CN106435841A - Polyacrylonitrile porous carbon fiber preparation method - Google Patents
Polyacrylonitrile porous carbon fiber preparation method Download PDFInfo
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- CN106435841A CN106435841A CN201610841234.8A CN201610841234A CN106435841A CN 106435841 A CN106435841 A CN 106435841A CN 201610841234 A CN201610841234 A CN 201610841234A CN 106435841 A CN106435841 A CN 106435841A
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- polyacrylonitrile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a polyacrylonitrile porous carbon fiber preparation method. The method comprises the steps of 1, preparing PAN/PS solution, 2, conducting electrostatic blowing to spin the PAN/PS as-spun fiber, 3, conducting the pre-oxidation processing of the as-spun fiber, 4, carbonizing the pre-oxidated fiber. The method is characterized in that the PAN/PS as-spun fiber is spun under the collective functions of both the electrostatic drawing and the air flow drawing, thus not only accelerating the spinning speed, but also let the fiber acquire a higher degree of orientation in the fiber forming process. The acquired as-spun fiber has good conical structure, and is a highly efficient preparation method of Polyacrylonitrile porous carbon fiber. The Polyacrylonitrile porous carbon fiber prepared by using the method has the advantages of being fluffy, having porous beehive structure, having high specific surface area and the like, and can be broadly applied in the application such as electrochemistry, adsorption, catalyst and hydrogen storage.
Description
Technical field
The invention belongs to carbon fibre material technical field is and in particular to a kind of system of efficient polyacrylonitrile-radical porous carbon fiber
Preparation Method.
Background technology
Carbon fiber is that one kind has high intensity, high-moduluss, low-density, high temperature resistant, resistance to chemical attack, low resistance, thermal conductivity system
The superperformance high-performance fibers such as number height, radiation hardness, therefore it has a wide range of applications, and is in particular in Aero-Space, friendship
The logical field such as transport, sports equipment.With the continuous progress of technology, the diameter of fiber is less and less, the appearance of carbon nano-fiber
The specific surface area of carbon fiber is made to increase manyfold, this makes carbon fiber have new application in fields such as hydrogen storage, catalysis, absorption.
In order to increase the specific surface area of carbon fiber further, can make the surface of carbon fiber or inside loose structure and (includes micropore, big
Hole, mesoporous), the breakthrough of this technology makes carbon fiber have wider application in energy storage and transfer field.
At present, the preparation of porous carbon fiber and research main include chemical vapor infiltration (cattle is strong, Zhang Xiaobin, Cheng Jipeng,
Deng. the preparation of porous filamentous nanocarbon and its applied research [J] in ultracapacitor. functional material, 2009,40 (2)：
314-316.), template (Yang J, Xie J, Zhou X, et al.Functionalized N-doped porous
carbon nanofiber webs for a lithium-sulfur battery with high capacity and
Rate performance [J] .The Journal of Physical Chemistry C, 2014,118 (4)：1800-
1807.), wet spinning (Li G, Xie T, Yang S, et al.Microwave absorption enhancement of
porous carbon fibers compared with carbon nanofibers[J].The Journal of
Physical Chemistry C, 2012,116 (16)：9196-9201.) and method of electrostatic spinning (Moon S C, Choi J K,
Farris R J.Highly porous polyacrylonitrile/polystyrene nanofibers by
Electrospinning [J] .Fibers and Polymers, 2008,9 (3)：276-280.) etc., it is compared to chemical gaseous phase
The complexity such as deposition, wet spinning, template, the preparation method of expensive carbon nano-fiber, it is simple, high that electrostatic spinning has equipment
Effect, low cost, the advantages of continuously can prepare nanofiber, researcher both domestic and external prepares polyacrylonitrile using electrostatic spinning
Mainly by two ways, including polyacrylonitrile, polyacrylonitrile and additive (polymer and slaine), the former forms base carbon fibre
Be a kind of carbon fiber of entity structure, the latter formed be the carbon fiber with loose structure.But electrostatic spinning spinning efficiency
Low, this directly limits the road of its industrialization.And molten the blowing of electrostatic is a kind of proposition of novelty by electrostatic spinning process and air-flow
Blowing process is combined together, and relies on electrostatic field force and the coupling of air-flow drafting force to carry out drawing-off to fiber, in addition,
Air-flow can accelerate the volatilization of solvent, the carbon fiber fibril excellent to prepare appearance structure, improve its production efficiency simultaneously.
Content of the invention
In order to overcome the existing shortcoming preparing porous carbon fiber technology and deficiency, the main object of the present invention is offer one
Plant the method efficiently preparing polyacrylonitrile (PAN)/polystyrene (PS) porous carbon fiber, the PAN/PS that the method prepares is many
Hole carbon fiber has fluffy, porous honeycomb coaly structure, the size in hole is nanoscale, specific surface area is big, material using extensively
Etc. good characteristics.
The purpose of the present invention is achieved through the following technical solutions：A kind of preparation side of polyacrylonitrile-radical porous carbon fiber is provided
Method, is specifically designed a kind of molten blowing technology of electrostatic and prepares polyacrylonitrile-radical porous carbon fiber, its feature comprises the following steps：
(1) preparation of PAN/PS solution：The polystyrene taking certain mass is poured into and is filled DMF solvent
In, stirring at 70 DEG C makes it be completely dissolved, and then adds a certain amount of polyacrylonitrile, stirs 12h under room temperature；
(2) the standby PAN/PS as-spun fibre of the molten blowing of electrostatic：The solution preparing is added in syringe pump, according to certain
Feed flow speed carries out that electrostatic is molten to blow spinning, and the positive pole of high voltage power supply is connected at spinning nozzle needle point and applies certain voltage, spinning nozzle
The blast size of attenuating blast wind is adjusted according to quantitative valve, and spinning liquid drawing-off under high voltage electric field and air drawing field action is thin
Change and obtain polyacrylonitrile/polystyrene as-spun fibre, and be deposited in the reception device of certain distance；
(3) pre-oxidation treatment of PAN/PS as-spun fibre：In the atmosphere of air or oxygen, by the as-spun fibre liter of preparation
To 200-300 DEG C, heating rate is 2 DEG C/min to temperature, is incubated 1h, then naturally cools to room temperature, obtains the polypropylene pre-oxidizing
Nitrile/styroflex；
(4) carbonization treatment of PAN/PS preoxidized fiber：Under the atmosphere of nitrogen, by the polyacrylonitrile/polyphenyl second of pre-oxidation
Alkene fiber is warming up to 800-1000 DEG C, and heating rate is 5 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtain polypropylene
The porous carbon fiber of itrile group.
The preparation method of described polyacrylonitrile-radical porous carbon fiber it is characterised in that：Step 1) described polyacrylonitrile/poly-
In styrene solution, polyacrylonitrile and the mass ratio of polystyrene are 1: 1-3: 1, and in solution, the mass fraction of polyacrylonitrile is 13-
15%, the mass fraction of polystyrene is 5-13%.
The preparation method of described polyacrylonitrile-radical porous carbon fiber it is characterised in that：Step 2) described polyacrylonitrile/poly-
The electrostatic of styrene as-spun fibre is molten to blow preparation technology：The delivery rate of spinning liquid is 20-30ml/h, and the voltage of high voltage power supply is
35-45kV, the pressure of spinning nozzle air-flow is 0.01-0.1MPa, and reception device is 50-80cm with the distance of spinning nozzle.
The core of the polyacrylonitrile-radical porous carbon fiber being prepared by such scheme is PAN/PS as-spun fibre in electrostatic
Drawing-off and air drawing collective effect spinning obtain, and the appearance structure of fiber is excellent, and obtaining fibrous membrane, to have a structure fluffy, spins
Silk speed is fast, high times of traditional electrostatic spinning of ratio, and the polyacrylonitrile-radical porous carbon fiber obtaining has
The pore structure of honeycomb coaly, being evenly distributed of hole, in nanoscale, specific surface area is big, and flexibility is good in aperture.Prepared by the present invention
Polyacrylonitrile-radical porous carbon fiber has broad application prospects in fields such as electrochemistry, catalysis, hydrogen storage, and is porous carbon fiber
Industrialization production provide new thinking.
Brief description
Fig. 1 is the SEM photograph of polyacrylonitrile-radical porous carbon fiber in embodiment 2.
Fig. 2 is the TEM photo of polyacrylonitrile-radical porous carbon fiber in embodiment 2.
Fig. 3 is the SEM photograph of polyacrylonitrile-radical porous carbon fiber in embodiment 3.
Fig. 4 is the TEM photo of polyacrylonitrile-radical porous carbon fiber in embodiment 3.
Specific embodiment
The present embodiments relate to a kind of polyacrylonitrile-radical porous carbon fiber and its preparation process, real to wherein several groups below
Apply example to be described in detail respectively.
Embodiment 1：
(1) preparation of PAN/PS solution：Take 1.17g PS microgranule, add 20g DMF, stirring at 70 DEG C makes it completely molten
Solution.Then add 3.5g PAN, under room temperature, stir 12h, now, the content of PAN is the content of 15%, PS is 5%；
(2) the standby PAN/PS as-spun fibre of the molten blowing of electrostatic：The solution preparing is added in syringe pump, feed flow speed is
20ml/h, spinning tip diameter is 0.8mm, and the positive pole of high voltage power supply is connected at spinning nozzle needle point, and minus earth is processed, its high pressure
The voltage of power supply is 35kv, and spinning nozzle drawing-off blast is adjusted to 0.01MPa, and reception device is 50cm with the distance of spinning nozzle；
(3) pre-oxidation treatment of PAN/PS as-spun fibre：In atmosphere, the as-spun fibre of preparation is warming up to 200 DEG C, rises
Warm speed is 2 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtains the PAN/PS fiber pre-oxidizing；
(4) carbonization treatment of PAN/PS preoxidized fiber：Under the atmosphere of nitrogen, the PAN/PS fiber of pre-oxidation is warming up to
800 DEG C, heating rate is 5 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtain the porous carbon fiber of polyacrylonitrile-radical.
Embodiment 2：
(1) preparation of PAN/PS solution：Take 1.75g PS microgranule, add 20gDMF, stirring at 70 DEG C makes it be completely dissolved.
Then add 3.5gPAN, under room temperature, stir 12h, now, the content of PAN is the content of 13.8%, PS is 7%；
(2) the standby PAN/PS as-spun fibre of the molten blowing of electrostatic：The solution preparing is added in syringe pump, feed flow speed is
23ml/h, spinning tip diameter is 0.8mm, and the positive pole of high voltage power supply is connected at spinning nozzle needle point, and minus earth is processed, its high pressure
The voltage of power supply is 40kv, and spinning nozzle drawing-off blast is adjusted to 0.04MPa, and reception device is 60cm with the distance of spinning nozzle；
(3) pre-oxidation treatment of PAN/PS as-spun fibre：In atmosphere, the as-spun fibre of preparation is warming up to 260 DEG C, rises
Warm speed is 2 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtains the PAN/PS fiber pre-oxidizing；
(4) carbonization treatment of PAN/PS preoxidized fiber：Under the atmosphere of nitrogen, the PAN/PS fiber of pre-oxidation is warming up to
900 DEG C, heating rate is 5 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtain the porous carbon fiber of polyacrylonitrile-radical.
Embodiment 3：
(1) preparation of PAN/PS solution：Take 2.33g PS microgranule, add 20g DMF, stirring at 70 DEG C makes it completely molten
Solution.Then add 3.5g PAN, under room temperature, stir 12h, now, the content of PAN is the content of 13.6%, PS is 9%；
(2) the standby PAN/PS as-spun fibre of the molten blowing of electrostatic：The solution preparing is added in syringe pump, feed flow speed is
27ml/h, spinning tip diameter is 0.8mm, and the positive pole of high voltage power supply is connected at spinning nozzle needle point, and minus earth is processed, its high pressure
The voltage of power supply is 40kv, and spinning nozzle drawing-off blast is adjusted to 0.07MPa, and reception device is 70cm with the distance of spinning nozzle；
(3) pre-oxidation treatment of PAN/PS as-spun fibre：In atmosphere, the as-spun fibre of preparation is warming up to 260 DEG C, rises
Warm speed is 2 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtains the PAN/PS fiber pre-oxidizing；
(4) carbonization treatment of PAN/PS preoxidized fiber：Under the atmosphere of nitrogen, the PAN/PS fiber of pre-oxidation is warming up to
1000 DEG C, heating rate is 5 DEG C/min, is incubated 1h, then naturally cools to room temperature, and the porous carbon obtaining polyacrylonitrile-radical is fine
Dimension.
Embodiment 4：
(1) preparation of PAN/PS solution：Take 3.5g PS microgranule, add 20g DMF, stirring at 70 DEG C makes it be completely dissolved.
Then add 3.5g PAN, under room temperature, stir 12h, now, the content of PAN is the content of 13%, PS is 13%；
(2) the standby PAN/PS as-spun fibre of the molten blowing of electrostatic：The solution preparing is added in syringe pump, feed flow speed is
30ml/h, spinning tip diameter is 0.8mm, and the positive pole of high voltage power supply is connected at spinning nozzle needle point, and minus earth is processed, its high pressure
The voltage of power supply is 45kv, and spinning nozzle drawing-off blast is adjusted to 0.1MPa, and reception device is 80cm with the distance of spinning nozzle；
(3) pre-oxidation treatment of PAN/PS as-spun fibre：In atmosphere, the as-spun fibre of preparation is warming up to 300 DEG C, rises
Warm speed is 2 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtains the PAN/PS fiber pre-oxidizing；
(4) carbonization treatment of PAN/PS preoxidized fiber：Under the atmosphere of nitrogen, the PAN/PS fiber of pre-oxidation is warming up to
1000 DEG C, heating rate is 5 DEG C/min, is incubated 1h, then naturally cools to room temperature, and the porous carbon obtaining polyacrylonitrile-radical is fine
Dimension.
Claims (3)
1. a kind of preparation method of polyacrylonitrile-radical porous carbon fiber, its feature comprises the following steps：
(1) preparation of polyacrylonitrile/polystyrene solution：The polystyrene taking certain mass is poured into and is filled N, N- dimethyl formyl
In amine solvent, stirring at 70 DEG C makes it be completely dissolved, and then adds a certain amount of polyacrylonitrile, stirs 12h under room temperature；
(2) the standby polyacrylonitrile/polystyrene as-spun fibre of the molten blowing of electrostatic：The solution preparing is added in syringe pump, presses
Carry out according to certain feed flow speed that electrostatic is molten to blow spinning, the positive pole of high voltage power supply is connected at spinning nozzle needle point and applies certain electricity
Pressure, the blast size of spinning nozzle attenuating blast wind is adjusted according to quantitative valve, and spinning liquid is made in high voltage electric field and air drawing field
Obtain polyacrylonitrile/polystyrene as-spun fibre with lower drawing-off refinement, and be deposited in the reception device of certain distance；
(3) pre-oxidation treatment of polyacrylonitrile/polystyrene as-spun fibre：In the atmosphere of air or oxygen, preparation is first
Raw fiber is warming up to 200-300 DEG C, and heating rate is 2 DEG C/min, is incubated 1h, then naturally cools to room temperature, pre-oxidized
Polyacrylonitrile/styroflex；
(4) carbonization treatment of polyacrylonitrile/polystyrene preoxidized fiber：Under the atmosphere of nitrogen, by pre-oxidation polyacrylonitrile/
Styroflex is warming up to 800-1000 DEG C, and heating rate is 5 DEG C/min, is incubated 1h, then naturally cools to room temperature, obtain
The porous carbon fiber of polyacrylonitrile-radical.
2. polyacrylonitrile-radical porous carbon fiber according to claim 1 preparation method it is characterised in that：Described polypropylene
In nitrile/polystyrene solution, polyacrylonitrile and the mass ratio of polystyrene are 1: 1-3: 1, the mass fraction of polyacrylonitrile in solution
For 13-15%, the mass fraction of polystyrene is 5-13%.
3. polyacrylonitrile-radical porous carbon fiber according to claim 1 and 2 preparation method it is characterised in that：Described poly-
The electrostatic of acrylonitrile/polystyrene as-spun fibre is molten to blow preparation technology：The delivery rate of spinning liquid is 20-30ml/h, high-tension electricity
The voltage in source is 35-45kV, and the pressure of spinning nozzle air-flow is 0.01-0.1MPa, and reception device is 50- with the distance of spinning nozzle
80cm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106848314A (en) * | 2017-02-27 | 2017-06-13 | 天津工业大学 | The method that lithium-sulfur cell prepares positive electrode with the preparation method of double-layer porous carbon nano-fiber and using it |
| CN107051382A (en) * | 2017-04-21 | 2017-08-18 | 中国科学院城市环境研究所 | A kind of carbon dioxide adsorption porous carbon nanofiber material and preparation method thereof |
| CN107482194A (en) * | 2017-08-04 | 2017-12-15 | 浙江理工大学 | A kind of amorphous germanium dioxide/multi-pipeline carbon nano-fiber and preparation method thereof |
| CN107623120A (en) * | 2017-10-12 | 2018-01-23 | 中国科学技术大学 | Flexible electrode material, its preparation method and lithium/sodium-ion battery |
| CN109786685A (en) * | 2018-12-11 | 2019-05-21 | 天津工业大学 | A kind of preparation method of flexible electrode material |
| CN110258123A (en) * | 2019-06-27 | 2019-09-20 | 山东大学 | The hydrogen storage active carbon fiber felt and its preparation method and application of one specific admixture hollow glass microballoon |
| CN114678544A (en) * | 2022-04-01 | 2022-06-28 | 昆明理工大学 | Preparation method of 3D multi-stage pore nitrogen-doped carbon-supported monatomic Fe catalyst |
| CN115948821A (en) * | 2023-02-21 | 2023-04-11 | 江南大学 | Hollow, porous and multi-layer polyacrylonitrile-based carbon fiber and preparation method thereof |
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| CN102936764A (en) * | 2012-11-27 | 2013-02-20 | 天津工业大学 | Preparation method of polyacrylonitrile-based carbon nanofibers |
| CN104342783A (en) * | 2013-07-31 | 2015-02-11 | 国家纳米科学中心 | A nanometer or nanometer porous carbon fiber bundle, a preparing method thereof and applications of the bundle |
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| CN106848314B (en) * | 2017-02-27 | 2019-04-16 | 天津工业大学 | The lithium-sulfur cell preparation method of double-layer porous carbon nano-fiber and the method for preparing positive electrode using it |
| CN106848314A (en) * | 2017-02-27 | 2017-06-13 | 天津工业大学 | The method that lithium-sulfur cell prepares positive electrode with the preparation method of double-layer porous carbon nano-fiber and using it |
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| CN107482194A (en) * | 2017-08-04 | 2017-12-15 | 浙江理工大学 | A kind of amorphous germanium dioxide/multi-pipeline carbon nano-fiber and preparation method thereof |
| CN107482194B (en) * | 2017-08-04 | 2019-12-20 | 浙江理工大学 | Amorphous germanium dioxide/multi-pipeline carbon nanofiber and preparation method thereof |
| CN107623120A (en) * | 2017-10-12 | 2018-01-23 | 中国科学技术大学 | Flexible electrode material, its preparation method and lithium/sodium-ion battery |
| CN109786685A (en) * | 2018-12-11 | 2019-05-21 | 天津工业大学 | A kind of preparation method of flexible electrode material |
| CN110258123A (en) * | 2019-06-27 | 2019-09-20 | 山东大学 | The hydrogen storage active carbon fiber felt and its preparation method and application of one specific admixture hollow glass microballoon |
| CN110258123B (en) * | 2019-06-27 | 2024-02-23 | 山东大学 | Active carbon fiber felt for hydrogen storage of hybrid hollow glass microspheres and preparation method and application thereof |
| CN114678544A (en) * | 2022-04-01 | 2022-06-28 | 昆明理工大学 | Preparation method of 3D multi-stage pore nitrogen-doped carbon-supported monatomic Fe catalyst |
| CN114678544B (en) * | 2022-04-01 | 2023-04-07 | 昆明理工大学 | Preparation method of 3D hierarchical pore nitrogen-doped carbon-supported monatomic Fe catalyst |
| CN115948821A (en) * | 2023-02-21 | 2023-04-11 | 江南大学 | Hollow, porous and multi-layer polyacrylonitrile-based carbon fiber and preparation method thereof |
| CN115948821B (en) * | 2023-02-21 | 2023-09-22 | 江南大学 | Hollow, porous and multi-layer polyacrylonitrile-based carbon fiber and preparation method thereof |
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Application publication date: 20170222 |