CN116024701A - Polyacrylonitrile-based large-tow carbon fiber and preparation method thereof - Google Patents
Polyacrylonitrile-based large-tow carbon fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of polyacrylonitrile-based large-tow carbon fibers, which solves the problems of concentrated heat release, easy fiber breakage, aggregation of carbon fiber products, poor spreading effect and difficult application in the preoxidation process in the prior art. The method comprises the following specific steps: performing four-temperature-zone pre-oxidation treatment on the polyacrylonitrile fiber by using a pre-oxidation furnace, and controlling the tow width of the pre-oxidized fiber through drafting matching to prepare the pre-oxidized fiber; and (3) performing low-temperature carbonization treatment in a three-temperature area by using a low-temperature carbonization furnace, and performing high-temperature carbonization treatment in the three-temperature area by using a high-temperature carbonization furnace to obtain the polyacrylonitrile-based large-tow carbon fiber. In the continuous preparation process of the fiber, the continuous preparation of the large-tow carbon fiber is realized by matching the temperature, the draft ratio and the residence time of pre-oxidation, low-temperature carbonization and high-temperature carbonization and controlling the running width of the fiber, so that the problems are well solved, and the method can be used in the industrial production of the polyacrylonitrile-based large-tow carbon fiber preparation process.
Description
Technical Field
The invention belongs to the field of carbon fibers, and particularly relates to a polyacrylonitrile-based large-tow carbon fiber and a preparation method thereof.
Background
The carbon fiber is an inorganic polymer fiber containing 92% or more of carbon and composed of a polymeric precursor or an allotropic unit of carbon, and belongs to a typical high-performance fiber. The high-specific-strength high-specific-modulus high-temperature-resistant corrosion-resistant creep-resistant conductive material has the advantages of high specific strength, high specific modulus, high temperature resistance, corrosion resistance, low specific gravity and the like, and is widely applied to the fields of automobiles, aircrafts, rail transit, wind power generation, sports equipment and the like. Carbon fibers are classified into polyacrylonitrile-based, pitch-based and viscose-based carbon fibers by filaments, with most of them being commercially available as polyacrylonitrile-based carbon fibers.
The carbon fibers have a size tow fraction, wherein the size tow carbon fibers are larger than or equal to 48K. The small-tow carbon fiber is mainly applied to the field of national defense and military industry, and the industrial field is more in need of the large-tow carbon fiber due to the advantage of low cost. However, in the production and application process of large tows, there are also a lot of technical problems to be solved, mainly in: the reaction heat is concentrated when the large tow precursor is preoxidized, the heat is not easy to be dissipated, and melting and filament doubling, fracture and even spontaneous combustion are easy to occur; the poor resin wettability caused by poor aggregation and spreading effects of large-tow carbon fibers, uneven distribution of the carbon fibers and the resin, and easy defect generation can influence the strength and rigidity of the carbon fibers and the composite material, so that the product performance is unstable. Thus, it is necessary to slow down the concentrated heat release during the preoxidation of large tow strands and control the width of the tow. At present, a comonomer mode is adopted to reduce the initial temperature of pre-oxidation of the precursor, or the pre-oxidation atmosphere (CN 111647973A) is adjusted to achieve the aim of control; the large-tow carbon fiber is subjected to widening and flattening treatment (CN 107904738A) so as to avoid the generation of product defects.
The existing technical proposal can improve the pre-oxidation speed, reduce the heat release amount or optimize the pre-oxidation structure, but only stays in the research of small tow fiber precursors or is difficult to apply in large scale; further expanding treatment is carried out on the large-tow carbon fibers, so that the cost is increased and the performance is damaged.
Disclosure of Invention
In order to solve the problems of concentrated heat release, easy fiber breakage, poor aggregation and expansion effects of carbon fiber products and difficult application in the preoxidation process in the prior art, the invention provides a preparation method of polyacrylonitrile preoxidized fibers, which has the characteristics of mild heat release, difficult fiber breakage and excellent performance of final products in the preoxidation process.
The invention aims to provide a preparation method of polyacrylonitrile-based large-tow carbon fiber, which comprises the steps of pre-oxidizing, carbonizing at low temperature and carbonizing at high temperature a polyacrylonitrile fiber precursor to obtain the polyacrylonitrile-based large-tow carbon fiber, wherein the width of the tow in the pre-oxidizing process is 0.0003-0.0007 times, preferably 0.0004-0.0006 times, of the number of the polyacrylonitrile fiber precursor in terms of millimeter.
In the above-mentioned preparation method, the catalyst,
the number of the polyacrylonitrile fiber precursor is 48000-600000, preferably 48000-360000;
the water content of the polyacrylonitrile fiber precursor is 7wt% or less, preferably 5wt% or less;
the fineness of the polyacrylonitrile fiber precursor is 0.2 to 3.0dtex, preferably 0.5 to 2.5dtex.
In the preparation method, the pre-oxidation treatment is provided with four temperature areas:
the temperature of the four temperature areas of the pre-oxidation is 160-220 ℃, 180-240 ℃, 200-260 ℃ and 210-280 ℃ respectively, and the temperature of the four temperature areas is gradually increased, preferably, the temperature of the four temperature areas is 180-200 ℃, 200-220 ℃, 220-240 ℃ and 230-260 ℃ respectively;
the pre-oxidation residence time of each pre-oxidation temperature zone is 10-30 min, preferably 15-25 min;
the draft ratio of the four temperature areas of pre-oxidation is respectively 0.5-3.5%, -2.5 to-0.5%, preferably, the draft ratio of the four temperature areas is respectively 1-3%, -2 to-1%, and-2 to-1%.
In the preparation method, the low-temperature carbonization is provided with three temperature areas:
the temperature of the three low-temperature carbonization regions is 300-600 ℃, 400-700 ℃, 600-900 ℃ and the temperature of the three temperature regions is gradually increased, preferably, the temperature of the three temperature regions is 350-550 ℃, 450-650 ℃ and 650-850 ℃ respectively;
the residence time of each temperature zone of the low-temperature carbonization is 1-20 min, preferably 2-10 min;
the draft ratio of each temperature zone of the low-temperature carbonization is 0.5-10%, preferably 2-7%.
In the preparation method, three temperature areas are arranged in the high-temperature carbonization way:
the temperature of the three high-temperature carbonization temperature areas is 900-1300 ℃, 1100-1400 ℃, 1200-1600 ℃ and the temperature of the three temperature areas is gradually increased, preferably, the temperature of the three temperature areas is 1000-1250 ℃, 1200-1350 ℃ and 1300-1500 ℃ respectively;
the residence time of each temperature zone of the high-temperature carbonization is 1-20 min, preferably 2-10 min;
the draft ratio of each temperature zone of the high-temperature carbonization is-5.0 to-0.5 percent, preferably-3.5 to-1.5 percent.
The second purpose of the invention is to provide a polyacrylonitrile-based large-tow carbon fiber which is prepared by the preparation method.
The tensile strength of the polyacrylonitrile-based large-tow carbon fiber obtained by the preparation method is more than or equal to 3.5GPa, and the tensile modulus is more than or equal to 230GPa.
The invention relates to a method for preparing polyacrylonitrile fiber precursor, which comprises the steps of controlling the relation between the width of a fiber and the number of fibers N in a preoxidation process to ensure that the width of the fiber meets the width W (mm) = (0.0003-0.0007) ×N, preferably W (mm) = (0.0004-0.0006) ×N, and matching the temperature, draft ratio and residence time of the preoxidation, and controlling the fiber to be in a proper width range to ensure that the fiber of a large fiber bundle has good heat dissipation when the fiber undergoes severe oxidation reaction, and single fibers are not easy to adhere, so that the problems of smoke generation, breakage and the like of the fiber bundle caused by overhigh local temperature are avoided. And meanwhile, the temperature, the draft ratio and the residence time of low-temperature carbonization and high-temperature carbonization are matched, so that the continuous preparation of the large-tow carbon fiber is realized.
By adopting the technical scheme, the pre-oxidation furnace is used for carrying out the pre-oxidation treatment of the polyacrylonitrile fiber in a four-temperature zone, and the width of the tow of the pre-oxidized fiber is controlled through drafting matching to prepare the pre-oxidized fiber; the low-temperature carbonization treatment in the three-temperature area is performed by using a low-temperature carbonization furnace, and then the high-temperature carbonization treatment in the three-temperature area is performed by using a high-temperature carbonization furnace, so that the polyacrylonitrile-based large-tow carbon fiber is obtained, the tensile strength of the large-tow carbon fiber is more than 3.5GPa, and the tensile modulus is more than 230GPa, and a better technical effect is achieved.
The invention realizes continuous preparation of large-tow carbon fibers by matching the temperature, the draft ratio and the residence time of pre-oxidation, low-temperature carbonization and high-temperature carbonization and controlling the running width of the fibers, and can be used in industrial production in the preparation process of polyacrylonitrile-based large-tow carbon fibers.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The test instruments and test conditions used in the examples are as follows:
the tensile strength and tensile modulus of the carbon fibers were tested according to GB/T3362-2017.
[ example 1 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 190 ℃, 210 ℃, 230 ℃ and 245 ℃, the drafting multiplying power is 2%, 1.5% and 1.5%, the residence time of each temperature-zone is 15min, and the fiber running width is 24mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 750 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1100 ℃, 1250 ℃ and 1400 ℃, the fiber draft ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The tensile strength of the obtained carbon fiber was 3.9GPa, and the tensile modulus was 251GPa.
[ example 2 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 190 ℃, 210 ℃, 230 ℃ and 245 ℃, the drafting multiplying power is 2.5%, 1.0% and 1.0%, the residence time of each temperature zone is 15min, and the filament running width of the fiber is 20mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 750 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1100 ℃, 1250 ℃ and 1400 ℃, the fiber draft ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The resulting carbon fiber had a tensile strength of 3.8GPa and a tensile modulus of 243GPa.
[ example 3 ]
Pre-oxidizing 120K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 190 ℃, 210 ℃, 230 ℃ and 245 ℃, the drafting multiplying power is 2%, 1.5% and 1.5%, the residence time of each temperature-zone is 15min, and the fiber running width is 60mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 750 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1100 ℃, 1250 ℃ and 1400 ℃, the fiber draft ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The resulting carbon fiber had a tensile strength of 3.6GPa and a tensile modulus of 233GPa.
[ example 4 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 180 ℃, 200 ℃, 240 ℃ and 260 ℃, the drafting multiplying power is 2%, 1.5%, 2% and 2%, the residence time of each temperature-zone is 15min, and the fiber running width is 24mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 750 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1100 ℃, 1250 ℃ and 1400 ℃, the fiber draft ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The resulting carbon fiber had a tensile strength of 3.7GPa and a tensile modulus of 244GPa.
[ example 5 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 190 ℃, 210 ℃, 230 ℃ and 245 ℃, the drafting multiplying power is 2%, 1.5% and 1.5%, the residence time of each temperature-zone is 15min, and the fiber running width is 24mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 800 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1200 ℃, 1350 ℃ and 1450 ℃, the fiber drafting ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The resulting carbon fiber had a tensile strength of 3.6GPa and a tensile modulus of 258GPa.
[ comparative example 1 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 190 ℃, 210 ℃, 230 ℃ and 245 ℃, the drafting multiplying power is 4%, 1.5% and 1.5%, the residence time of each temperature-zone is 15min, and the fiber running width is 9mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 750 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1100 ℃, 1250 ℃ and 1400 ℃, the fiber draft ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The resulting carbon fiber had a tensile strength of 2.3GPa and a tensile modulus of 217GPa.
[ comparative example 2 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 190 ℃, 210 ℃, 230 ℃ and 245 ℃, the drafting multiplying power is 3%, 0.5% and 3%, the residence time of each temperature-zone is 15min, and the fiber running width is 35mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 450 ℃, 550 ℃ and 750 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1100 ℃, 1250 ℃ and 1400 ℃, the fiber draft ratio is-3.0%, and the fiber residence time is 3min, so as to prepare the large-tow carbon fiber. The resulting carbon fiber had a tensile strength of 2.1GPa and a tensile modulus of 223GPa.
[ comparative example 3 ]
Pre-oxidizing 48K polyacrylonitrile fiber (fineness of 1.5dtex, water content of 2%) in an air atmosphere in a four-temperature-zone pre-oxidizing furnace, wherein the pre-oxidizing temperature of the four-temperature-zone pre-oxidizing furnace is 160 ℃, 170 ℃, 190 ℃ and 230 ℃, the drafting multiplying power is 4%, 2%, 1.5% and 1.5%, the residence time of each temperature-zone is 15min, and the fiber running width is 24mm;
carrying out low-temperature carbonization treatment on the pre-oxidized fiber in three temperature areas by using a low-temperature carbonization furnace under the nitrogen atmosphere, wherein the low-temperature carbonization treatment temperature of each temperature area is 400 ℃, 500 ℃ and 700 ℃, the fiber drawing multiplying power is 4.5%, and the fiber residence time is 3min;
and (3) carrying out high-temperature carbonization treatment of the low-carbon fiber in three temperature areas by using a high-temperature carbonization furnace under the nitrogen atmosphere, wherein the high-temperature carbonization treatment temperature of each temperature area is 1000 ℃, 1150 ℃ and 1300 ℃, the fiber drafting multiplying power is-3.0%, and the fiber residence time is 3min, so that the large-tow carbon fiber is prepared. The resulting carbon fiber had a tensile strength of 2.3GPa and a tensile modulus of 210GPa.
Obviously, by adopting the technical scheme of the invention, the concentrated heat release in the pre-oxidation process can be slowed down, the problem of melting yarn breakage caused by concentrated heat release is avoided, the final product has a good expanding effect, is convenient for subsequent application, has a great technical advantage, and can be used in the industrial production of the polyacrylonitrile-based large-tow carbon fiber preparation process.
Claims (11)
1. The preparation method of the polyacrylonitrile-based large-tow carbon fiber comprises the steps of pre-oxidizing polyacrylonitrile fiber precursors, carbonizing at low temperature and carbonizing at high temperature to obtain the polyacrylonitrile large-tow carbon fiber, wherein the width of the tows in the pre-oxidizing process is 0.0003-0.0007 times of the number of the polyacrylonitrile fiber precursors in millimeter.
2. The preparation method according to claim 1, wherein,
the width of the filament bundle in the pre-oxidation treatment process is 0.0004 to 0.0006 times of the number of the polyacrylonitrile fiber precursor in millimeter.
3. The method according to claim 1, wherein,
the number of the polyacrylonitrile fiber precursor is 48000-600000, preferably 48000-360000; and/or the number of the groups of groups,
the water content of the polyacrylonitrile fiber precursor is 7wt% or less, preferably 5wt% or less; and/or the number of the groups of groups,
the fineness of the polyacrylonitrile fiber precursor is 0.2 to 3.0dtex, preferably 0.5 to 2.5dtex.
4. The method according to claim 1, wherein,
the pre-oxidation treatment is provided with four temperature areas.
5. The method according to claim 4, wherein,
the temperature of the four temperature areas of the pre-oxidation is 160-220 ℃, 180-240 ℃, 200-260 ℃ and 210-280 ℃ respectively, and the temperature of the four temperature areas is gradually increased; preferably, the temperatures of the four temperature areas are 180-200 ℃, 200-220 ℃, 220-240 ℃ and 230-260 ℃ respectively; and/or the number of the groups of groups,
the pre-oxidation residence time of each pre-oxidation temperature zone is 10-30 min, preferably 15-25 min; and/or the number of the groups of groups,
the draft ratio of the four temperature areas of pre-oxidation is respectively 0.5-3.5%, -2.5 to-0.5%, preferably, the draft ratio of the four temperature areas is respectively 1-3%, -2 to-1%, and-2 to-1%.
6. The method according to claim 1, wherein,
the low-temperature carbonization is provided with three temperature areas.
7. The method according to claim 6, wherein,
the temperature of the three low-temperature carbonization regions is 300-600 ℃, 400-700 ℃ and 600-900 ℃ respectively, and the temperatures of the three temperature regions are gradually increased; preferably, the temperatures of the three temperature areas are respectively 350-550 ℃, 450-650 ℃ and 650-850 ℃; and/or the number of the groups of groups,
the residence time of each temperature zone of the low-temperature carbonization is 1-20 min, preferably 2-10 min; and/or the number of the groups of groups,
the draft ratio of each temperature zone of the low-temperature carbonization is 0.5-10%, preferably 2-7%.
8. The method according to claim 1, wherein,
and the high-temperature carbonization is provided with three temperature areas.
9. The method according to claim 8, wherein,
the temperature of the three high-temperature carbonization temperature areas is 900-1300 ℃, 1100-1400 ℃, 1200-1600 ℃ respectively, and the temperature of the three temperature areas is gradually increased; preferably, the temperatures of the three temperature areas are 1000-1250 ℃, 1200-1350 ℃ and 1300-1500 ℃ respectively; and/or the number of the groups of groups,
the residence time of each temperature zone of the high-temperature carbonization is 1-20 min, preferably 2-10 min; and/or the number of the groups of groups,
the draft ratio of each temperature zone of the high-temperature carbonization is-5.0 to-0.5 percent, preferably-3.5 to-1.5 percent.
10. A polyacrylonitrile-based large tow carbon fiber prepared by the preparation method of any one of claims 1 to 9.
11. The polyacrylonitrile-based big-tow carbon fiber according to claim 10, wherein the carbon fiber has a tensile strength of 3.5GPa or more and a tensile modulus of 230GPa or more.
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