CN103243416A - Preparation method of polyindole/carbon nanotube composite nanofiber membrane - Google Patents
Preparation method of polyindole/carbon nanotube composite nanofiber membrane Download PDFInfo
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- CN103243416A CN103243416A CN2013101827318A CN201310182731A CN103243416A CN 103243416 A CN103243416 A CN 103243416A CN 2013101827318 A CN2013101827318 A CN 2013101827318A CN 201310182731 A CN201310182731 A CN 201310182731A CN 103243416 A CN103243416 A CN 103243416A
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Abstract
The invention discloses a preparation method of a polyindole/carbon nanotube composite nanofiber membrane, and belongs to the preparation technologies of electroactive materials. The method comprises the following processes of: acidifying a carbon nanotube so that the surface of the carbon nanotube is provided with carboxyl, and then dispersing the carbon nanotube into acetonitrile to obtain a carbon nanotube solution; dissolving polyindole into acetonitrile to obtain a transparent and pale yellow polyindole acetonitrile solution; mixing the carbon nanotube solution with the polyindole acetonitrile solution; and then electrospinning, wherein the regulating range of high voltage static is 10 to 30kV, the flow rate of an injection pump ranges from 0.05 to 0.3mL/h, and the receiving distance ranges from 10 to 20cm. The preparation method is simple in process, and the polyindole/carbon nanotube composite nanofiber membrane prepared thereby has the advantages of being high in conductivity and excellent in electroactive performance.
Description
Technical field
The present invention relates to a kind of poly-indoles/CNT (CNTs contains single wall and Duo Bi (n=2-20)) and carry out the preparation method of spinning film forming by high-pressure electrostatic, belong to the technology of preparing of electroactive material.
Background technology
In recent years, along with the further investigation of people to the various performances of conducting polymer, conducting polymer has great application prospect at aspects such as secondary cell, Schottky diode, light emitting diode and transistors.Poly-indoles is a kind of heterocycle polymer of nitrogen atom, and its structure and: polyaniline, polypyrrole are closely similar, in that it has characteristics such as heat endurance height, Eo+ height in nature.Poly-indoles can gather indoles by anodic oxidation indoles monomer is synthetic, and finds that it has very excellent chemical property; Also can synthesize poly-indoles and derivative thereof with electrochemical method simultaneously.As conducting polymer, poly-indoles also has certain electroactive characteristic, can produce strain under effect of electric field.But graininess or membranaceous poly-indoles, its electroactive poor-performing is difficult to satisfy practical application request.To gather indoles and be prepared into nanofiber and can effectively improve its specific area, thereby promote its electroactive performance.
CNT has particular structure, makes it have many potential using values, strengthens aspects such as body, semi-conducting material, catalyst carrier in the nanometer of engineering material and is all placed high hopes by people.In addition, CNT has good conjugated system, high electron affinity energy and energy of ionization, photostability is stronger, and excellent photoelectric performance and physical and mechanical properties make it have application prospect widely at aspects such as improving polymeric material optics, electricity, mechanics, calorifics.Along with the maturation of carbon nanotube preparation technology and the continuous reduction of CNT cost, the application study of CNT more and more becomes the emphasis of research.If it is compound that CNT and poly-indoles are carried out molecular level, carry out electrostatic spinning then, the electroactive material that then is expected to obtain having high electroactive performance.
Also do not relate at present the poly-indoles/preparation of CNT electroactive material and the report of aspect of performance and the patent with high electroactive performance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of poly-indoles/CNT composite nano-fiber membrane makes material with this method and has high electroactive performance.
The present invention is realized by following technical proposals.The preparation method of a kind of poly-indoles/CNT composite nano-fiber membrane, this method is at first carried out acidification with CNT, make its surface have carboxyl, again it is carried out ultrasonic the mixing with poly-indoles in being dissolved in acetonitrile, by the composite nano-fiber membrane that the electrostatic spinning preparation has high electroactive performance, this method is characterized in that comprising following process:
1) carbon nano-tube solution preparation: single wall or multi-walled carbon nano-tubes are joined by quality HNO
3/ H
2SO
4Be in 1: 1 the mixed acid, be mixed with the solution of 0.01-0.1g/mL, solution is heated to the 60-90min that refluxes under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the acetonitrile, it is 5～15mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) poly-indoles formulations prepared from solutions: the poly-indoles that at room temperature with molecular weight is 5-10 ten thousand is dissolved in the acetonitrile, is mixed with volume mass mark (g/L) and is 8～20% solution, and magnetic agitation 6h obtains transparent light yellow poly-indole acetonitrile solution.
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the poly-indole acetonitrile solution of acquisition mixed according to the mass ratio of solute in 0.06: 1～0.24: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and is fixed on the micro-injection pump, and the aluminium foil of placing vertical ground connection according to syringe needle a distance receives.High-pressure electrostatic adjustable range 10～30kV, syringe pump flow velocity 0.05～0.3mL/h, receiving range 10～20cm.Obtaining directly is 80～200nm tunica fibrosa.
Preparation method's process of the present invention is simple, and the poly-indoles/CNT composite nano-fiber membrane that obtains has electrical conductivity height, advantage that electroactive performance is good.
The specific embodiment
Embodiment 1:
1) carbon nano-tube solution preparation: the HNO that the 4.0g Single Walled Carbon Nanotube is joined 200ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.02g/mL, solution is heated to the 60min that refluxes under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 6.0mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) poly-indoles formulations prepared from solutions: at room temperature be that 60,000 poly-indoles is dissolved in the acetonitrile with molecular weight, be mixed with volume mass mark (g/L) and be 10% solution, magnetic agitation 6h obtains transparent light yellow poly-indole acetonitrile solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the poly-indole acetonitrile solution of acquisition mixes according to the mass ratio of solute at 0.08: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 30kV, syringe pump flow velocity 0.05mL/h, receiving range 20cm, obtaining directly is 80～100nm tunica fibrosa.
Embodiment 2:
1) acidifying of nanotube: the HNO that the 4.0g Single Walled Carbon Nanotube is joined 100ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.04g/mL, solution is heated to the 80min that refluxes under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 8.0mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) poly-indoles formulations prepared from solutions: at room temperature be that 60,000 poly-indoles is dissolved in the acetonitrile with molecular weight, be mixed with volume mass mark (g/L) and be 12% solution, magnetic agitation 6h obtains transparent light yellow poly-indole acetonitrile solution;
3) composite solution preparation: the carbon nano-tube solution that step 1) is obtained, with carbon nano-tube solution and step 2) the poly-indole acetonitrile solution of acquisition mixes according to the mass ratio of solute at 0.1: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 25kV, syringe pump flow velocity 0.1mL/h, receiving range 15cm, obtaining directly is 100～120nm tunica fibrosa.
Embodiment 3:
1) acidifying of nanotube: the HNO that the 8.0g Single Walled Carbon Nanotube is joined 100ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.08g/mL, solution is heated to the 90min that refluxes under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 10mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) poly-indoles formulations prepared from solutions: at room temperature be that 100,000 poly-indoles is dissolved in the acetonitrile with molecular weight, be mixed with volume mass mark (g/L) and be 14% solution, magnetic agitation 6h obtains transparent light yellow poly-indole acetonitrile solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the poly-indole acetonitrile solution of acquisition mixes according to the mass ratio of solute at 0.15: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 20kV, syringe pump flow velocity 0.2mL/h, receiving range 20cm, obtaining directly is 120～160nm tunica fibrosa.
Embodiment 4:
1) acidifying of nanotube: the HNO that the 8.0g Single Walled Carbon Nanotube is joined 200ml
3/ H
2SO
4In the mixed acid of (1: 1), be mixed with the solution of 0.08g/mL, solution is heated to the 70min that refluxes under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the deionized water, it is the 12mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) poly-indoles formulations prepared from solutions: at room temperature be that 100,000 poly-indoles is dissolved in the acetonitrile with molecular weight, be mixed with volume mass mark (g/L) and be 18% solution, magnetic agitation 6h obtains transparent light yellow poly-indole acetonitrile solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the poly-indole acetonitrile solution of acquisition mixes according to the mass ratio of solute at 0.20: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 30kV, syringe pump flow velocity 0.25mL/h, receiving range 15cm, obtaining directly is 170～200nm tunica fibrosa.
Claims (1)
1. the preparation method of poly-indoles/CNT composite nano-fiber membrane, this method is at first carried out acidification with CNT, make its surface have carboxyl, again it is carried out ultrasonic the mixing with poly-indoles in being dissolved in acetonitrile, by the composite nano-fiber membrane that the electrostatic spinning preparation has high electroactive performance, this method is characterized in that comprising following process:
1) carbon nano-tube solution preparation: single wall or multi-walled carbon nano-tubes are joined by quality HNO
3/ H
2SO
4Be in 1: 1 the mixed acid, be mixed with the solution of 0.01-0.1g/mL, solution is heated to the 60-90min that refluxes under the fluidized state, spend deionised water after the filtration to faintly acid, at 60 ℃ of following vacuumize 24h, get a certain amount of dried CNT and be scattered in the acetonitrile, it is 5～15mg/mL carbon nano-tube solution that ultrasonic decentralized system gets concentration;
2) poly-indoles formulations prepared from solutions: the poly-indoles that at room temperature with molecular weight is 5-10 ten thousand is dissolved in the acetonitrile, is mixed with volume mass mark (g/L) and is 8～20% solution, and magnetic agitation 6h obtains transparent light yellow poly-indole acetonitrile solution;
3) composite solution preparation: carbon nano-tube solution and step 2 that step 1) is obtained) the poly-indole acetonitrile solution of acquisition mixed according to the mass ratio of solute in 0.06: 1～0.24: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: the composite solution that step 3) is obtained joins in the syringe, and be fixed on the micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 10～30kV, syringe pump flow velocity 0.05～0.3mL/h, receiving range 10～20cm, obtaining directly is 80～200nm tunica fibrosa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361766A (en) * | 2013-07-25 | 2013-10-23 | 黑龙江大学 | Interpenetrating polyaniline/carbon nanotube composite nanofiber material preparation method and application |
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| CN103361766B (en) * | 2013-07-25 | 2017-03-01 | 黑龙江大学 | Interpenetrating structure Polymerization of Polyaniline/carbon Nanotube composite nano-fiber material preparation method and application |
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Application publication date: 20130814 |