CN109610049B - Method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization - Google Patents
Method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization Download PDFInfo
- Publication number
- CN109610049B CN109610049B CN201811548944.7A CN201811548944A CN109610049B CN 109610049 B CN109610049 B CN 109610049B CN 201811548944 A CN201811548944 A CN 201811548944A CN 109610049 B CN109610049 B CN 109610049B
- Authority
- CN
- China
- Prior art keywords
- mesophase pitch
- asphalt
- thermal polymerization
- temperature
- based carbon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/155—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from petroleum pitch
-
- 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
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Fibers (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention relates to a method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization, which comprises the following steps: 1) adding an active component containing branched-chain aromatic hydrocarbon into the high-aromaticity condensed ring asphalt to uniformly mix asphalt raw materials in a hot state; 2) self-boosting the uniformly mixed asphalt raw material in a closed container to carry out co-heating polymerization reaction; 3) and carrying out melt spinning, oxidation non-melting and high-temperature carbonization treatment on the mesophase pitch obtained by the co-thermal polymerization reaction to obtain the mesophase pitch-based carbon fiber. The aim of reducing the splitting degree of the mesophase pitch-based carbon fibers is fulfilled by regulating and controlling the composition and the structure of the mesophase pitch raw materials, so that the structure and the performance of the carbon fibers are improved.
Description
Technical Field
The invention belongs to the technical field of mesophase pitch-based carbon fibers, and particularly relates to a method for regulating and controlling the composition and structure of mesophase pitch through a co-thermal polymerization reaction.
Background
The mesophase pitch is a condensed ring aromatic hydrocarbon aggregate with regular and ordered molecular arrangement, has the advantages of high carbon yield, melt-regulated orientation, easy graphitization and the like, and is a high-quality precursor raw material for preparing high-performance and multifunctional carbon materials. A spinnable mesophase pitch feedstock for use as high performance mesophase pitch-based carbon fibers, the essential requirements of which are: the content of hetero atoms and ash is low, the molecular size is moderate, the molecular weight distribution is narrow, the molecular structure composition is uniform, the aromaticity is high, the condensation degree is low, the intermediate phase asphalt melt is rich in alkyl short chains and naphthenic groups and the like, and particularly has proper viscosity, fluidity and thermal stability in the melt spinning process. Usually, mesophase pitch (such as coal pitch-based mesophase pitch) prepared by thermal polymerization at 400-450 ℃ for a long time (5-10H) has a regular condensed ring molecular composition and an ideal preferred orientation texture (namely high-content optical anisotropy), but the pitch with high mesophase content usually has the defects of higher condensation degree, fewer alkyl side chains or branched chains, lower H/C ratio and the like, so that the problems of higher melt spinning temperature, difficult oxidation and stabilization of the spun pitch fiber and the like are caused, and the pitch with high mesophase content is easy to form mesophase pitch-based carbon fiber with a radial cross-section structure.
The section structure of the intermediate phase pitch-based carbon fiber prepared by taking the intermediate phase pitch as a raw material at present presents various textures (disordered structure, radial structure, folded radial structure, concentric circle structure and the like). The fiber with the radial and radial structure has higher molecular orientation degree, perfect crystal growth and development after graphitization treatment and larger crystallite dimension, thereby having excellent axial electric conduction and heat conduction performance, but the wedge-shaped splitting is caused by the stress concentration generated at the circle center because the growth and the orientation direction of the graphite crystallite are inconsistent in the high-temperature heat treatment process, and the fiber structure damage and the performance reduction can not be avoided due to the splitting. The existing research at home and abroad changes the section texture of the mesophase pitch-based carbon fiber by blending the mesophase pitch raw material composition or carrying out macromolecule doping modification on the mesophase pitch raw material (such as blending with a certain amount of isotropic pitch or polyacrylonitrile or polyimide or doping with a second-phase carbon filler, such as a carbon nano-tube, carbon black, graphene and the like), reduces the splitting degree of the mesophase pitch-based carbon fiber or avoids forming a radial structure, thereby regulating or improving the performance of the mesophase pitch-based carbon fiber.
Therefore, it is a research focus in the art how to adjust the structure and properties of the mesophase pitch raw material in order to control the degree of splitting of the mesophase pitch-based carbon fibers. The high-aromaticity condensed ring asphalt modified by the active component containing branched-chain aromatic hydrocarbon is adopted, and the composition and the structure of a mesophase asphalt raw material are regulated and controlled through a co-thermal polymerization reaction, so that the purpose of improving or enhancing the structure and the performance of the mesophase asphalt-based carbon fiber is achieved.
Disclosure of Invention
Aiming at the problems, the invention adopts the active component containing the branched-chain aromatic hydrocarbon to modify the condensed ring asphalt, the formation and the conversion of the asphalt mesophase liquid crystal are accelerated by the co-thermal polymerization reaction, and the composition and the structure of the mesophase asphalt are regulated and controlled. Meanwhile, the aim of reducing the splitting degree of the mesophase pitch-based carbon fibers is fulfilled by regulating and controlling the composition and the structure of the mesophase pitch raw materials, so that the structure and the performance of the mesophase pitch-based carbon fibers are improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for regulating and controlling the composition and structure of mesophase pitch by a co-thermal polymerization reaction comprises the following steps:
1) adding an active component containing branched-chain aromatic hydrocarbon into the high-aromaticity condensed ring asphalt to uniformly mix asphalt raw materials in a hot state;
2) self-boosting the uniformly mixed asphalt raw material in a closed container to carry out co-heating polymerization reaction;
3) and carrying out melt spinning, oxidation non-melting and high-temperature carbonization treatment on the mesophase pitch obtained by the co-thermal polymerization reaction to obtain the mesophase pitch-based carbon fiber.
The pressure of the asphalt raw material is automatically increased in the closed container to form volatile components, the volatile components are changed into gas in the closed container, so that the pressure in the closed container is automatically increased, and the pressure is uncertain due to different raw material components.
Wherein the high-aromaticity condensed ring asphalt is any one of naphthalene asphalt, anthracene asphalt and coal asphalt.
The branched-chain aromatic hydrocarbon-containing active component is a cyclohexane soluble component in petroleum asphalt or heavy oil, and the adding amount of the branched-chain aromatic hydrocarbon-containing active component is 4-15 wt% of high-aromaticity fused ring asphalt. Wherein the cyclohexane-soluble component in the petroleum asphalt or the heavy oil means a component from which cyclohexane has been removed, which is a product well known to those skilled in the art.
Wherein the thermal state mixing process conditions are as follows: in nitrogen atmosphere, the softening temperature of the high-aromaticity condensed ring asphalt is 80 ℃ higher, and the mixture is stirred for 2 hours at the speed of 500 r/min.
Wherein the co-thermal polymerization reaction conditions are as follows: stirring at the temperature of 386-432 ℃ at the speed of 550-1180 r/min for 3-6 h.
Wherein the melt spinning, oxidation non-melting and high-temperature carbonization treatment conditions are respectively as follows: melt spinning at 60 ℃ higher than the softening temperature of the mesophase pitch, oxidation non-melting at 20 ℃ lower than the softening temperature of the mesophase pitch, and carbonization at 1000 ℃ in nitrogen atmosphere. The melt spinning, oxidative infusions and high temperature charring are all carried out by means well known to those skilled in the art.
In addition, the invention also provides the mesophase pitch-based carbon fiber obtained by using the method for regulating and controlling the composition and the structure of the mesophase pitch through the co-thermal polymerization reaction.
Compared with the prior art, the invention has the advantages that:
(1) the high-aromaticity condensed ring asphalt modified by the active component containing the branched-chain aromatic hydrocarbon is adopted, the formation and conversion of the asphalt mesophase liquid crystal are accelerated through the co-thermal polymerization reaction, the formation time of the whole liquid crystal mesophase asphalt is shortened, and the preparation time of the whole mesophase asphalt is shortened by 0.5-2.5 h compared with the condensed ring asphalt raw material without the active component;
(2) the introduction of the active component containing branched chain aromatic hydrocarbon changes the composition and structure of plane macromolecules of the condensed ring asphalt, compared with the original mesophase asphalt without the active component, the branched chain aromatic hydrocarbon component is doped into the condensed ring asphalt molecules, the H/C molar ratio is increased by 0.05-0.2, the softening point of the mesophase asphalt can be reduced by 8-25 ℃, the viscosity and the fluidity of mesophase asphalt melt are adjusted, and the stable spinning fiber forming is facilitated;
(3) the branched aromatic hydrocarbon-containing active component is introduced into the mesophase pitch raw material, so that the oxidation stabilization of mesophase pitch fibers can be accelerated, the non-melting time can be shortened by 1-3 h at the same oxidation temperature, and the production cost of the mesophase pitch-based carbon fibers is reduced;
(4) the aim of reducing the splitting degree of the mesophase pitch-based carbon fiber can be fulfilled by regulating and controlling the composition and the structure of the mesophase pitch raw material, the splitting degree (splitting rate and splitting angle) of the carbon fiber is reduced by 50-95% compared with the mesophase pitch-based carbon fiber prepared from the original mesophase pitch without adding the active component, and the structure and the performance of the mesophase pitch-based carbon fiber are obviously improved or enhanced, so that the wide application of the mesophase pitch-based carbon fiber in a composite material is accelerated.
(5) The mesophase pitch obtained by the co-thermal polymerization reaction is used as a raw material, and the mesophase pitch-based carbon fiber is prepared by melt spinning, oxidation infusibility and high-temperature carbonization treatment, so that the oxidation infusibility time of the mesophase pitch fiber can be shortened, and the splitting degree of the mesophase pitch-based carbon fiber can be reduced.
Detailed Description
The principles and features of the present invention are described below in conjunction with specific examples, which are provided only for illustrating the advantages of the present invention in controlling the composition and structure of mesophase pitch using the co-thermal polymerization, and are not intended to limit the scope of the present invention.
Example 1
A method for regulating and controlling the composition and structure of mesophase pitch by a co-thermal polymerization reaction. The specific process is as follows:
(1) adding 12 wt.% of cyclohexane soluble component in petroleum asphalt into high-aromaticity condensed ring naphthalene asphalt, and stirring for 2 hours at the speed of 500r/min in a nitrogen atmosphere at the temperature which is 80 ℃ higher than the softening temperature of the naphthalene asphalt so as to uniformly mix asphalt raw materials in a hot state;
(2) carrying out co-thermal polymerization reaction on the uniformly mixed asphalt raw materials in a self-boosting closed container, wherein the co-thermal polymerization reaction conditions are as follows: stirring at the temperature of 422 ℃ for 5 hours at the speed of 750 r/min;
(3) the mesophase pitch obtained by the co-thermal polymerization is used as a raw material, and the mesophase pitch-based carbon fiber is prepared by adopting melt spinning at 60 ℃ higher than the softening temperature of the mesophase pitch, oxidation non-melting at 20 ℃ lower than the softening temperature of the mesophase pitch and carbonization at 1000 ℃ in nitrogen atmosphere.
Compared with the naphthalene asphalt raw material without the active component, the preparation time of the integral mesophase asphalt of the embodiment is shortened by 1.5 h; compared with the original mesophase pitch without the active component, the H/C molar ratio of the mesophase pitch prepared by the embodiment is increased by 0.15, the softening point is reduced by 20 ℃, and the non-melting time of the spun mesophase pitch fiber can be shortened by 3 hours; compared with the mesophase pitch-based carbon fiber prepared from the original mesophase pitch without the active component, the degree of splitting of the mesophase pitch-based carbon fiber prepared by the embodiment is reduced by 95%, and the structure and the performance of the mesophase pitch-based carbon fiber are obviously improved or enhanced.
Example 2
A method for regulating and controlling the composition and structure of mesophase pitch by a co-thermal polymerization reaction. The specific process is as follows:
(1) adding 8 wt.% of cyclohexane soluble component in petroleum asphalt into the high-aromaticity condensed ring anthracene asphalt, in a nitrogen atmosphere, the softening temperature of the cyclohexane soluble component is 80 ℃ higher than that of the anthracene asphalt, and stirring the mixture for 2 hours at the speed of 500r/min to ensure that the asphalt raw materials are uniformly mixed in a hot state;
(2) the asphalt raw materials which are uniformly mixed are subjected to self-boosting in a closed container to carry out the co-thermal polymerization reaction, wherein the co-thermal polymerization reaction conditions are as follows: stirring at the temperature of 410 ℃ for 4 hours at the speed of 1100 r/min;
(3) the mesophase pitch obtained by the co-thermal polymerization is used as a raw material, and the mesophase pitch-based carbon fiber is prepared by adopting melt spinning at 60 ℃ higher than the softening temperature of the mesophase pitch, oxidation non-melting at 20 ℃ lower than the softening temperature of the mesophase pitch and carbonization at 1000 ℃ in nitrogen atmosphere.
Compared with anthracene asphalt raw material without active component, the preparation time of the integral mesophase asphalt of the embodiment is shortened by 2 h; compared with the original mesophase pitch without the active component, the H/C molar ratio of the mesophase pitch prepared by the embodiment is increased by 0.1, the softening point is reduced by 15 ℃, and the non-melting time of the spun mesophase pitch fiber can be shortened by 2 hours; compared with the mesophase pitch-based carbon fiber prepared from the original mesophase pitch without the active component, the degree of splitting of the mesophase pitch-based carbon fiber prepared by the embodiment is reduced by 75%, and the structure and the performance of the mesophase pitch-based carbon fiber are obviously improved or enhanced.
Example 3
A method for regulating and controlling the composition and structure of mesophase pitch by a co-thermal polymerization reaction. The specific process is as follows
(1) Adding 5 wt.% of cyclohexane soluble component in heavy oil into the high-aromaticity fused ring coal pitch, and stirring for 2 hours at a speed of 500r/min in a nitrogen atmosphere at a temperature higher than the softening temperature of the coal pitch to uniformly mix the pitch raw materials in a hot state;
(2) the asphalt raw materials which are uniformly mixed are subjected to self-boosting in a closed container to carry out the co-thermal polymerization reaction, wherein the co-thermal polymerization reaction conditions are as follows: stirring at 390 ℃ for 3.5h at the speed of 700 r/min;
(3) the mesophase pitch obtained by the co-thermal polymerization is used as a raw material, and the mesophase pitch-based carbon fiber is prepared by adopting melt spinning at 60 ℃ higher than the softening temperature of the mesophase pitch, oxidation non-melting at 20 ℃ lower than the softening temperature of the mesophase pitch and carbonization at 1000 ℃ in nitrogen atmosphere.
Compared with the coal tar pitch raw material without the added active component, the preparation time of the integral mesophase pitch of the embodiment is shortened by 1 h; compared with the original mesophase pitch without the active component, the H/C molar ratio of the mesophase pitch prepared by the embodiment is increased by 0.08, the softening point is reduced by 10 ℃, and the non-melting time of the spun mesophase pitch fiber can be shortened by 1.5H; compared with the mesophase pitch-based carbon fiber prepared from the original mesophase pitch without the active component, the degree of splitting of the mesophase pitch-based carbon fiber prepared by the embodiment is reduced by 60%, and the structure and the performance of the mesophase pitch-based carbon fiber are obviously improved or enhanced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (2)
1. A method for regulating and controlling the composition and structure of mesophase pitch through co-thermal polymerization is characterized by comprising the following steps:
1) adding an active component containing branched-chain aromatic hydrocarbon into the high-aromaticity condensed ring asphalt to uniformly mix asphalt raw materials in a hot state;
2) self-boosting the uniformly mixed asphalt raw material in a closed container to carry out co-heating polymerization reaction;
3) carrying out melt spinning, oxidation non-melting and high-temperature carbonization treatment on the mesophase pitch obtained by the co-thermal polymerization reaction to obtain mesophase pitch-based carbon fibers;
the high-aromaticity fused ring asphalt is any one of naphthalene asphalt, anthracene asphalt and coal asphalt, the branched-chain aromatic hydrocarbon-containing active component is a cyclohexane soluble component in petroleum asphalt or heavy oil, the addition amount of the cyclohexane soluble component is 4-15 wt% of the high-aromaticity fused ring asphalt, and the hot-state mixing process conditions are as follows: stirring for 2 hours at the speed of 500r/min at the temperature which is 80 ℃ higher than the softening temperature of the high-aromaticity condensed ring asphalt in a nitrogen atmosphere, wherein the co-thermal polymerization reaction conditions are as follows: stirring at the speed of 550-1180 r/min for 3-6 hours at the temperature of 386-432 ℃, carrying out melt spinning at the temperature 60 ℃ higher than the softening temperature of the mesophase pitch, carrying out oxidation without melting at the temperature 20 ℃ lower than the softening temperature of the mesophase pitch, and carrying out carbonization at the temperature of 1000 ℃ in a nitrogen atmosphere.
2. A mesophase pitch-based carbon fiber prepared by the method for controlling the composition and structure of mesophase pitch using the co-thermal polymerization according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811548944.7A CN109610049B (en) | 2018-12-18 | 2018-12-18 | Method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811548944.7A CN109610049B (en) | 2018-12-18 | 2018-12-18 | Method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109610049A CN109610049A (en) | 2019-04-12 |
| CN109610049B true CN109610049B (en) | 2021-09-14 |
Family
ID=66009747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811548944.7A Active CN109610049B (en) | 2018-12-18 | 2018-12-18 | Method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109610049B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0055024B1 (en) * | 1980-11-19 | 1984-10-03 | Toa Nenryo Kogyo Kabushiki Kaisha | Carbonaceous pitch, production thereof and carbon fibers therefrom |
| CN103305942A (en) * | 2013-06-06 | 2013-09-18 | 天津大学 | Spinneret plate and method for preparing mesophase pitch-based strip carbon fibers |
| CN104610994A (en) * | 2015-01-16 | 2015-05-13 | 中国海洋石油总公司 | Preparation method of mesophase pitch with low softening point and high mesophase content |
| CN106435840A (en) * | 2016-10-21 | 2017-02-22 | 中国石油大学(华东) | Preparation method of asphalt based carbon fiber |
-
2018
- 2018-12-18 CN CN201811548944.7A patent/CN109610049B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0055024B1 (en) * | 1980-11-19 | 1984-10-03 | Toa Nenryo Kogyo Kabushiki Kaisha | Carbonaceous pitch, production thereof and carbon fibers therefrom |
| CN103305942A (en) * | 2013-06-06 | 2013-09-18 | 天津大学 | Spinneret plate and method for preparing mesophase pitch-based strip carbon fibers |
| CN104610994A (en) * | 2015-01-16 | 2015-05-13 | 中国海洋石油总公司 | Preparation method of mesophase pitch with low softening point and high mesophase content |
| CN106435840A (en) * | 2016-10-21 | 2017-02-22 | 中国石油大学(华东) | Preparation method of asphalt based carbon fiber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109610049A (en) | 2019-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mochida et al. | Chemistry of synthesis, structure, preparation and application of aromatic-derived mesophase pitch | |
| Jin et al. | Accelerating the oxidative stabilization of pitch fibers and improving the physical performance of carbon fibers by modifying naphthalene-based mesophase pitch with C9 resin | |
| CN106544758B (en) | A kind of preparation method of high modulus pitch-based carbon fiber | |
| CN104087331A (en) | Mesophase pitch raw material as well as preparation method and application of mesophase pitch raw material in preparing high-performance carbon fiber | |
| CN110003932B (en) | Method for preparing high-quality mesophase pitch by ternary co-carbonization | |
| Jiang et al. | Controlling spinning pitch property by tetrahydrofuran-soluble fraction of coal tar pitch co-carbonization with petrolatum | |
| CN108485694B (en) | Method for preparing high-quality mesophase pitch by co-carbonization method | |
| CN111718740B (en) | Spinnable mesophase pitch prepared by solvent synergistic hydrogenation, preparation method and application | |
| CN111575053B (en) | Method for preparing mesophase pitch by size exclusion separation-thermal polycondensation and application thereof | |
| Guo et al. | Hydrogenation of coal tar pitch for improved mesophase pitch molecular orientation and carbon fiber processing | |
| CN1053001C (en) | Process for preparing middle phase asphalt | |
| CN104151532A (en) | Mesophase pitch raw material used for preparing high-modulus high-thermal-conductivity carbon fiber, and preparation method thereof | |
| CN108611113B (en) | Method for preparing mesophase pitch and carbon fiber by deep oxidation-catalytic polycondensation | |
| JP6026593B2 (en) | Carbon fiber pitch manufacturing method | |
| CN109610049B (en) | Method for regulating and controlling composition and structure of mesophase pitch through co-thermal polymerization | |
| CN112281260B (en) | Spinnable asphalt prepared by controlling raw material fraction, method and application of spinnable asphalt in preparation of carbon fibers | |
| CN112625722B (en) | Method for preparing spinnable asphalt by combining raw materials and application of spinnable asphalt in preparation of carbon fibers | |
| CN103923681B (en) | Mesophase pitch and utilize gelatin liquefaction refined asphaltic bitumen to prepare the method for mesophase pitch | |
| CN108264915A (en) | A kind of preparation method for spinning mesophase pitch | |
| CN105778057A (en) | Method for preparing mesophase pitch through co-carbonization | |
| CN106403579B (en) | A kind of method that mesophase pitch prepares high-quality needle coke electrode material | |
| CN116516525A (en) | Low-cost carbon fiber preparation method | |
| Chen et al. | Effect of isopropyl chloride addition in AlCl3 catalytic system on the formation of coal tar pitch-based mesophases | |
| KR20150118432A (en) | Optical anisotropic pitches from residual fuel oil, method for preparing the same, and pitch carbon fibers using the same | |
| JP2780231B2 (en) | Carbon fiber production method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |