CN115341308B - Continuous production method for preparing polyacrylonitrile spinning solution by X-ray irradiation - Google Patents
Continuous production method for preparing polyacrylonitrile spinning solution by X-ray irradiation Download PDFInfo
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- 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
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/04—Polymerisation in solution
- C08F2/06—Organic solvent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/54—Polymerisation initiated by wave energy or particle radiation by X-rays or electrons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention discloses a continuous production method for preparing a polyacrylonitrile spinning solution by using X-ray irradiation, which relates to the technical field of polyacrylonitrile processing, and comprises the steps of firstly putting acrylonitrile, vinyl comonomer and solvent into a mixing kettle, simultaneously introducing inert gas to deoxidize, stirring and mixing, metering the obtained mixed solution into a tubular reactor, putting the tubular reactor into an electron beam irradiation device, and performing polymerization reaction by using the X-ray irradiation mixed solution generated by an electron beam conversion target to obtain the polyacrylonitrile spinning solution; the polyacrylonitrile spinning solution prepared by the invention can be directly conveyed to a spinning production line, and is subjected to dry-jet wet spinning or wet spinning by a spinning metering pump, and the carbon fiber precursor is obtained by molding.
Description
Technical field:
the invention relates to the technical field of polyacrylonitrile processing, in particular to a continuous production method for preparing a polyacrylonitrile spinning solution by using X-ray irradiation.
The background technology is as follows:
the polyacrylonitrile-based carbon fiber has the excellent performances of light weight, high specific strength and specific rigidity, good fatigue resistance, corrosion resistance, strong designability and the like, and is widely applied to various fields of national economy such as aerospace, transportation, sports and leisure, building reinforcement and the like.
At present, in the field of polyacrylonitrile precursor preparation for carbon fibers, the preparation of polyacrylonitrile spinning solution is almost produced by adopting a chemical initiator method. Patent CN106591995a provides a method for preparing a spinning dope, the chemical initiator added affects the purity of the product, the decomposition of the initiator also reduces the molecular weight of the product and adversely affects the thermal properties of the product. In addition, the chemical initiator method is used for producing the polyacrylonitrile spinning solution, the reaction period is as long as 10-15 h, and the production efficiency is low.
The polyacrylonitrile spinning solution can also be prepared by adopting two irradiation processes of cobalt 60 gamma-ray irradiation or electron beam target-transferring X-ray irradiation. The two methods do not need extra heat source and chemical initiator, and have the advantages of controllable conditions, mild reaction, high production efficiency and the like.
Yang Tingting (chemical engineering new material, 2022,50 (6): 126-130) and using cobalt 60 gamma-ray to irradiate and polymerize acrylonitrile in organic solvent to obtain polyacrylonitrile with high relative molecular mass, the optimum irradiation time is 80min. The patent CN202111104302.X uses cobalt 60 gamma-ray solvent radiation method to prepare high-quality polyacrylonitrile copolymer, and the production efficiency is lower because the radiation time is long and the batch method is used for production.
TABLE 1 differentiation of Electron Beam and gamma rays
As shown in table 1 (refer to shandong agricultural science, 2009 (12): 102-104.), the electron beam irradiation method is safe and reliable, pollution-free and low in running cost, and the high-energy electron beam can be converted into X-rays having a higher penetrating power. The patent CN202210338864.9 utilizes an electron beam transfer target X-ray radiation polymerization method to rapidly irradiate and initiate the aqueous solution of acrylonitrile and comonomer at room temperature to form heterogeneous precipitation copolymerization reaction, and has the advantages of extremely short irradiation reaction time of only 10-120 s, continuous production and production efficiency far higher than that of a cobalt 60 gamma-ray irradiation method. Although the irradiation time of the process is extremely short and the process is continuous, the disadvantage is that the reaction product needs to be subjected to multiple processes such as precipitation, filtration, drying, screening, crushing and the like to prepare powder, and the powder needs to be dissolved and filtered by an organic or inorganic solvent before use to prepare the polyacrylonitrile spinning solution for spinning, so that the whole operation process is long, and the subsequent spinning period is prolonged.
The invention comprises the following steps:
one of the technical problems to be solved by the invention is that when the polyacrylonitrile stock solution is prepared by adopting a chemical polymerization method in the prior art, a chemical initiator is added to influence the purity, molecular weight and thermal performance of the product, the reaction temperature is high, the reaction time is long, and the production efficiency is low; the cobalt 60 gamma-ray radiation method is adopted to improve the purity of the product, the reaction is carried out at normal temperature, the reaction time is also greatly shortened, but compared with the electron beam target-rotating X-ray radiation method, the method belongs to batch method production, the reaction time is still longer, and the production efficiency is not high. The invention provides a continuous production method for preparing polyacrylonitrile spinning solution by using X-ray irradiation, which has extremely short reaction time, realizes continuous production and greatly improves production efficiency.
The second technical problem to be solved by the invention is that in the prior art, a solvent method is adopted to prepare the polyacrylonitrile stock solution, and the solvent method is adopted to produce the polyacrylonitrile stock solution in a kettle type intermittent method due to extremely high viscosity. The invention provides a continuous production method for preparing a polyacrylonitrile spinning solution by using a tubular reactor and using X-ray irradiation, wherein a stirring component and the inner wall of an inner chamber of the tubular reactor are both adhered with a polytetrafluoroethylene coating, so that the flow resistance of a polyacrylonitrile stock solution in the reactor is effectively reduced, the continuous production can be realized by using an air compressor to pressurize and pump, and the production efficiency is greatly improved.
The third technical problem to be solved by the invention is that in the water phase precipitation polymerization method for preparing polyacrylonitrile by electron beam X-ray irradiation in the prior art, although continuous production can be realized by using a tubular reactor, the reaction product needs to be subjected to complex procedures of demulsification, precipitation, drying, crushing, sieving and the like to prepare powder; before spinning, the powder is swelled, dissolved and filtered by solvent to obtain polyacrylonitrile spinning solution, which is a two-step process with complex production operation. The invention provides a continuous production method for preparing a polyacrylonitrile spinning solution by using X-ray irradiation, the obtained polyacrylonitrile spinning solution can be directly used for dry-jet wet spinning or solution spinning without secondary dissolution, one-step rapid spinning is realized, spinning productivity is improved, production cost is reduced, and energy-saving, environment-friendly and green production is realized.
The invention aims to provide a continuous production method for preparing a polyacrylonitrile spinning solution by using X-ray irradiation, which comprises the steps of firstly putting acrylonitrile, vinyl comonomer and solvent into a mixing kettle, simultaneously introducing inert gas to deoxidize, stirring and mixing, metering the obtained mixed solution into a tubular reactor, putting the tubular reactor into an electron beam irradiation device, and performing polymerization reaction by using the X-ray irradiation mixed solution generated by an electron beam conversion target to obtain the polyacrylonitrile spinning solution.
And directly conveying the polyacrylonitrile spinning solution to a spinning production line, carrying out dry-jet wet spinning or wet spinning by a spinning metering pump, and forming to obtain the carbon fiber precursor.
Preferably, the solvent is organic solvent or inorganic solvent, the organic solvent is one or more of dimethyl sulfoxide, N-dimethylformamide, dimethylacetamide, sulfolane and ethylene carbonate, and the inorganic solvent is ZnCl with the concentration of 47-54wt% 2 An aqueous solution or an aqueous NaSCN solution.
Preferably, the weight ratio of the acrylonitrile to the vinyl comonomer is as follows: 100 parts of acrylonitrile and 2.0 to 5.0 parts of vinyl comonomer.
Preferably, the ratio of the total mass of the acrylonitrile and the vinyl comonomer to the mass of the solvent is 1.0 (3.0-5.0). The solvent dosage is controlled to obtain polyacrylonitrile spinning solution with proper concentration for direct spinning, and the unnecessary increase of cost caused by excessive use of solvent can be avoided.
Preferably, the inert gas includes at least one selected from nitrogen, helium, neon, argon, krypton or xenon, and the purity of the inert gas is 99.99%.
Preferably, the vinyl comonomer is one or a mixture of more than one of itaconic acid, methyl itaconate, acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, vinyl acetate, acrylamide, methacrylamide, N-hydroxy acrylamide, styrene, vinyl chloride and vinylidene chloride in any proportion. Other vinyl comonomers that can be copolymerized with acrylonitrile and that facilitate improved performance of the carbon fiber can also be used.
Preferably, the tubular reactor is one or more of a horizontal tubular reactor, a U-shaped tubular reactor, a vertical pipe reactor, a coil pipe reactor and a multi-pipe parallel tubular reactor.
Preferably, a polytetrafluoroethylene coating is attached to the stirring assembly of the tubular reactor and the inner wall of the inner chamber, and the spraying thickness of the coating is 100-300 mu m.
Preferably, the polymerization reaction temperature is 10-40 ℃ and the irradiation time is 8-60s.
Preferably, the polymerization reaction is completed when irradiated to an absorbed dose of 20-130kGy at a dose rate of 2600 Gy/s.
Preferably, the viscosity of the polyacrylonitrile spinning solution is 280-430Pa.s, and the solid content is 18-23wt%.
The beneficial effects of the invention are as follows:
(1) Compared with the cobalt 60 gamma ray irradiation method, the method of the invention has the advantages of no need of adding chemical initiator, extremely short polymerization reaction time, high reaction efficiency and popularization value.
(2) Unlike available water phase suspension polymerization process, the present invention belongs to homogeneous solution polymerization process, and has high stability, easy control, effectively controlled molecular weight and distribution of polyacrylonitrile and high purity of the product.
(3) The tubular reactor used in the invention is provided with a polytetrafluoroethylene coating layer attached to the stirring assembly and the inner wall of the inner chamber, so that the flow resistance of the spinning solution is reduced, the air compressor is used for filter pressing and discharging, the problem of difficult discharging due to high viscosity of the spinning solution is solved, the traditional polymerization reactor for batch polymerization of homogeneous solution is replaced, continuous production can be realized, the cost is greatly reduced, and the method has potential application value.
(4) The existing polyacrylonitrile water phase polymerization is a two-step process, namely, firstly, aqueous slurry is synthesized, then demulsified, dried into powder, crushed and screened into fine powder, and the spinning can be realized after an organic solvent (such as dimethyl sulfoxide) is dissolved when the polyacrylonitrile water phase polymerization is used; the method can use an organic solvent and an inorganic solvent system, and the polyacrylonitrile spinning solution is synthesized, so that spinning can be directly carried out, and the production process is optimized.
Description of the drawings:
FIG. 1 is a flow chart of the process for synthesizing a polyacrylonitrile spinning solution to prepare carbon fiber precursors according to the present invention.
The specific embodiment is as follows:
the invention is further described below with reference to specific embodiments and illustrations in order to make the technical means, the creation features, the achievement of the purpose and the effect of the implementation of the invention easy to understand.
Example 1
(1) 100g of acrylonitrile, 2.5g of methyl acrylate, 1.0g of itaconic acid and 365g of dimethyl sulfoxide are put into a stainless steel mixing kettle, and N is simultaneously introduced 2 Deoxidizing, stirring and mixing for 40min, metering the obtained mixed solution into a tubular reactor, then placing the tubular reactor into an irradiation device, performing polymerization reaction by using X-ray irradiation mixed solution generated by an electron beam conversion target at normal temperature, controlling the radiation dosage rate to be 2600Gy/s, and performing filter pressing and discharging by using an air compressor after radiating for 15s to obtain the polyacrylonitrile spinning solution with the viscosity of 425 Pa.s.
(2) And directly conveying the polyacrylonitrile spinning solution to a spinning production line, directly carrying out dry-jet wet spinning or wet spinning through a spinning metering pump, and forming to obtain the carbon fiber precursor.
Example 2
(1) 100g of acrylonitrile, 2g of methyl acrylate, 1.5g of itaconic acid and 365g of mixed solvent (dimethyl sulfoxide with the mass ratio of 4:1)And N, N-dimethylformamide) are put into a stainless steel mixing kettle and simultaneously N is introduced 2 Deoxidizing, stirring and mixing for 40min, metering the obtained mixed solution into a tubular reactor, then placing the tubular reactor into an irradiation device, performing polymerization reaction by using X-ray irradiation mixed solution generated by an electron beam conversion target at normal temperature, controlling the radiation dosage rate to be 2600Gy/s, and performing filter pressing and discharging by using an air compressor after radiating for 20s to obtain the polyacrylonitrile spinning solution with the viscosity of 392 Pa.s.
(2) And directly conveying the polyacrylonitrile spinning solution to a spinning production line, directly carrying out dry-jet wet spinning or wet spinning through a spinning metering pump, and forming to obtain the carbon fiber precursor.
Example 3
(1) 100g of acrylonitrile, 2.5g of methyl acrylate, 1.5g of itaconic acid and 370g of NaSCN aqueous solution with the concentration of 49.0 weight percent are put into a stainless steel mixing kettle, and N is simultaneously introduced 2 Deoxidizing, stirring and mixing for 40min, metering the obtained mixed solution into a tubular reactor, then placing the tubular reactor into an irradiation device, performing polymerization reaction by using X-ray irradiation mixed solution generated by an electron beam conversion target at normal temperature, controlling the radiation dosage rate to be 2600Gy/s, and performing filter pressing and discharging by using an air compressor after radiating for 30s to obtain the polyacrylonitrile spinning solution with the viscosity of 353 Pa.s.
(2) And directly conveying the polyacrylonitrile spinning solution to a spinning production line, directly carrying out dry-jet wet spinning or wet spinning through a spinning metering pump, and forming to obtain the carbon fiber precursor.
Example 4
(1) 100g of acrylonitrile, 2g of methyl acrylate, 1.5g of itaconic acid and 410g of ZnCl with a concentration of 51.0 wt.% 2 The aqueous solution is put into a stainless steel mixing kettle and simultaneously N is introduced 2 Deoxidizing, stirring and mixing for 40min, metering the obtained mixed solution into a tubular reactor, then placing the tubular reactor into an irradiation device, performing polymerization reaction by using X-ray irradiation mixed solution generated by an electron beam conversion target at normal temperature, controlling the radiation dosage rate to be 2600Gy/s, and performing filter pressing and discharging by using an air compressor after radiating for 8s to obtain the polyacrylonitrile spinning solution with the viscosity of 330 Pa.s.
(2) And directly conveying the polyacrylonitrile spinning solution to a spinning production line, directly carrying out dry-jet wet spinning or wet spinning through a spinning metering pump, and forming to obtain the carbon fiber precursor.
Comparative example 1 (solvent polymerization method Using chemical initiator)
(1) At N 2 Under the protection, 100g of acrylonitrile, 2g of methyl acrylate, 1.5g of itaconic acid and 365g of NaSCN aqueous solution with the concentration of 49.0wt% are sequentially added into a stainless steel polymerization kettle to be stirred, an initiator azodiisobutyronitrile (accounting for 0.6 percent of the total monomer mass) is added dropwise to react for 3.5 hours at the temperature of 78 ℃, and a polyacrylonitrile spinning solution with the viscosity of 236 Pa.s is obtained after discharging.
(2) And filtering the polyacrylonitrile spinning solution, conveying the filtered polyacrylonitrile spinning solution to a spinning metering pump, carrying out wet spinning or dry-jet wet spinning, and forming to obtain the carbon fiber precursor.
Comparative example 2 (polymerization Using Mixed solvent of chemical initiator)
(1) At N 2 Under the protection, 100g of acrylonitrile, 2g of methyl acrylate, 1.5g of itaconic acid and 365g of mixed solvent (dimethyl sulfoxide and N, N-dimethylformamide with the mass ratio of 4:1) are sequentially added into a stainless steel polymerization kettle to be stirred, an initiator azodiisobutyronitrile (accounting for 0.6 percent of the total monomer mass) is dropwise added to react for 4.0 hours at 80 ℃, and a polyacrylonitrile spinning solution with the viscosity of 256 Pa.s is obtained after discharging.
(2) And filtering the obtained polyacrylonitrile spinning solution, conveying to a spinning metering pump, carrying out wet spinning or dry-jet wet spinning, and forming to obtain the carbon fiber precursor.
The polyacrylonitrile solutions prepared in examples 1 to 4 and comparative examples 1 to 2 were subjected to gel permeation chromatography to determine the weight average molecular weight, number average molecular weight and molecular weight distribution of the polymerization products.
TABLE 2 data for the performance measurements of the Polyacrylonitrile copolymers prepared in examples 1-4 and comparative examples 1-2
As can be seen from Table 2, the molecular weight of polyacrylonitrile prepared by the electron beam irradiation polymerization method of the present invention is larger and the molecular weight distribution is narrower.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A continuous production method for preparing polyacrylonitrile spinning solution by X-ray irradiation is characterized in that: firstly, putting acrylonitrile, vinyl comonomer and solvent into a mixing kettle, simultaneously introducing inert gas to deoxidize, stirring and mixing, metering the obtained mixed solution into a tubular reactor, putting the tubular reactor into an electron beam irradiation device, and performing polymerization reaction by using X-ray irradiation mixed solution generated by an electron beam conversion target to obtain a polyacrylonitrile spinning solution;
the solvent is organic solvent or inorganic solvent, the organic solvent is one or more of dimethyl sulfoxide, N-dimethylformamide, dimethylacetamide, sulfolane and ethylene carbonate, and the inorganic solvent is ZnCl with the concentration of 47-54wt% 2 An aqueous solution or an aqueous NaSCN solution;
the polyacrylonitrile spinning solution is directly conveyed to a spinning production line, dry-jet wet spinning or wet spinning is carried out through a spinning metering pump, and carbon fiber precursor is obtained through molding;
the vinyl comonomer is one or a mixture of more than one of itaconic acid, methyl itaconate, acrylic acid, methacrylic acid, methyl acrylate, ethyl acrylate, vinyl acetate, acrylamide, methacrylamide, N-hydroxy acrylamide, styrene, vinyl chloride and vinylidene chloride in any proportion.
2. The continuous production method according to claim 1, characterized in that: the weight ratio of the acrylonitrile to the vinyl comonomer is as follows: 100 parts of acrylonitrile and 2.0 to 5.0 parts of vinyl comonomer;
the ratio of the total mass of the acrylonitrile and the vinyl comonomer to the mass of the solvent is 1.0 (3.0-5.0).
3. The continuous production method according to claim 1, characterized in that: the inert gas includes at least one selected from nitrogen, helium, neon, argon, krypton, or xenon.
4. The continuous production method according to claim 1, characterized in that: the tubular reactor is one or more of a horizontal tubular reactor, a U-shaped tubular reactor, a vertical pipe reactor, a coil pipe reactor and a multi-pipe parallel tubular reactor.
5. The continuous production method according to claim 1, characterized in that: a polytetrafluoroethylene coating is adhered to the stirring assembly of the tubular reactor and the inner wall of the inner chamber, and the spraying thickness of the coating is 100-300 mu m.
6. The continuous production method according to claim 1, characterized in that: the temperature of the polymerization reaction is 10-40 ℃, and the irradiation time is 8-60s;
the polymerization reaction is completed when the irradiation is carried out at a dose rate of 2600Gy/s to an absorbed dose of 20-130 kGy.
7. The continuous production method according to claim 1, characterized in that: the viscosity of the polyacrylonitrile spinning solution is 280-430Pa.s, and the solid content is 18-23wt%.
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| JP2004149980A (en) * | 2002-10-31 | 2004-05-27 | Toho Tenax Co Ltd | Carbon fiber strand and method for producing the same |
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| US5364581A (en) * | 1993-05-06 | 1994-11-15 | Kenneth Wilkinson | Process of making polyacrylonitrile fibers |
| CN101693769A (en) * | 2009-08-10 | 2010-04-14 | 刘剑洪 | Method for preparing polyacrylonitrile, acrylonitrile copolymer and mixture material thereof |
| CN102517671B (en) * | 2011-12-09 | 2013-11-13 | 东华大学 | Method for preparing carbon fiber precursor by two-step process of aqueous suspension and solution polymerization |
| CN104558394A (en) * | 2013-10-28 | 2015-04-29 | 中国石油化工股份有限公司 | Method for preparing viscosity-controllable polyacrylonitrile carbon fiber spinning solution |
| CN103614801A (en) * | 2013-12-03 | 2014-03-05 | 国家电网公司 | Method for preparing high-crystallinity polyacrylonitrile nascent fiber |
| US20220162779A1 (en) * | 2020-11-25 | 2022-05-26 | Circufiber Inc. | Low friction infrared-emitting fiber and methods of making the same |
| CN112813539B (en) * | 2021-02-05 | 2023-07-18 | 天津工业大学 | Preparation method of polyacrylonitrile-based carbon fiber |
| CN114621391B (en) * | 2022-04-01 | 2023-06-20 | 安徽大学 | Electron beam target-rotating X-ray radiation polymerization method of polyacrylonitrile for carbon fiber precursor |
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