CN107675363A - A kind of preparation method of carbon nanofiber membrane - Google Patents

A kind of preparation method of carbon nanofiber membrane Download PDF

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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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CN
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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Application number
CN201711066851.6A
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Chinese (zh)
Inventor
李长英
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Shaanxi Yipinda Petrochemical Co Ltd
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Shaanxi Yipinda Petrochemical Co Ltd
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Publication date
Application filed by Shaanxi Yipinda Petrochemical Co Ltd filed Critical Shaanxi Yipinda Petrochemical Co Ltd
Priority to CN201711066851.6A priority Critical patent/CN107675363A/en
Publication of CN107675363A publication Critical patent/CN107675363A/en
Withdrawn legal-status Critical Current

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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/42Non-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
    • D04H1/4282Addition polymers
    • D04H1/43Acrylonitrile series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-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
    • D04H1/72Non-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
    • D04H1/728Non-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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06CFINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00Heating or cooling textile fabrics
    • D06C7/04Carbonising 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

A kind of preparation method of carbon nanofiber membrane
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.
CN201711066851.6A 2017-11-03 2017-11-03 A kind of preparation method of carbon nanofiber membrane Withdrawn CN107675363A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711066851.6A CN107675363A (en) 2017-11-03 2017-11-03 A kind of preparation method of carbon nanofiber membrane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711066851.6A CN107675363A (en) 2017-11-03 2017-11-03 A kind of preparation method of carbon nanofiber membrane

Publications (1)

Publication Number Publication Date
CN107675363A true CN107675363A (en) 2018-02-09

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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)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
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