CN116516525A - Low-cost carbon fiber preparation method - Google Patents
Low-cost carbon fiber preparation method Download PDFInfo
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- CN116516525A CN116516525A CN202210239245.4A CN202210239245A CN116516525A CN 116516525 A CN116516525 A CN 116516525A CN 202210239245 A CN202210239245 A CN 202210239245A CN 116516525 A CN116516525 A CN 116516525A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 50
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 50
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003027 oil sand Substances 0.000 claims abstract description 76
- 239000002699 waste material Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000010306 acid treatment Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000002074 melt spinning Methods 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical group CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 10
- 238000010000 carbonizing Methods 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 239000000835 fiber Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000009987 spinning Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000010426 asphalt Substances 0.000 description 12
- 239000011302 mesophase pitch Substances 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000011295 pitch Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses a low-cost carbon fiber preparation method, which relates to the technical field of new chemical materials, and comprises the steps of taking oil sand or heavy component raw materials in oil sand waste as a carbon source, evaporating the obtained asphaltene, performing heat treatment at 200-400 ℃, performing melt spinning after the heat treatment, and performing acid treatment, oxidation treatment and carbonization treatment to obtain the asphaltene carbon fiber; the heavy component raw materials comprise asphaltenes and also comprise various heavy components obtained by other methods. The prepared high-performance low-cost oil sand and oil sand waste carbon fiber has high mechanical strength, controllable element content, stable spinning process and low cost, and is easy to industrially popularize.
Description
Technical Field
The invention relates to the technical field of new chemical materials, in particular to a low-cost carbon fiber preparation method.
Background
Heavy components in oil sands and oil sand waste materials are of great interest because of their extremely low cost and very abundant sources. The heavy components in the oil sand and the oil sand waste contain a large amount of flaky condensed ring olefins with relatively high molecular mass, aromatic cyclizing degree and heat stability, the olefins can just form a mesophase pitch molecule flaky structure unit through simple cyclization and polycondensation reaction, and the mesophase pitch molecule is a high-quality precursor for producing high-modulus high-heat-conductivity carbon fibers. It is particularly pointed out that the price of asphaltenes, which are rich in carbon components in oil sands and oil sand waste materials, is only $0.02/pound, which is about 1/150 to 1/300 of the price of PAN raw materials ($3 to 6/pound), and thus has great development potential. As the component with the highest relative molecular mass in the crude oil system, the asphaltene has the basic characteristics of strong polarity and high aromaticity, and has low H/C atomic ratio (1:1-1.2:1), thereby being very beneficial to the production and manufacture of high-performance carbon fibers.
Patent CN111363577B discloses a preparation method of coal-series general-purpose asphalt carbon fiber, which has the characteristics of environmental protection, simple process flow and the like. Patent CN111575052B provides a novel method for preparing mesophase pitch and high modulus pitch-based carbon fibers using heavy oil, which can obtain a wide area streamline optical anisotropic mesophase structure having a large area, and has good spinnability, and is suitable for preparing high modulus mesophase pitch-based carbon fibers. The patent CN106929084B adopts petroleum asphalt to prepare spinnable mesophase pitch, and is suitable for preparing high-performance carbon fibers. The patent CN113637147A adopts aromatic compounds, concentrated hydrochloric acid, glacial acetic acid, paraformaldehyde and a catalyst to react after being mixed to obtain the synthetic asphalt, and has the characteristics of low raw material price, high reaction conversion rate and the like. Patent CN113801673a discloses a production method of high-temperature impregnating asphalt, the invention can obviously improve the softening point of asphalt, narrow molecular weight distribution, reduce volatile components, and the obtained high-temperature impregnating asphalt has better wettability and impregnating effect. Patent CN113621130a discloses a preparation method of high-quality asphalt, which is cheap and easy to obtain, has mild reaction conditions and excellent spinnability, and is beneficial to preparing high-quality asphalt-based carbon fiber products. The patent CN112608760B adopts heavy oil to prepare mesophase pitch under the condition of microwave heating, so that materials are heated uniformly, coking is avoided, and the invention has the advantages of high mesophase content, uniform mesophase structure distribution and the like. The patent CN113549466A obtains high-quality mesophase pitch by adopting the procedures of extractive distillation, extractant separation, entrainer separation, thermal polycondensation reaction and the like on pitch raw materials.
The above patents disclose various pitch-based carbon fiber production and preparation techniques, but do not relate to the process technology of producing carbon fibers from oil sand or heavy components in oil sand waste.
Disclosure of Invention
Aiming at the technical problems, the invention overcomes the defects of the prior art and provides a low-cost carbon fiber preparation method, which takes oil sand or heavy component raw materials in oil sand waste as a carbon source, evaporates the obtained asphaltene, carries out heat treatment at 200-400 ℃, carries out melt spinning after the heat treatment, and then carries out acid treatment, oxidation treatment and carbonization treatment to obtain the asphaltene carbon fiber; the heavy component raw materials comprise asphaltenes and also comprise various heavy components obtained by other methods.
The technical scheme of the invention is as follows:
the preparation method of the low-cost carbon fiber specifically comprises the following steps:
s1, grinding heavy components in massive oil sand or oil sand waste into fine powder, treating by a solvent deasphalting method, and carrying out suction filtration and drying on the heavy components in the obtained oil sand or oil sand waste;
s2, carrying out heat treatment on heavy components in the dried oil sand or oil sand waste, controlling the temperature at 200-400 ℃, and keeping inert gas introduced in the heat treatment process;
s3, carrying out melt spinning on the raw materials subjected to heat treatment, wherein the temperature is controlled at 160-260 ℃ and the speed is controlled at 100-200 rpm;
s4, carrying out acid treatment on the obtained precursor;
s5, oxidizing and carbonizing the fibers subjected to the acid treatment, wherein the oxidizing is carried out for 0.1-10 h under the air atmosphere at the temperature of 250-350 ℃, and the carbonizing is carried out for 0.1-10 h under the inert gas atmosphere at the temperature of 1000-1500 ℃.
In the aforementioned low-cost carbon fiber preparation method, in step S1, the ratio of the solvent to the heavy component in the oil sand or the oil sand waste is 100:1-1:1.
In the preparation method of the low-cost carbon fiber, pentane or heptane is adopted as the solvent.
The solvent deasphalting method is a method for separating out or precipitating asphaltenes from various alkanes.
In the aforementioned low-cost carbon fiber preparation method, in step S4, the acid treatment is performed in nitric acid or sulfuric acid solution, and the volume fraction of nitric acid or sulfuric acid is 1% -50%.
According to the low-cost carbon fiber preparation method, the element content of the obtained carbon fiber is regulated by oxygen partial pressure in the following manner: 2vol%, 10vol% and 40vol% oxygen pressure bottles with different compositions are introduced, and 21vol% oxygen partial pressure condition is replaced by compressed air.
The beneficial effects of the invention are as follows:
(1) The invention overcomes the defects of large component discreteness, discontinuous spinning, high cost and the like of the traditional asphalt carbon fiber, prepares the high-performance low-cost oil sand and heavy component carbon fiber in the oil sand waste by pretreating the heavy component in the low-cost oil sand and the oil sand waste and then carrying out melt spinning and a series of treatment processes, and has the advantages of high mechanical strength, controllable element content, stable spinning process and low cost, and is easy for industrialized popularization compared with the traditional asphalt carbon fiber;
(2) The tensile strength of the heavy component carbon fiber in the oil sand and the oil sand waste material is 1000-3000 MPa, and the Young modulus is 50-250 GPa;
(3) After the heavy component carbon fibers in the oil sand and the oil sand waste material are subjected to different carbonization temperatures, the H/C molar ratio is less than or equal to 0.02, and NOS/C is less than or equal to 0.07;
(4) The weight loss of heavy component fiber precursor in the oil sand and the oil sand waste obtained by the invention is less than or equal to 10wt% when the temperature is below 400 ℃;
(5) The element content of the heavy component carbon fiber in the oil sand and the oil sand waste can be adjusted through the partial pressure of oxygen, thereby being beneficial to further optimizing the mechanical property in the carbonization process.
Drawings
FIG. 1 is an example of a low cost carbon fiber precursor prepared from heavy components in a typical oil sand or oil sand waste;
FIG. 2 is an example of a low cost fine denier carbon fiber produced from heavy components in a typical oil sand or oil sand waste;
FIG. 3 is a typical filament thermogravimetric plot;
FIG. 4 is a graph showing the molar ratio NOS/C as a function of oxygen partial pressure;
FIG. 5 is a graph of H/C molar ratio as a function of partial pressure of oxygen;
FIG. 6 is a graph showing the change in the O/C molar ratio with the partial pressure of oxygen.
Detailed Description
Example 1
The preparation method of the low-cost carbon fiber provided by the embodiment specifically comprises the following steps:
s1, grinding heavy components in massive oil sand or oil sand waste into fine powder, treating by a solvent deasphalting method, and carrying out suction filtration and drying on the heavy components in the obtained oil sand or oil sand waste by adopting pentane and the proportion of the heavy components in the oil sand or oil sand waste is 80:1-10:1 as a solvent;
s2, carrying out heat treatment on heavy components in the dried oil sand or oil sand waste, controlling the temperature at 200-400 ℃, and keeping nitrogen gas introduced in the heat treatment process;
s3, carrying out melt spinning on the raw materials subjected to heat treatment, wherein the temperature is controlled to be 180-250 ℃, and the speed is controlled to be 100-200 rpm;
s4, performing acid treatment on the obtained precursor, wherein the acid treatment is performed in a sulfuric acid solution, and the volume fraction of sulfuric acid is 10%;
s5, oxidizing and carbonizing the fibers subjected to the acid treatment, wherein the oxidizing is carried out for 1-6 hours in an air atmosphere at the temperature of 250-350 ℃, and the carbonizing is carried out for 1-5 hours in an inert gas atmosphere at the temperature of 800-1000 ℃.
The obtained carbon fiber has excellent mechanical property, high carbon content, tensile strength up to 600-800 MPa and Young's modulus up to 40-70 GPa.
Example 2
The preparation method of the low-cost carbon fiber provided by the embodiment specifically comprises the following steps:
s1, grinding heavy components in massive oil sand or oil sand waste into fine powder, treating by a solvent deasphalting method, wherein pentane is adopted as a solvent, the proportion of the pentane to the heavy components in the oil sand or oil sand waste is 80:1-10:1, and performing suction filtration and drying on the heavy components in the obtained oil sand or oil sand waste;
s2, carrying out heat treatment on heavy components in the dried oil sand or oil sand waste, controlling the temperature at 200-400 ℃, and keeping nitrogen gas introduced in the heat treatment process;
s3, carrying out melt spinning on the raw materials subjected to heat treatment, wherein the temperature is controlled to be 200-250 ℃, and the speed is controlled to be 100-200 rpm;
s4, performing acid treatment on the obtained precursor, wherein the acid treatment is performed in a nitric acid solution, and the volume fraction of nitric acid is 10%;
s5, oxidizing and carbonizing the fibers subjected to the acid treatment, wherein the oxidizing is carried out for 1-5 hours in an air atmosphere at the temperature of 250-300 ℃, and the carbonizing is carried out for 1-6 hours in an inert gas atmosphere at the temperature of 800-1200 ℃.
The obtained carbon fiber has excellent mechanical property, high carbon content, tensile strength up to 800-1000 MPa and Young's modulus up to 50-80 GPa.
Example 3
The preparation method of the low-cost carbon fiber provided by the embodiment specifically comprises the following steps:
s1, grinding heavy components in massive oil sand or oil sand waste into fine powder, treating by a solvent deasphalting method, wherein the ratio of the solvent to the heavy components in the oil sand or oil sand waste is 80:1-10:1, and performing suction filtration and drying on the heavy components in the obtained oil sand or oil sand waste;
s2, carrying out heat treatment on heavy components in the dried oil sand or oil sand waste, controlling the temperature at 200-400 ℃, and keeping nitrogen gas introduced in the heat treatment process;
s3, carrying out melt spinning on the raw materials subjected to heat treatment, wherein the temperature is controlled to be 200-230 ℃ and the speed is controlled to be 100-200 rpm;
s4, performing acid treatment on the obtained precursor, wherein the acid treatment is performed in a nitric acid solution, and the volume fraction of nitric acid is 10%;
s5, oxidizing and carbonizing the fibers subjected to the acid treatment, wherein the oxidizing is carried out for 1-6 hours in an air atmosphere at the temperature of 250-350 ℃, and the carbonizing is carried out for 1-5 hours in an inert gas atmosphere at the temperature of 800-1000 ℃.
The obtained carbon fiber has excellent mechanical property, high carbon content, tensile strength up to 800-1200 MPa and Young's modulus up to 80-100 GPa.
TABLE 1 variation of fiber elements with carbonization temperature
As is clear from Table 1, the hetero atoms contained in the fiber filaments were substantially removed by the different carbonization temperatures, NOS/C was as low as 0.024wt%, and H/C was as low as 0.
As shown in FIG. 1, the fibril developed by the present invention has smooth surface and no obvious defect.
As shown in figure 2, the carbon fiber developed by the invention is uniform and straight, and has no obvious uneven thickness.
As shown in figure 3, before the temperature of 400 ℃, the asphaltene fiber does not find a large-scale weightlessness decomposition phenomenon, so that the stability of an oxidation treatment temperature range is ensured.
As shown in fig. 4, 5 and 6, the present invention can adjust the relative proportions of elements by partial pressure of oxygen. The relative NOS/C ratio increases with increasing oxygen partial pressure, while H/C, O/C decreases with increasing oxygen partial pressure.
The heavy components in the oil sand and the oil sand waste are high-performance carbon fibers which are obtained by taking substances rich in polycyclic aromatic hydrocarbon in petroleum asphalt as raw materials and carrying out fine modulation, spinning, acid treatment, oxidation and carbonization treatment, have the excellent characteristics of high strength, high modulus, high temperature resistance, corrosion resistance, fatigue resistance, creep resistance, high electric conduction and heat conduction and the like, can meet the market diversity requirements, and are expected to be widely applied to various fields of aerospace, sports and leisure, transportation, civil construction and the like. Compared with asphalt carbon fibers, the mechanical properties of the carbon fibers prepared from the heavy components in the oil sand and the oil sand waste mainly depend on the pre-treatment process, and the spinning performance and the mechanical properties of the heavy components in the oil sand and the oil sand waste are greatly improved after the pretreatment, so that the process flow is short and the industrial popularization is easy.
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (7)
1. A preparation method of low-cost carbon fiber is characterized in that: taking oil sand or heavy component raw materials in oil sand waste as a carbon source, evaporating the obtained asphaltene, performing heat treatment at 200-400 ℃, performing melt spinning after the heat treatment, and performing acid treatment, oxidation treatment and carbonization treatment to obtain the asphaltene carbon fiber; the heavy component raw materials comprise asphaltenes and also comprise various heavy components obtained by other methods.
2. The method for preparing the low-cost carbon fiber according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
s1, grinding heavy components in massive oil sand or oil sand waste into fine powder, treating by a solvent deasphalting method, and carrying out suction filtration and drying on the heavy components in the obtained oil sand or oil sand waste;
s2, carrying out heat treatment on heavy components in the dried oil sand or oil sand waste, controlling the temperature at 200-400 ℃, and keeping inert gas introduced in the heat treatment process;
s3, carrying out melt spinning on the raw materials subjected to heat treatment, wherein the temperature is controlled at 160-260 ℃ and the speed is controlled at 100-200 rpm;
s4, carrying out acid treatment on the obtained precursor;
s5, oxidizing and carbonizing the fibers subjected to the acid treatment, wherein the oxidizing is carried out for 0.1-10 h under the air atmosphere at the temperature of 250-350 ℃, and the carbonizing is carried out for 0.1-10 h under the inert gas atmosphere at the temperature of 1000-1500 ℃.
3. The method for preparing the low-cost carbon fiber according to claim 2, wherein: the ratio of the solvent to the oil sand or the heavy components in the oil sand waste in the step S1 is 100:1-1:1.
4. A method of producing a low cost carbon fiber according to claim 3, wherein: the solvent is pentane or heptane.
5. The method for preparing the low-cost carbon fiber according to claim 2, wherein: the solvent deasphalting method is a method of precipitating or precipitating asphaltenes by various alkanes.
6. A method for producing a low-cost carbon fiber according to claim 1 or 2, characterized in that: and step S4, the acid treatment is performed in a nitric acid or sulfuric acid solution, and the volume fraction of the nitric acid or sulfuric acid is 1-50%.
7. A method for producing a low-cost carbon fiber according to claim 1 or 2, characterized in that: the element content of the obtained carbon fiber is regulated by oxygen partial pressure in the following way: 2vol%, 10vol% and 40vol% oxygen pressure bottles with different compositions are introduced, and 21vol% oxygen partial pressure condition is replaced by compressed air.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210239245.4A CN116516525A (en) | 2022-03-09 | 2022-03-09 | Low-cost carbon fiber preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210239245.4A CN116516525A (en) | 2022-03-09 | 2022-03-09 | Low-cost carbon fiber preparation method |
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| CN202210239245.4A Pending CN116516525A (en) | 2022-03-09 | 2022-03-09 | Low-cost carbon fiber preparation method |
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