CN107675363A - A kind of preparation method of carbon nanofiber membrane - Google Patents
A kind of preparation method of carbon nanofiber membrane Download PDFInfo
- Publication number
- CN107675363A CN107675363A CN201711066851.6A CN201711066851A CN107675363A CN 107675363 A CN107675363 A CN 107675363A CN 201711066851 A CN201711066851 A CN 201711066851A CN 107675363 A CN107675363 A CN 107675363A
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- China
- Prior art keywords
- preparation
- carbon nanofiber
- nanofiber membrane
- nitrogen
- pan
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/43—Acrylonitrile series
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
Abstract
The present invention relates to a kind of preparation method of carbon nanofiber membrane.A kind of preparation method of carbon nanofiber membrane, comprises the following steps:Take following materials for later use, acrylonitrile, Shanghai Jinshan petrochemical industry Co., Ltd;Dimethylformamide, Chemical Reagent Co., Ltd., Sinopharm Group, analyze pure, nitrogen, Nanjing Wonder special gas Co., Ltd, deionized water;Nano fibrous membrane prepared by the method for the invention, carbonized film surface is smooth, zero defect, and with the rise of carburizing temperature, filamentary structure becomes finer and close and ordering, and graphite layers are away from reduction.
Description
Technical field
The present invention relates to a kind of preparation method of carbon nanofiber membrane.
Background technology
CNFs refers to 1-dimention nano fiber carbon material, have it is light, intensity is high, thermal conductivity is good, specific surface area is big and
The features such as being not easy reunion and differential mode atom, electronic structure, in composite, catalyst carrier, hydrogen storage material, repeatable charging
There is huge application prospect in the fields such as battery.CNFs preparation method generally has arc process, Laser vaporization and chemical gaseous phase
Sedimentation.However, these method energy charges are big, condition is relatively harsh, production cost is high, impurity in products is more.Electrostatic spinning skill
Art can realize it is simple, prepare effectively and economically continuous nano-fibre, obtained fiber compared with it is long, impurity is few, specific surface area
Greatly.
The content of the invention
To obtain high-quality CNFs, the present invention proposes a kind of preparation method of carbon nanofiber membrane.
A kind of preparation method of carbon nanofiber membrane of the present invention, comprises the following steps:
(1)Take following materials for later use, acrylonitrile, Shanghai Jinshan petrochemical industry Co., Ltd;Dimethylformamide, Chinese medicines group chemistry examination
Agent Co., Ltd, analyze pure, nitrogen, Nanjing Wonder special gas Co., Ltd, deionized water;
(2)PAN is added into DMF, under 30 DEG C of environment, with 600 rpms of 4~6h of stirring and dissolving, obtaining mass fraction is
14% PAN spinning solutions;
(3)At ambient temperature, distance 15cm, 15~18kV of voltage, 0.5 milliliter of flow velocity are received per hour, after continuous electro-spinning 4h
It is standby that PAN fiber film is put into 70 DEG C of oven drying 12h of people;
(4)PAN fiber film is cut into 2 cm x 4cm are rectangular-shaped to be put into Noah's ark;
(5)In air atmosphere, first pre-oxidized in tube furnace, then in a nitrogen atmosphere, rise to respectively 700 DEG C-
1100 DEG C are carbonized;
(6)Pre oxidation is warming up to 3 centigrade per minutes, is incubated 1h;Then boiler tube is vacuumized, is passed through nitrogen, maintained
Stable nitrogen atmosphere, it is warming up to 700 DEG C -1100 DEG C respectively from Pre oxidation with 6 centigrade per minutes, is incubated 0.5h;Most
After naturally cool to room temperature after produce.
Preferably, the step(5)Temperature be carbonized for 70 degrees Celsius.
Preferably, the nitrogen is warming up to 1100 DEG C from Pre oxidation respectively with 6 centigrade per minutes.
Nano fibrous membrane prepared by the method for the invention, carbonized film surface is smooth, zero defect, with the liter of carburizing temperature
Height, filamentary structure become finer and close and ordering, and graphite layers are away from reduction.
Embodiment
Embodiment 1.
A kind of preparation method of carbon nanofiber membrane of the present invention, comprises the following steps:
(1)Take following materials for later use, acrylonitrile, Shanghai Jinshan petrochemical industry Co., Ltd;Dimethylformamide, Chinese medicines group chemistry examination
Agent Co., Ltd, analyze pure, nitrogen, Nanjing Wonder special gas Co., Ltd, deionized water;
(2)PAN is added into DMF, under 30 DEG C of environment, with 600 rpms of 4~6h of stirring and dissolving, obtaining mass fraction is
14% PAN spinning solutions;
(3)At ambient temperature, distance 15cm, 15~18kV of voltage, 0.5 milliliter of flow velocity are received per hour, after continuous electro-spinning 4h
It is standby that PAN fiber film is put into 70 DEG C of oven drying 12h of people;
(4)PAN fiber film is cut into 2 cm x 4cm are rectangular-shaped to be put into Noah's ark;
(5)In air atmosphere, first pre-oxidized in tube furnace, then in a nitrogen atmosphere, rise to 700 DEG C of progress respectively
Carbonization;
(6)Pre oxidation is warming up to 3 centigrade per minutes, is incubated 1h;Then boiler tube is vacuumized, is passed through nitrogen, maintained
Stable nitrogen atmosphere, it is warming up to 700 DEG C respectively from Pre oxidation with 6 centigrade per minutes, is incubated 0.5h;It is last naturally cold
But to producing after room temperature.
Embodiment 2.
A kind of preparation method of carbon nanofiber membrane of the present invention, comprises the following steps:
(1)Take following materials for later use, acrylonitrile, Shanghai Jinshan petrochemical industry Co., Ltd;Dimethylformamide, Chinese medicines group chemistry examination
Agent Co., Ltd, analyze pure, nitrogen, Nanjing Wonder special gas Co., Ltd, deionized water;
(2)PAN is added into DMF, under 30 DEG C of environment, with 600 rpms of 4~6h of stirring and dissolving, obtaining mass fraction is
14% PAN spinning solutions;
(3)At ambient temperature, distance 15cm, 15~18kV of voltage, 0.5 milliliter of flow velocity are received per hour, after continuous electro-spinning 4h
It is standby that PAN fiber film is put into 70 DEG C of oven drying 12h of people;
(4)PAN fiber film is cut into 2 cm x 4cm are rectangular-shaped to be put into Noah's ark;
(5)In air atmosphere, first pre-oxidized in tube furnace, then in a nitrogen atmosphere, rise to 1100 DEG C respectively and enter
Row carbonization;
(6)Pre oxidation is warming up to 3 centigrade per minutes, is incubated 1h;Then boiler tube is vacuumized, is passed through nitrogen, maintained
Stable nitrogen atmosphere, it is warming up to 1100 DEG C respectively from Pre oxidation with 6 centigrade per minutes, is incubated 0.5h;It is last natural
Produced after being cooled to room temperature.
Claims (3)
1. a kind of preparation method of carbon nanofiber membrane, it is characterised in that comprise the following steps:
(1)Take following materials for later use, acrylonitrile, Shanghai Jinshan petrochemical industry Co., Ltd;Dimethylformamide, Chinese medicines group chemistry examination
Agent Co., Ltd, analyze pure, nitrogen, Nanjing Wonder special gas Co., Ltd, deionized water;
(2)PAN is added into DMF, under 30 DEG C of environment, with 600 rpms of 4~6h of stirring and dissolving, obtaining mass fraction is
14% PAN spinning solutions;
(3)At ambient temperature, distance 15cm, 15~18kV of voltage, 0.5 milliliter of flow velocity are received per hour, after continuous electro-spinning 4h
It is standby that PAN fiber film is put into 70 DEG C of oven drying 12h of people;
(4)PAN fiber film is cut into 2 cm x 4cm are rectangular-shaped to be put into Noah's ark;
(5)In air atmosphere, first pre-oxidized in tube furnace, then in a nitrogen atmosphere, rise to respectively 700 DEG C-
1100 DEG C are carbonized;
(6)Pre oxidation is warming up to 3 centigrade per minutes, is incubated 1h;Then boiler tube is vacuumized, is passed through nitrogen, maintained
Stable nitrogen atmosphere, it is warming up to 700 DEG C -1100 DEG C respectively from Pre oxidation with 6 centigrade per minutes, is incubated 0.5h;Most
After naturally cool to room temperature after produce.
A kind of 2. preparation method of carbon nanofiber membrane as is described in the claims, it is characterised in that the step(5)Temperature
It is carbonized for 70 degrees Celsius.
3. a kind of preparation method of carbon nanofiber membrane as is described in the claims, it is characterised in that the nitrogen is with 6 degrees Celsius
It is per minute to be warming up to 1100 DEG C respectively from Pre oxidation.
Priority Applications (1)
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CN201711066851.6A CN107675363A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of carbon nanofiber membrane |
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CN201711066851.6A CN107675363A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of carbon nanofiber membrane |
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CN201711066851.6A Withdrawn CN107675363A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of carbon nanofiber membrane |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109378225A (en) * | 2018-10-31 | 2019-02-22 | 南通纺织丝绸产业技术研究院 | Orderly carbon-based composite electrode material and preparation method thereof |
CN111485328A (en) * | 2020-03-18 | 2020-08-04 | 浙江恒澜科技有限公司 | Preparation method and device of flame-retardant nanofiber composite material |
-
2017
- 2017-11-03 CN CN201711066851.6A patent/CN107675363A/en not_active Withdrawn
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109378225A (en) * | 2018-10-31 | 2019-02-22 | 南通纺织丝绸产业技术研究院 | Orderly carbon-based composite electrode material and preparation method thereof |
CN111485328A (en) * | 2020-03-18 | 2020-08-04 | 浙江恒澜科技有限公司 | Preparation method and device of flame-retardant nanofiber composite material |
CN111485328B (en) * | 2020-03-18 | 2021-06-18 | 浙江恒澜科技有限公司 | Preparation method and device of flame-retardant nanofiber composite material |
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Application publication date: 20180209 |