CN103103629A - Fullerene-polymer composite nanofiber and preparation method thereof - Google Patents
Fullerene-polymer composite nanofiber and preparation method thereof Download PDFInfo
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- CN103103629A CN103103629A CN2013100584215A CN201310058421A CN103103629A CN 103103629 A CN103103629 A CN 103103629A CN 2013100584215 A CN2013100584215 A CN 2013100584215A CN 201310058421 A CN201310058421 A CN 201310058421A CN 103103629 A CN103103629 A CN 103103629A
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Abstract
The invention discloses a fullerene-polymer composite nanofiber and a preparation method thereof. The preparation method comprises the following steps: conducting ball milling mixing on 2-20 wt% of fullerene and 80-98 wt% of a polymer material; dissolving the uniformly mixed mixture in a solvent, and thoroughly stirring to obtain a spinning solution; and preparing the uniformly stirred spinning solution into the fullerene-polymer composite nanofiber by an electrospinning method. The method provided by the invention solves the problem of incompatibility of fullerene and polymer material in solvent; meanwhile, the invention can greatly improve addition amount of the fullerene; and under high addition amount of fullerenes, the prepared composite nanofiber shows no phenomenon of fullerene particle aggregation.
Description
Technical field
The present invention relates to the nano-fiber material field, relate in particular to a kind of fullerene-macromolecule composite nano fiber and preparation method thereof.
Background technology
At present, C
60, C
70With its unique structure and extremely people's attention of character, become the important selection in the fields such as current physics, chemistry, material and life science Deng fullerene-based material.The molecular structure of the closed shell football shaped of fullerene height symmetry has determined that it has unique physics and chemistry performance, the various chemical modification objects of fullerene have the performance of various uniquenesses, such as the fullerene polymer derivative as functional material in good using values in aspect such as photoelectricity, biologically active, catalysis, lubricants.
Nanofiber is a kind of nano material of accurate one-dimentional structure, has and the similar high length-diameter ratio of CNT, except having the characteristics such as mechanical property excellence, specific area be large, also has the advantages such as easy machine-shaping, microstructure is controlled.
Yet, at present also do not have fullerene and Polymer materialspreparation to obtain the simple and effective method of blended fiber, expect the blended fiber of several different materials, need first prepare the fullerene polymer mixed solution, but the deliquescent restriction due to fullerene, therefore be difficult to find suitable solvent to make two kinds of materials evenly mix dissolving fully when preparation fullerene polymer mixed solution, cause existing fullerene to obtain mixing nanofiber with Polymer materialspreparation, fullerene and macromolecular material can't be realized effectively compound at aspect of performance.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of fullerene-macromolecule composite nano fiber and preparation method thereof, be intended to solve existing fullerene and macromolecule is incompatible, can't prepare the problem of blended fiber.
Technical scheme of the present invention is as follows:
The preparation method of a kind of fullerene-macromolecule composite nano fiber wherein, comprises step:
S1, by the quality percentage composition, 2% ~ 20% fullerene and 80% ~ 98% macromolecular material are carried out ball milling mix;
S2, the mixture that mixes is dissolved in solvent, and fully stirs and make spinning solution;
S3, by electrospinning process, the spinning solution that stirs is made fullerene-high molecular composite nano fiber.
The preparation method of described fullerene-macromolecule composite nano fiber, wherein, in described step S1, the quality percentage composition of described fullerene is 3% ~ 10%.
The preparation method of described fullerene-macromolecule composite nano fiber, wherein, described macromolecular material is one or more in polyacrylonitrile, polymethyl methacrylate, PVK, polyvinylpyrrolidone, chitin, carboxymethyl cellulose or shitosan.
The preparation method of described fullerene-macromolecule composite nano fiber, wherein, described fullerene is C
60, C
70Or C
60With C
70Mixture.
The preparation method of described fullerene-macromolecule composite nano fiber wherein, in described step S1, adopts ball mill to carry out ball milling to fullerene and macromolecular material and mixes, and described ball mill is the low temperature intermittent ball mill.
The preparation method of described fullerene-macromolecule composite nano fiber, wherein, described solvent is DMF.
A kind of fullerene-macromolecule composite nano fiber wherein, adopts preparation method as claimed in claim 1 to prepare.
Beneficial effect: fullerene provided by the invention-macromolecule composite nano fiber and preparation method thereof has solved fullerene and macromolecular material inconsistent problem in solvent, the present invention simultaneously can also improve the addition of fullerene greatly, and in the situation that higher fullerene addition, the phenomenon that fullerenic particles is assembled does not appear in the composite nano fiber that makes.
Description of drawings
Fig. 1 is the morphology characterization figure of the fullerene for preparing of embodiment 1-macromolecule composite nano fiber.
Fig. 2 is the morphology characterization figure of the fullerene for preparing of embodiment 2-macromolecule composite nano fiber.
Fig. 3 is the morphology characterization figure of the fullerene for preparing of embodiment 3-macromolecule composite nano fiber.
Fig. 4 to Fig. 5 is the electron microscope scanning figure of the spinning solution different amplification for preparing of embodiment 4.
Fig. 6 is the afm scan figure of the spinning solution for preparing of embodiment 4.
The specific embodiment
The invention provides a kind of fullerene-macromolecule composite nano fiber and preparation method thereof, clearer, clear and definite for making purpose of the present invention, technical scheme and effect, below the present invention is described in more detail.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The preparation method of fullerene provided by the invention-macromolecule composite nano fiber, it comprises step:
S1, by the quality percentage composition, 2% ~ 20% fullerene and 80% ~ 98% macromolecular material are carried out ball milling mix;
S2, the mixture that mixes is dissolved in solvent, and fully stirs and make spinning solution;
S3, by electrospinning process, the spinning solution that stirs is made fullerene-high molecular composite nano fiber.
In step S1, the present invention makes fullerene be dispersed among the powder of macromolecular material by the ball milling hybrid mode, after mixture is dissolved into solvent, macromolecular material has good hydrotropy effect for fullerene, macromolecular material can form micella in solvent simultaneously, for fullerene, good burden effect is arranged, and these two kinds of effects can guarantee in the final composite nano fiber that forms, the fullerene Uniform Dispersion, and can not assemble.So, method provided by the invention has solved fullerene and macromolecular material inconsistent problem in solvent, the present invention simultaneously can also improve the addition of fullerene greatly, and in the situation that higher fullerene addition, the phenomenon that fullerenic particles is assembled does not appear in the composite nano fiber that makes.
Further, in step S1, the quality percentage composition of described fullerene is preferably 3% ~ 10%, contains the fullerene of high level in the composite nano fiber that can guarantee like this to make at last, can make again fullerene the situation of particle aggregation can not occur.
Further, described macromolecular material is preferably one or more in polyacrylonitrile, polymethyl methacrylate, PVK, polyvinylpyrrolidone, chitin, carboxymethyl cellulose or shitosan.These macromolecular materials have better solubilization-aid effect for fullerene, from having improved the quality stability of composite nano fiber.
Further, described fullerene is C
60, C
70Or C
60With C
70Mixture, C
60, C
70Best with the compatible effect of macromolecular material.
In step S1, the present invention preferably adopts ball mill to carry out ball milling to fullerene and macromolecular material to mix, described ball mill is the low temperature intermittent ball mill, as its name suggests, the low temperature intermittent ball mill adopts exactly and in step mode, fullerene and macromolecular material is carried out ball milling mix under cryogenic conditions, can make like this temperature when both carrying out ball milling be unlikely to too high, avoid destroying the molecular structure of fullerene, macromolecular material.Temperature control during the ball mill ball milling is at 15 ~ 20 ℃, and the ball mill start and stop once: turn round after 1 ~ 20 minute, stop 20 ~ 40 minutes, according to this ball milling method, mixture is carried out ball milling and mix, ball milling effect preferably can be guaranteed, temperature can be controlled again unlikely too high.
Further, in step S2, described solvent is DMF(N, dinethylformamide), DMF is a kind of solvent of function admirable, it is all good solvent to multiple macromolecular material, can be used for the composite nano fiber in synthetic the present invention.
in step S3, the present invention adopts electrospinning process that spinning solution is prepared into composite nano fiber, specifically realize by an electrostatic spinning apparatus, described electrostatic spinning apparatus comprises high voltage source, measuring pump, shower nozzle, receiver, (structure about electrostatic spinning apparatus can be with reference to content of the prior art for container, the present invention repeats no more), spinning solution is moved in the container of electrostatic spinning apparatus, this container is provided with a taphole, the place is provided with a metal needle at described taphole, the aperture of described metal needle can be set to 0.1 ~ 1.6mm, the receiving range of receiver and metal needle is set to 10 ~ 20cm, and switch on power, the output voltage of high voltage source is adjusted to suitable voltage, spinning solution in container flows out from taphole and carries out electrostatic spinning, and controlled the flow velocity of spinning solution by measuring pump, preferably be controlled to be 0.1 ~ 5ml/h, like this in container all spinning solution spinning complete after, collect the nonwoven fabric on receiver, the nonwoven fabric that makes is size has tens long fibers to the hundreds of nanometer to consist of.
The basic principle of electrostatic spinning is by with high-pressure electrostatic on the spinning solution band, and the drop of charged spinning solution taylor cone summit at capillary under the effect of electric field is accelerated, forms charged jet, is deposited on receiver at last.
Based on the preparation method of above-mentioned fullerene-macromolecule composite nano fiber, the present invention also provides a kind of fullerene-macromolecule composite nano fiber, and it adopts above-mentioned preparation method to prepare.
The present invention will be described in more detail below by specific embodiment.
Embodiment one
1.5g polyacrylonitrile and 100mgC
60Move to after mixing in ball grinder, ball grinder is contained in ball mill.Ball milling speed 500 is set turns/h, the ball milling temperature setting is set to 20 degree, and start and stop once comprise: often turn 10 minutes, stop 20 minutes, continuous like this carrying out makes mixture after 12 start and stop, and mixture is dissolved in DMF, is made into mass fraction and is 10% spinning solution.Inject spinning solution in the container of device for spinning, it is 20kv that voltage is set, and accepting distance is 15cm.After spinning finishes, collect nonwoven fabric, carry out morphology characterization.
Can find out from Fig. 1, although resulting composite nano fiber thickness and inhomogeneous, the large-scale clustering phenomena of fullerenic particles does not appear in prepared composite nano fiber thickness.
Embodiment two
1.5g polymethyl methacrylate and 100mgC
60Move to after mixing in ball grinder, ball grinder is contained in ball mill.Ball milling speed 600 is set turns/h, the ball milling temperature is 20 degree, and start and stop once comprise: often turn 15 minutes, stop 30 minutes, continuous like this carrying out makes mixture after 12 start and stop, and mixture is dissolved in DMF, is made into mass fraction and is 12% spinning solution.Inject spinning solution in the container of device for spinning, it is 15kv that voltage is set, and accepting distance is 10cm.After spinning finishes, collect nonwoven fabric, carry out morphology characterization.
Fullerene and polymethyl methacrylate have formed uniform composite nano fiber as can be seen from Figure 2, and do not occur the phenomenon that fullerene is assembled on a large scale.
Embodiment three: 1.5g PVK and 100mgC
60Move to after mixing in ball grinder, ball grinder is contained in ball mill.Ball milling speed 600 is set turns/h, the ball milling temperature is 20 degree, and start and stop once comprise: often turn 15 minutes, stop 30 minutes, continuous like this carrying out makes mixture after 12 start and stop, and mixture is dissolved in DMF, is made into mass fraction and is 12% spinning solution.Inject spinning solution in the container of device for spinning, it is 15kv that voltage is set, and accepting distance is 10cm.After spinning finishes, collect nonwoven fabric, carry out morphology characterization.
As can be seen from Figure 3, fullerene and PVK have formed uniform composite nano fiber, do not occur simultaneously the phenomenon that fullerene is assembled on a large scale.
Embodiment four
For fullerene in spinning solution and the existence of macromolecular material are described, the present invention is by the TEM(electron microscope) and the AFM(AFM) carry out morphology characterization.Take polyacrylonitrile as example, specific as follows: mix in ball mill completely that fullerene and polyacrylonitrile powder are dissolved in DMF, make spinning solution after fully stirring, filter out a small amount of insoluble matter, lower floor's solution carries out AFM and TEM characterizes.
Can find out from Fig. 4 to Fig. 6, fullerenic particles is surrounded by polyacrylonitrile, and Uniform Dispersion, and fullerene cluster size is about 10nm.In ball milling mixed process, fullerene just has been dispersed among the polyacrylonitrile powder, after in mixed-powder is dissolved into DMF, there is good hydrotropy effect in polyacrylonitrile for fullerene, simultaneously polyacrylonitrile forms micella in DMF also can have good burden effect to fullerene, and two kinds of effects have guaranteed the Uniform Dispersion of fullerene in the nanofiber of final formation and do not found the clustering phenomena of fullerene.
In sum, preparation method provided by the invention, hydrotropy effect and the burden effect of macromolecular material have been utilized, make fullerene can be dispersed in spinning solution, the composite nano fiber that makes had at last both improved the addition of fullerene, can guarantee that again fullerenic particles clustering phenomena can not occur, resulting composite nano fiber has had that good mechanical performance, specific area are large concurrently, easily machine-shaping, microstructure is controlled and the physics and chemistry performance of the various uniquenesses of fullerene.
Should be understood that, application of the present invention is not limited to above-mentioned giving an example, and for those of ordinary skills, can be improved according to the above description or conversion, and all these improve and conversion all should belong to the protection domain of claims of the present invention.
Claims (7)
1. the preparation method of fullerene-macromolecule composite nano fiber, is characterized in that, comprises step:
S1, by the quality percentage composition, 2% ~ 20% fullerene and 80% ~ 98% macromolecular material are carried out ball milling mix;
S2, the mixture that mixes is dissolved in solvent, and fully stirs and make spinning solution;
S3, by electrospinning process, the spinning solution that stirs is made fullerene-high molecular composite nano fiber.
2. the preparation method of fullerene-macromolecule composite nano fiber according to claim 1, is characterized in that, in described step S1, the quality percentage composition of described fullerene is 3% ~ 10%.
3. the preparation method of fullerene-macromolecule composite nano fiber according to claim 1, it is characterized in that, described macromolecular material is one or more in polyacrylonitrile, polymethyl methacrylate, PVK, polyvinylpyrrolidone, chitin, carboxymethyl cellulose or shitosan.
4. the preparation method of fullerene-macromolecule composite nano fiber according to claim 1, is characterized in that, described fullerene is C
60, C
70Or C
60With C
70Mixture.
5. the preparation method of fullerene-macromolecule composite nano fiber according to claim 1, is characterized in that, in described step S1, adopts ball mill to carry out ball milling to fullerene and macromolecular material and mixes, and described ball mill is the low temperature intermittent ball mill.
6. the preparation method of fullerene-macromolecule composite nano fiber according to claim 1, is characterized in that, described solvent is DMF.
7. fullerene-macromolecule composite nano fiber, is characterized in that, adopts preparation method as claimed in claim 1 to prepare.
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Cited By (11)
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|---|---|---|---|---|
| CN105926053A (en) * | 2016-06-08 | 2016-09-07 | 海南大学 | Electrostatic spinning method of chitosan |
| CN110306256A (en) * | 2019-07-16 | 2019-10-08 | 高金鹿 | A kind of preparation method of high temperature resistant para-aramid fiber |
| CN110496694A (en) * | 2019-08-30 | 2019-11-26 | 大连工业大学 | A kind of waste wool fiber dust and its preparation method and application |
| CN110669511A (en) * | 2019-10-18 | 2020-01-10 | 安徽大学 | Fullerene crystal near-infrared light-emitting film and preparation method thereof |
| CN110904522A (en) * | 2019-12-12 | 2020-03-24 | 上海奥领纺织新材料有限公司 | Fullerene skin-friendly composite fiber and preparation method thereof |
| CN111172664A (en) * | 2019-12-27 | 2020-05-19 | 常熟市欣鑫经纬编有限公司 | Rabbit hair wool fiber-like fabric |
| CN113122959A (en) * | 2021-04-09 | 2021-07-16 | 天津工业大学 | Bulletproof composite fiber material and preparation method thereof |
| CN114622347A (en) * | 2022-02-28 | 2022-06-14 | 五邑大学 | Fiber membrane and preparation method and application thereof |
| EP3848014A4 (en) * | 2018-08-02 | 2022-08-10 | Beijing Fullcan Biotechnology Co., Ltd | Water-soluble fullerene topical composition |
| CN115582104A (en) * | 2022-11-28 | 2023-01-10 | 佛山(华南)新材料研究院 | Dioxin separation membrane and preparation method thereof |
| CN115772725A (en) * | 2022-11-03 | 2023-03-10 | 苏州经贸职业技术学院 | Preparation of functional fullerene fiber blended silk fabric |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105926053A (en) * | 2016-06-08 | 2016-09-07 | 海南大学 | Electrostatic spinning method of chitosan |
| EP3848014A4 (en) * | 2018-08-02 | 2022-08-10 | Beijing Fullcan Biotechnology Co., Ltd | Water-soluble fullerene topical composition |
| CN110306256B (en) * | 2019-07-16 | 2021-10-01 | 高金鹿 | Preparation method of high-temperature-resistant para-aramid fiber |
| CN110306256A (en) * | 2019-07-16 | 2019-10-08 | 高金鹿 | A kind of preparation method of high temperature resistant para-aramid fiber |
| CN110496694A (en) * | 2019-08-30 | 2019-11-26 | 大连工业大学 | A kind of waste wool fiber dust and its preparation method and application |
| CN110496694B (en) * | 2019-08-30 | 2021-07-09 | 大连工业大学 | Waste wool fiber powder and preparation method and application thereof |
| CN110669511A (en) * | 2019-10-18 | 2020-01-10 | 安徽大学 | Fullerene crystal near-infrared light-emitting film and preparation method thereof |
| CN110669511B (en) * | 2019-10-18 | 2022-07-26 | 安徽大学 | Fullerene crystal near-infrared light-emitting film and preparation method thereof |
| CN110904522A (en) * | 2019-12-12 | 2020-03-24 | 上海奥领纺织新材料有限公司 | Fullerene skin-friendly composite fiber and preparation method thereof |
| CN111172664B (en) * | 2019-12-27 | 2021-06-25 | 常熟市欣鑫经纬编有限公司 | Rabbit hair wool fiber-like fabric |
| CN111172664A (en) * | 2019-12-27 | 2020-05-19 | 常熟市欣鑫经纬编有限公司 | Rabbit hair wool fiber-like fabric |
| CN113122959A (en) * | 2021-04-09 | 2021-07-16 | 天津工业大学 | Bulletproof composite fiber material and preparation method thereof |
| CN113122959B (en) * | 2021-04-09 | 2021-12-10 | 天津工业大学 | Bulletproof composite fiber material and preparation method thereof |
| CN114622347A (en) * | 2022-02-28 | 2022-06-14 | 五邑大学 | Fiber membrane and preparation method and application thereof |
| CN115772725A (en) * | 2022-11-03 | 2023-03-10 | 苏州经贸职业技术学院 | Preparation of functional fullerene fiber blended silk fabric |
| CN115582104A (en) * | 2022-11-28 | 2023-01-10 | 佛山(华南)新材料研究院 | Dioxin separation membrane and preparation method thereof |
| CN115582104B (en) * | 2022-11-28 | 2023-03-14 | 佛山(华南)新材料研究院 | Dioxin separation membrane and preparation method thereof |
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Effective date of registration: 20210629 Address after: No. 1001, Longgang Avenue, Pingxi community, Pingdi street, Longgang District, Shenzhen, Guangdong 518000 Patentee after: Shenzhen TONGCHAN Lixing Technology Group Co.,Ltd. Patentee after: PEKING University SHENZHEN GRADUATE SCHOOL Address before: No. 1001, Longgang Avenue, Longgang District, Shenzhen, Guangdong 518000 Patentee before: Shenzhen Lihe Technology Innovation Co.,Ltd. Patentee before: PEKING University SHENZHEN GRADUATE SCHOOL |