
（2）According to volume ratio 2:1, by step（1）Solution add the vegetable oil containing sorbitan trioleate in, its
In, sorbitan trioleate is 1 with the mass ratio of vegetable oil:60,30min is stirred at 80 DEG C；
（3）In step（2）Product in add glutaraldehyde, wherein, the mass ratio of glutaraldehyde and polyvinyl alcohol is 1:9, stirring
After 10min, Arlacel-80 is added, persistently after stirring 1h, then ultrasonic under conditions of ultrasonic power is 200W
Process 1h；
（4）By step（3）Product be centrifuged 50min under the rotating speed of 2000rpm, isolate precipitation, by precipitation acetone, go from
Sub- water is respectively washed 3 times, is finally cleaned with acetone again 3 times, and products therefrom is vacuum dried, and obtains white powder and is poly- second
Enol microballoon.
Embodiment 3
The preparation method of polyvinyl alcohol microparticles, comprises the steps of：
（1）According to mass concentration 5%, polyvinyl alcohol is weighed, be dissolved in deionized water, stand 30min, then with 10 DEG C/min
Heating rate be warming up to 80 DEG C, stir 30min；
（2）According to volume ratio 2:1, by step（1）Solution add the vegetable oil containing sorbitan trioleate in, its
In, sorbitan trioleate is 1 with the mass ratio of vegetable oil:60,30min is stirred at 70 DEG C；
（3）In step（2）Product in add glutaraldehyde, wherein, the mass ratio of glutaraldehyde and polyvinyl alcohol is 1:9, stirring
After 10min, Arlacel-80 is added, wherein, the quality for adding Arlacel-80 is polyvinyl alcohol matter
Amount 0.03 times, persistently stirring 1h after, then ultrasonic power be 200W under conditions of ultrasonically treated 1h；
（4）By step（3）Product be centrifuged 50min under the rotating speed of 2000rpm, isolate precipitation, by precipitation acetone, go from
Sub- water is respectively washed 3 times, is finally cleaned with acetone again 3 times, and products therefrom is vacuum dried, wherein, vacuum drying condition
For 4h being dried at 80 DEG C, obtain white powder and be polyvinyl alcohol microparticles.
Claims (5)
1. the preparation method of polyvinyl alcohol microparticles, it is characterised in that：Comprise the steps of：
（1）According to mass concentration 2.5%-10%, polyvinyl alcohol is weighed, be dissolved in deionized water, stood 30min, then heat up
To 80 DEG C, 30min is stirred；
（2）According to volume ratio 2:1, by step（1）Solution add the vegetable oil containing sorbitan trioleate in,
30min is stirred at 60-80 DEG C；
（3）In step（2）Product in add glutaraldehyde, wherein, the mass ratio of glutaraldehyde and polyvinyl alcohol is 1:9, stirring
After 10min, Arlacel-80 is added, persistently after stirring 1h, then ultrasonic under conditions of ultrasonic power is 200W
Process 1h；
（4）By step（3）Product be centrifuged 50min under the rotating speed of 2000rpm, isolate precipitation, by precipitation acetone, go from
Sub- water is respectively washed 3 times, is finally cleaned with acetone again 3 times, and products therefrom is vacuum dried, and obtains white powder and is poly- second
Enol microballoon.
2. the preparation method of polyvinyl alcohol microparticles according to claim 1, it is characterised in that：Step（1）Middle heating rate
For 10 DEG C/min.
3. the preparation method of polyvinyl alcohol microparticles according to claim 1, it is characterised in that：Step（2）Middle anhydrosorbitol
Alcohol trioleate is 1 with the mass ratio of vegetable oil:60.
4. the preparation method of polyvinyl alcohol microparticles according to claim 1, it is characterised in that：Step（3）Middle addition is dehydrated
0.03 times for polyvinyl alcohol quality of the quality of sorbitol monooleate.
5. the preparation method of polyvinyl alcohol microparticles according to claim 1, it is characterised in that：Step（4）Middle vacuum drying
Condition be 80 DEG C at dry 4h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611064644.2A CN106496609A (en) | 2016-11-28 | 2016-11-28 | The preparation method of polyvinyl alcohol microparticles |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107497484A (en) * | 2017-07-12 | 2017-12-22 | 马鞍山科信网络科技有限公司 | A kind of hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst and preparation method thereof |
| CN107601476A (en) * | 2017-09-11 | 2018-01-19 | 长沙小新新能源科技有限公司 | A kind of preparation method of High-performance graphene perforated membrane |
| CN109675532A (en) * | 2019-01-04 | 2019-04-26 | 蚌埠市辽源新材料有限公司 | A kind of hydrophilic porous polyvinyl alcohol resin and preparation method thereof, application |
-
2016
- 2016-11-28 CN CN201611064644.2A patent/CN106496609A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107497484A (en) * | 2017-07-12 | 2017-12-22 | 马鞍山科信网络科技有限公司 | A kind of hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst and preparation method thereof |
| CN107601476A (en) * | 2017-09-11 | 2018-01-19 | 长沙小新新能源科技有限公司 | A kind of preparation method of High-performance graphene perforated membrane |
| CN109675532A (en) * | 2019-01-04 | 2019-04-26 | 蚌埠市辽源新材料有限公司 | A kind of hydrophilic porous polyvinyl alcohol resin and preparation method thereof, application |
| CN109675532B (en) * | 2019-01-04 | 2022-03-11 | 蚌埠市辽源新材料有限公司 | Hydrophilic porous polyvinyl alcohol resin and preparation method and application thereof |
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Application publication date: 20170315 |