CN110029488A - A kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure - Google Patents
A kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure Download PDFInfo
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- CN110029488A CN110029488A CN201910191729.4A CN201910191729A CN110029488A CN 110029488 A CN110029488 A CN 110029488A CN 201910191729 A CN201910191729 A CN 201910191729A CN 110029488 A CN110029488 A CN 110029488A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0067—Inorganic membrane manufacture by carbonisation or pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- 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
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
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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
- D04H1/70—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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The present invention relates to a kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure.The present invention carries out liquid phase oxidation to raw coal using nitration mixture and obtains oxidized coal powder, and oxidized coal and polyacrylonitrile are dissolved in n,N-Dimethylformamide and are made into spinning solution；Spinning solution is spun by tunica fibrosa using method of electrostatic spinning, tunica fibrosa is pre-oxidized in air atmosphere；By chemical vapour deposition technique, pitch cracking is deposited on carbon fiber surface, the super-hydrophobic carbon-fiber film with nucleocapsid structure is obtained through high temperature carbonization.The water contact angle of gained carbon-fiber film is up to 159.5 °, and roll angle can keep ultra-hydrophobicity in strong acid, highly basic and organic solvent environment less than 3 ° for a long time.Gained carbon-fiber film of the invention has stronger oil and water separation capability, can be applied to the processing of oily waste water.
Description
Technical field
A kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure.
Background technique
Carbon fibre material has many advantages, such as that light weight, intensity height, high temperature resistant, anticorrosive, thermal conductivity is good, is answered extensively
With in the industries such as aerospace, automobile manufacture, sports goods.Currently, the method for preparing carbon fiber includes pulling method, mutually separates
Method, matrix polymerization method, self-assembly method and method of electrostatic spinning etc..Wherein, electrostatic spinning technique has easy to operate, fibre morphology
And the advantages that controlled diameter, it has also become prepare the main method of carbon fibre material.With the continuous progress of science and technology and people's lives
Horizontal continuous improvement, the super-hydrophobic carbon fiber with special wettability is in the row such as coal chemical industry, food processing, medicine, printing and dyeing
Industry has huge application prospect.Super-hydrophobic phenomenon, just advantageously, it has been found that lotus leaf is exactly a Typical Representative, passes through at thousands of years
To the further investigation of solid-liquid-gas three phase boundary, researcher sums up two main paths for preparing super hydrophobic material, first is that
Increase material roughness, second is that reducing the surface energy of material.Currently, super hydrophobic material is mostly with polyacrylonitrile (PAN), polyethylene
The high molecular polymers such as alcohol (PVA), polyvinylpyrrolidone (PVP), Kynoar (PVDF) are raw material, super-hydrophobic to realize
Performance usually requires to be modified with low surface energy compounds such as fluorine-containing or siloxanes.For example, 2011, Harbin industry is big
Jiang Zaixing, Huang Yudong et al. have invented " preparation method of super-hydrophobic carbon fiber fabric " (Chinese patent, Patent No.
CN102094324A), it was recently reported that a kind of preparation of the super-hydrophobic carbon fiber fabric of one strata perfluoroalkylsilane of surface covering
Method.
The super hydrophobic material reported at present may be implemented ultra-hydrophobicity under relatively mild conditions, but in strong acid, strong
Under the conditions of alkali, high temperature and organic solvent, the ultra-hydrophobicity of material just be cannot keep.In contrast, carbon fiber has acidproof, resistance to
The good characteristics such as alkali, high temperature resistant.Therefore, the super-hydrophobic carbon fiber tool that can be used under complicated, harsh industrial environment is prepared
There is important practical application value.
The present invention combines method of electrostatic spinning and chemical vapour deposition technique, does not need the object for modifying any low-surface-energy
Matter is prepared for a kind of super-hydrophobic carbon-fiber film that can be used under the environment such as strong acid, highly basic, high temperature, organic solvent.
Detailed description of the invention
Fig. 1 has the X-ray powder diffraction figure of the super-hydrophobic carbon-fiber film of nucleocapsid structure.
The transmission electron microscope photo of Fig. 2 carbon-fiber film.
Contact angle photo of Fig. 3 water droplet on carbon-fiber film.
The super-hydrophobic carbon-fiber film of Fig. 4 impregnated one month in different corrosive liquids after contact angle test.
Fig. 5 carries out water-oil separating using carbon-fiber film.
Summary of the invention
Asking for ultra-hydrophobicity can not be kept under strong acid, highly basic and high temperature for the super hydrophobic material reported at present
Topic, an object of the present invention are just to provide a kind of carbon fiber that ultra-hydrophobicity can be able to maintain in complicated and harsh environment
Tie up film.Another object of the present invention is just to provide a kind of without the super of the low-surface energy substances such as fluorine reagent, silane reagent modification
The preparation method of hydrophobic carbon fiber film.
The present invention provides a kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure, preparation step tool
Body is as follows:
(1) liquid phase oxidation is carried out to raw coal using nitration mixture (volume ratio of the concentrated sulfuric acid and concentrated nitric acid be 3:1), then by filtering,
Drying and grinding obtain oxidized coal powder；
(2) 0.8 gram of oxidized coal is weighed respectively and 0.8 gram of polyacrylonitrile powder (PAN) is dissolved in 10 milliliters of N, N- dimethyl
In formamide (DMF), by stirring and standing obtains uniform spinning solution, spinning solution is spun by fiber using method of electrostatic spinning
Film；
(3) tunica fibrosa is warming up to 280 DEG C in Muffle furnace with 2 DEG C/min, heat preservation is pre-oxidized for 1 hour, then naturally cold
But to room temperature；
(4) by chemical vapour deposition technique, pitch cracking is deposited on carbon fiber surface at 500 DEG C, keeps the temperature 1 hour, then
2 hours are kept the temperature at 1000 DEG C, the super-hydrophobic carbon-fiber film with nucleocapsid structure is obtained after natural cooling.
Compared with prior art, the resulting super-hydrophobic carbon-fiber film of the present invention has the advantages that
1. preparation process is simple, the raw materials such as pitch, coal are cheap and easy to get, are suitable for large-scale production.
2. only relying on the architectural characteristic of carbon-fiber film itself without the modification of the low-surface energy substances such as fluorine reagent, silane reagent
Ultra-hydrophobicity can be realized, the contact angle of gained tunica fibrosa is up to 159.5 °, and roll angle is less than 3 °.
3. super-hydrophobic carbon-fiber film prepared by can be kept for a long time in strong acid, highly basic and organic solvent environment
Ultra-hydrophobicity, by carbon-fiber film in 10M H2SO4, 6M KOH, acetone and saturation NaCl in impregnate 30 days, carbon-fiber film connects
Feeler is still greater than 150 °.
4. gained carbon-fiber film of the invention has stronger oil and water separation capability, the processing of oily waste water can be applied to.
Claims (7)
1. a kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure, it is characterised in that preparation method include with
Lower step:
Raw coal is prepared oxidized coal by nitration mixture oxidation by step 1；
Oxidized coal and polyacrylonitrile are dissolved in n,N-Dimethylformamide by step 2, are configured to after stirring, standing quiet
Electrospun liquid；
Spinning solution is spun into tunica fibrosa by method of electrostatic spinning by step 3；
Step 4 carries out pre-oxidation treatment to fiber membrane；
Step 5 is deposited on fiber film surface after cracking pitch by chemical vapour deposition technique, then carry out charcoal at high temperature
Change.
2. preparation method according to claim 1, which is characterized in that in the step 1, nitration mixture is the concentrated sulfuric acid and concentrated nitric acid
By the volume ratio mixed preparing of 3:1；Oxidized coal is that raw coal is added in nitration mixture to aoxidize, and then filters, dries and grind.
3. preparation method according to claim 1, which is characterized in that in the step 2, by 0.8 gram of oxidized coal and 0.8
Gram polyacrylonitrile is dissolved in 10 milliliters of N,N-dimethylformamides；8 hours are stood again after stirring 12 hours at room temperature.
4. preparation method according to claim 1, which is characterized in that in the step 3, the spinning parameter of tunica fibrosa is arranged
As follows: 18 Kv of positive high voltage, -2.5 Kv of negative high voltage, 0.4 millimeter of syringe needle internal diameter, the speed of injecting of spinning solution is 0.1 milli m/min
Clock, receiving the distance between roller and syringe needle is 20 centimetres, receives 100 revs/min of drum rotation speed, spinning temperature is 25 DEG C.
5. preparation method according to claim 1, which is characterized in that in the step 4, in air atmosphere, with 2 DEG C/
The heating rate of min is warming up to 280 DEG C, pre-oxidizes 1 hour to tunica fibrosa.
6. preparation method according to claim 1, which is characterized in that in the step 5, the chemical vapor deposition ginseng
Number, which is provided that, is warming up to 500 DEG C with 2 DEG C/min, and 8 grams of pitch cracking are deposited on 12 × 6 centimetres of carbon-fiber film surfaces,
Heat preservation 1 hour；Then 1000 DEG C are warming up to 5 DEG C/min, cooled to room temperature after soaking time 2 hours.
7. preparation method according to claim 1, which is characterized in that the diameter of the carbon fiber is 350-550 nanometers,
The thickness of shell is at 50-100 nanometers, and the water contact angle of carbon-fiber film is 159.5 °, and roll angle is less than 3 °.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910191729.4A CN110029488A (en) | 2019-03-14 | 2019-03-14 | A kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910191729.4A CN110029488A (en) | 2019-03-14 | 2019-03-14 | A kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure |
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| CN110029488A true CN110029488A (en) | 2019-07-19 |
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| CN201910191729.4A Pending CN110029488A (en) | 2019-03-14 | 2019-03-14 | A kind of super-hydrophobic carbon-fiber film and preparation method thereof with nucleocapsid structure |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113005775A (en) * | 2021-03-02 | 2021-06-22 | 山东招金膜天股份有限公司 | Preparation method of porous super-hydrophobic carbon fiber membrane suitable for severe environment |
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| US20030098237A1 (en) * | 2001-11-28 | 2003-05-29 | 3M Innovative Properties Company | Fuel cell gas diffusion layer coating process and treated article |
| CN101830098A (en) * | 2010-05-07 | 2010-09-15 | 中国人民解放军国防科学技术大学 | Polymer-matrix composite material with super-hydrophobic surface and preparation method thereof |
| CN102019996A (en) * | 2010-11-23 | 2011-04-20 | 哈尔滨工业大学 | Preparation method for extra hydrophobic carbon fabric boat |
| CN107988660A (en) * | 2017-11-14 | 2018-05-04 | 哈尔滨工业大学深圳研究生院 | A kind of thermal chemical vapor deposition prepares the method and its application of three-dimensional grapheme fiber |
-
2019
- 2019-03-14 CN CN201910191729.4A patent/CN110029488A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030098237A1 (en) * | 2001-11-28 | 2003-05-29 | 3M Innovative Properties Company | Fuel cell gas diffusion layer coating process and treated article |
| CN101830098A (en) * | 2010-05-07 | 2010-09-15 | 中国人民解放军国防科学技术大学 | Polymer-matrix composite material with super-hydrophobic surface and preparation method thereof |
| CN102019996A (en) * | 2010-11-23 | 2011-04-20 | 哈尔滨工业大学 | Preparation method for extra hydrophobic carbon fabric boat |
| CN107988660A (en) * | 2017-11-14 | 2018-05-04 | 哈尔滨工业大学深圳研究生院 | A kind of thermal chemical vapor deposition prepares the method and its application of three-dimensional grapheme fiber |
Non-Patent Citations (1)
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| 宋贤丽: "煤基碳纳米纤维复合材料的制备及其在超级电容器中的应用", 《中国优秀硕士学位论文全文数据库 (工程科技Ⅰ辑)》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113005775A (en) * | 2021-03-02 | 2021-06-22 | 山东招金膜天股份有限公司 | Preparation method of porous super-hydrophobic carbon fiber membrane suitable for severe environment |
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Application publication date: 20190719 |