CN102517693A - Preparation method of aramid-based carbon fiber - Google Patents
Preparation method of aramid-based carbon fiber Download PDFInfo
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- CN102517693A CN102517693A CN2011103690255A CN201110369025A CN102517693A CN 102517693 A CN102517693 A CN 102517693A CN 2011103690255 A CN2011103690255 A CN 2011103690255A CN 201110369025 A CN201110369025 A CN 201110369025A CN 102517693 A CN102517693 A CN 102517693A
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Abstract
The invention relates to a preparation method of aramid-based carbon fiber. The method comprises the following steps of: a, causing a polyisophthaloyl metaphenylene diamide spinning solution to enter coagulating bath through a spinneret plate; stretching with a solvent and washing; and performing dry hot stretching to obtain meta-aramid protofilament; b, stretching the meta-aramid protofilament by a filament guiding machine, and pre-oxidizing the meta-aramid protofilament in oxygen atmosphere of 230-350 DEG C for 2-12 minutes; and c, stretching the meta-aramid protofilament processed by the step b by the filament guiding machine, and performing high-temperature carbonization on the meta-aramid protofilament in nitrogen atmosphere of 400-1,800 DEG C for 2-15 minutes. The method provided by the invention has simple technology; the prepared aramid-based carbon fiber is soft and shiny black; the carbon content is about 95%; the aramid-based carbon fiber strand is 1-24 k, and the tensile strength is stable and reaches 4,900 MPa to the highest; the technological repeatability is high; and the maximum actual carbonization yield is 58%.
Description
Technical field
The present invention relates to a kind of preparation method of carbon fiber, relate in particular to a kind of preparation method of aramid fiber base carbon fibre.
Background technology
Carbon fiber is the excellent new material of a kind of mechanical property.Its proportion is less than 1/4 of steel; Also lighter than aluminium, specific strength is 20 times of iron, and metal materials such as same titanium, steel, aluminium are compared; Carbon fiber has characteristics such as intensity is big, modulus is high, density is low, linear expansion coefficient is little on physical property, can be called " king of new material ".Therefore, carbon fiber is widely used in Leisure Sport fields such as industrial circles such as military industry field, wind power generation blade, GOLF bat such as aircraft manufacturing.
Carbon fiber is except having the characteristic of general carbon materials: high temperature resistant, wear-resisting wiping, conduction, heat conduction and corrosion-resistant etc.; Its profile has significant anisotropism; Softness can be processed into various fabrics, again because proportion is little; Show very high intensity along the fiber axis direction, the specific strength of carbon-fibre reinforced epoxy resin composite material, specific modulus overall target are the highest in the existing structure material.Almost there is not other materials as carbon fiber, to have so much a series of excellent properties at present; The field that therefore strict demand is arranged in purport degree, rigidity, severe, fatigue properties etc.; Requiring high temperature, occasion that chemical stability is high, carbon fibre composite possesses irreplaceable advantage.
In the 21 century that receives the two restrictions of the ecological environment and the energy, asphalt base carbon fiber will increase sustainedly and stably, and becomes the carbon fiber kind that on cost structure, has competitiveness, has very good development prospect.
At present, carbon fiber is mainly made through carbonization by polyacrylonitrile fibre, pitch fibers, viscose or phenolic fibre, and wherein, what consumption was maximum is polyacrylonitrile (PAN) base carbon fibre.But the precursor that is used for making carbon fiber contains a large amount of HO atoms, and the carbonization actual recovery is merely 20-30%.
Summary of the invention
In order to solve the above-mentioned deficiency that prior art exists, technical problem to be solved by this invention provides a kind of preparation method of aramid fiber base carbon fibre, has that technology is simple, with short production cycle, environmental pollution is little, carbonization yield advantages of higher.
For achieving the above object, the technical scheme that the present invention adopts is:
A kind of preparation method of aramid fiber base carbon fibre, be made up of following step:
A, poly (m-phenylene isophthalmide) spinning dope is got into coagulating bath through spinnerets, stretch the back through washing through solvent, the xeothermic stretching of process obtains the meta-aramid precursor again;
B, through guiding machine stretching meta-aramid precursor, place 230-350 ℃ of oxygen atmosphere to carry out pre-oxidation the meta-aramid precursor simultaneously, the time is 2-12min;
C, through the guiding machine meta-aramid precursor after step b handles that stretches, place 400-1800 ℃ of nitrogen atmosphere to carry out high temperature cabonization the meta-aramid precursor simultaneously, the time is 2-15min.
Preferably, poly (m-phenylene isophthalmide) spinning dope described in the step a is the hyposaline spinning solution, and relative viscosity is 2.8-3.3.
Preferably, the solid content of said poly (m-phenylene isophthalmide) spinning dope is 13-18%, and calcium chloride content is 0-0.5%, and N-N dimethylacetylamide content is 81.5-87%.
Preferably, coagulating bath described in the step a is N-N dimethylacetylamide and water second-component system, and wherein, the concentration of coagulating bath is 40-60%, and the temperature of coagulating bath is 30-50 ℃.
Preferably, washing described in the step a is the washings of three roads, and first road, the washing of second road are for embathing, and the washing of the 3rd road is drip washing.
Preferably, extract operation through three road machineries after first road embathes, extract operation through three road machineries after second road embathes.
Preferably, the draw ratio that solvent described in the step a stretches is 1.5-2 times, and the draw ratio of xeothermic stretching is 2.5-4 times.
Preferably, the precursor of meta-aramid described in the step b passes through 230-260 ℃, 260-320 ℃, 320-350 ℃ three temperature subregions successively, and the time is 5-8min.
Preferably, the precursor of meta-aramid described in the step c passes through 400-800 ℃, 800-1200 ℃, 1200-1800 ℃ three temperature subregions successively, and the time is 6-10min, and nitrogen gas purity is 99.999%, adopts the gas positive seal.
The invention solves the defective that exists in the background technology; Technology of the present invention is simple, and the aramid fiber base carbon fibre that makes is soft, shiny black, and phosphorus content is about 95%; Aramid fiber base carbon fibre tow 1-24k; TENSILE STRENGTH is stable and be up to 4900MPa, good process repeatability, and actual carbonization yield is up to 58%.
The specific embodiment
Combine embodiment that the present invention is done further detailed explanation now.
Embodiment 1:
A, will be 2.8 by the relative viscosity that N-N dimethylacetylamide and water second-component system are formed, solid content is 16.8%, calcium chloride content is 0.3%, N-N dimethylacetylamide content be 82.9% poly (m-phenylene isophthalmide) spinning dope through spinnerets get into that concentration is 50%, temperature is 45 ℃ coagulating bath; Stretch 1.8 times after first road embathes, three road machineries are extracted operation, second road embathes, three road machineries are extracted operation, the 3rd road drip washing through solvent; After the drying, obtain the meta-aramid precursor for 3.5 times through xeothermic stretching again;
B, through guiding machine stretching meta-aramid precursor, through 240 ℃, 290 ℃, 330 ℃ three humidity provinces, the time is 6min with the meta-aramid precursor;
C, through the guiding machine meta-aramid precursor after step b handles that stretches, simultaneously with the meta-aramid precursor through 600,1000,1600 ℃ of three humidity provinces, the time is 8min, in purity is to carry out high temperature cabonization under 99.999% the nitrogen protection.Obtain soft, shiny black aramid fiber base carbon fibre, tensile strength of carbon fibers is 3600Mpa, and actual carbonization yield is 52.7%.
Embodiment 2:
A, will be 3.1 by the relative viscosity that N-N dimethylacetylamide and water second-component system are formed, solid content is 16.8%, calcium chloride content is 0.3%, N-N dimethylacetylamide content be 82.9% poly (m-phenylene isophthalmide) spinning dope through spinnerets get into that concentration is 50%, temperature is 45 ℃ coagulating bath; Stretch 1.8 times after first road embathes, three road machineries are extracted operation, second road embathes, three road machineries are extracted operation, the 3rd road drip washing through solvent; After the drying, obtain the meta-aramid precursor for 3.5 times through xeothermic stretching again;
B, through guiding machine stretching meta-aramid precursor, through 250 ℃, 300 ℃, 335 ℃ three humidity provinces, the time is 8min with the meta-aramid precursor;
C, through the guiding machine meta-aramid precursor after step b handles that stretches, simultaneously with the meta-aramid precursor through 700,1150,1600 ℃ of three humidity provinces, the time is 10min, in purity is to carry out high temperature cabonization under 99.999% the nitrogen protection.Obtain soft, shiny black aramid fiber base carbon fibre, tensile strength of carbon fibers is 3800Mpa, and actual carbonization yield is 53.4%.
Above foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification, must confirm technical scope according to the claim scope.
Claims (9)
1. the preparation method of an aramid fiber base carbon fibre is characterized in that, is made up of following step:
A, poly (m-phenylene isophthalmide) spinning dope is got into coagulating bath through spinnerets, stretch the back through washing through solvent, the xeothermic stretching of process obtains the meta-aramid precursor again;
B, through guiding machine stretching meta-aramid precursor, place 230-350 ℃ of oxygen atmosphere to carry out pre-oxidation the meta-aramid precursor simultaneously, the time is 2-12min;
C, through the guiding machine meta-aramid precursor after step b handles that stretches, place 400-1800 ℃ of nitrogen atmosphere to carry out high temperature cabonization the meta-aramid precursor simultaneously, the time is 2-15min.
2. the preparation method of aramid fiber base carbon fibre according to claim 1 is characterized in that: poly (m-phenylene isophthalmide) spinning dope described in the step a is the hyposaline spinning solution, and relative viscosity is 2.8-3.3.
3. the preparation method of aramid fiber base carbon fibre according to claim 2 is characterized in that: the solid content of said poly (m-phenylene isophthalmide) spinning dope is 13-18%, and calcium chloride content is 0-0.5%, and N-N dimethylacetylamide content is 81.5-87%.
4. the preparation method of aramid fiber base carbon fibre according to claim 1 is characterized in that: coagulating bath described in the step a is N-N dimethylacetylamide and water second-component system, and wherein, the concentration of coagulating bath is 40-60%, and the temperature of coagulating bath is 30-50 ℃.
5. the preparation method of aramid fiber base carbon fibre according to claim 1 is characterized in that: washing described in the step a is the washings of three roads, and first road, the washing of second road are for embathing, and the washing of the 3rd road is drip washing.
6. the preparation method of aramid fiber base carbon fibre according to claim 5 is characterized in that: extract operation through three road machineries after first road embathes, extract operation through three road machineries after second road embathes.
7. the preparation method of aramid fiber base carbon fibre according to claim 1 is characterized in that: the draw ratio that solvent described in the step a stretches is 1.5-2 times, and the draw ratio of xeothermic stretching is 2.5-4 times.
8. the preparation method of aramid fiber base carbon fibre according to claim 1 is characterized in that: the precursor of meta-aramid described in the step b passes through 230-260 ℃, 260-320 ℃, 320-350 ℃ three temperature subregions successively, and the time is 5-8min.
9. the preparation method of aramid fiber base carbon fibre according to claim 1; It is characterized in that: the precursor of meta-aramid described in the step c passes through 400-800 ℃, 800-1200 ℃, 1200-1800 ℃ three temperature subregions successively; Time is 6-10min; Nitrogen gas purity is 99.999%, adopts the gas positive seal.
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| CN2011103690255A CN102517693A (en) | 2011-11-21 | 2011-11-21 | Preparation method of aramid-based carbon fiber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396408A (en) * | 2018-01-30 | 2018-08-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of the multistage hole carbon fiber of aramid fiber base enhancing of N doping |
| CN110983494A (en) * | 2019-12-19 | 2020-04-10 | 超美斯新材料股份有限公司 | Preparation method of aramid-based carbon fiber |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3576590A (en) * | 1967-09-22 | 1971-04-27 | Monsanto Co | Sulfur treatment of aromatic polyamide shaped articles |
| US3699210A (en) * | 1968-09-06 | 1972-10-17 | Monsanto Res Corp | Method of graphitizing fibers |
| CN101285214A (en) * | 2008-03-18 | 2008-10-15 | 东华大学 | Preparation of low salt-containing aramid fiber 1313spinning solution and process for spinning fibre by wet method |
-
2011
- 2011-11-21 CN CN2011103690255A patent/CN102517693A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3576590A (en) * | 1967-09-22 | 1971-04-27 | Monsanto Co | Sulfur treatment of aromatic polyamide shaped articles |
| US3699210A (en) * | 1968-09-06 | 1972-10-17 | Monsanto Res Corp | Method of graphitizing fibers |
| CN101285214A (en) * | 2008-03-18 | 2008-10-15 | 东华大学 | Preparation of low salt-containing aramid fiber 1313spinning solution and process for spinning fibre by wet method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396408A (en) * | 2018-01-30 | 2018-08-14 | 东莞市联洲知识产权运营管理有限公司 | A kind of preparation method of the multistage hole carbon fiber of aramid fiber base enhancing of N doping |
| CN110983494A (en) * | 2019-12-19 | 2020-04-10 | 超美斯新材料股份有限公司 | Preparation method of aramid-based carbon fiber |
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Address after: Friendship Industrial Zone Wujiang City Lingzhen Suzhou City, Jiangsu province 215222 Applicant after: SRO ARAMID FIBER (JIANGSU) CO., LTD. Address before: Friendship Industrial Zone Wujiang City Lingzhen Suzhou City, Jiangsu province 215222 Applicant before: Shengou(Suzhou) Safety Protection Material Co., Ltd. |
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Application publication date: 20120627 |