CN102260513A - Coal pitch chemical modification method for carbon fiber preparation - Google Patents
Coal pitch chemical modification method for carbon fiber preparation Download PDFInfo
- Publication number
- CN102260513A CN102260513A CN201110179432XA CN201110179432A CN102260513A CN 102260513 A CN102260513 A CN 102260513A CN 201110179432X A CN201110179432X A CN 201110179432XA CN 201110179432 A CN201110179432 A CN 201110179432A CN 102260513 A CN102260513 A CN 102260513A
- Authority
- CN
- China
- Prior art keywords
- coal
- tar pitch
- coal pitch
- pitch
- chemical modification
- 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.)
- Pending
Links
Landscapes
- Working-Up Tar And Pitch (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a coal pitch chemical modification method for carbon fiber preparation. The method comprises the following operation steps of: drying coal pitch at the temperature of 110-120 DEG C to constant weight; mixing solvent quinoline with the coal pitch according to the volume mass ratio of (3-15):1 and stirring for 5-15 hours to obtain a mixed solution; filtering the mixed solution to obtain a filter solution; pouring the filter solution into a reactor; heating under the condition of continuously charging nitrogen and stirring; when heating to 80-120 DEG C, adding catalyst into the filter liquid according to the coal pitch mass of 1-16 percent, wherein the catalyst is the mixture of boron fluoride etherate and nitryl aromatic hydrocarbon; reacting at 100-180 DEG C for 5-10 hours; and heating and distilling to obtain solvent quinoline till the quinoline solvent is not distilled to obtain chemical modified coal pitch with the viscosity of 1,000-3,400Pa.s at 190 DEG C. The invention can smoothly realize the chemical modification of the coal pitch just by using chemical reaction catalyst, has the advantages of simple process and good modification effect and successfully realizes the aim of preparing carbon fiber precursor high-quality coal pitch, and the modified coal pitch achieves easy spinning and easy carbonization.
Description
Technical field
The invention belongs to the high-strength carbon fiber preparing technical field, be specifically related to a kind of carbon fiber precursor coal-tar pitch chemical modification method.
Background technology
The raw material of preparation carbon fiber is the material of high carbon content.Having Commercial Prospect is polyacrylonitrile and pitch etc.Pitch is the resistates of petrochemical industry product after processing of carbon, can be divided into petroleum pitch and coal-based pitch according to the source.There is large by product---coal-tar pitch in the coal tar industry, has only coal-tar pitch is carried out deep processing, just can make full use of the petrochemical industry resource of carbon.The coal Poly-generation technology is the new technique of maximum using coal resources, but also there is a large amount of useless excess---the coal-tar pitch problem that exists in the insurmountable course of processing in this technology.Have only the outlet that has solved the Poly-generation resistates, the coal Poly-generation technology just can develop in depth.One of approach that solves coal-based pitch is the feedstock production carbon fiber with the coal-tar pitch exactly, and the realization bituminous is turned waste into wealth, and can also reduce the discharging of energy consumption and pollutent simultaneously.Prepare carbon fiber with coal-based pitch much more the research report is arranged, and the domestic production line that comparative maturity is also arranged, but also there is the weak link of some theoretical investigationes in these production lines, the problem that the coal-tar pitch base carbon fibre matter that causes producing exists quality unstable and high performance to be obstructed.Coal-tar pitch prepares aspects such as the carbonization technology of equipment and technology that the present focus of carbon fiber mainly concentrates on the spinning of the modification of coal-tar pitch and reformation, coal-tar pitch, coal pitch fibers and equipment.The purpose of coal-tar pitch modification is in order to optimize molecular structure, to improve bituminous molecular weight and molecular weight distribution, with the preparation high-performance carbon fibre.The modification of coal-tar pitch mainly contains physically modified and two aspects of chemical modification, and physically modified belongs to the blending technology of external coal-tar pitch component, and purpose is to improve the Physical Processing performance of coal-tar pitch and strengthens spinning property.Chemical modification is to carry out the work from the component structure variation aspect of coal-tar pitch, can be the chemical modification that adds reactive component, also can be the chemical modification of non-extraneous component.The research work of [Yang Jianmin, the modulation of coal-tar pitch hydrogenation can be spun pitch research fuel and chemical industry, 2010,41 (2): 58] Yang Jianmin is exactly to adopt to add the chemical modification that the reactive component pure hydrogen is realized coal-tar pitch.Domestic a plurality of scientific research group studies two ethene derivatives be linking agent, under the effect of organic acid or mineral acid, coal-tar pitch is implemented the chemical modification of extraneous component, can prepare the raw material of wood-charcoal material modifying asphalt of excellent property.[woods waviness, Li Tiehu, Xie Gang, single tinkling of pieces of jade, Chen Yan. the crosslinked at low temperature legal system is equipped with raw material of wood-charcoal material modifying asphalt. the plain technology .2001 (4) of charcoal; Su Wu, woods waviness, Qin Tao, Xie Qionglin.The technology and the performance of Vinylstyrene modified coal pitch are ground. coal conversion .208 (3)].The interpolation of these components certainly will cause the carbon content of modified coal pitch to descend.The thermopolymerization technology belongs to coal-tar pitch chemical modification a kind of of non-extraneous component, [Xiao Jing, Wang Ying, Liu Yongdong, Lai Yanqing, Li Jili. the Progress in Modification of coal-tar pitch. carbon technique.2011(2)], high temperature thermopolymerization is meant pitch is heated to more than 400 ℃ to remove volatile matter, the method for modifying of raising high molecular aromatic compounds content and raising coking value.But pyroprocessing has been brought the consumption of the energy and the increase of production cost.The core content of the application's patent is exactly the chemical modification that realizes the non-extraneous component of low temperature coal-tar pitch in the chemical catalyst mode, the directly polycondensation of catalysis coal-tar pitch component, reach and optimize the coal-tar pitch microtexture, improve the purpose that the coal-tar pitch intermediate phase is formed, thereby promote the spinning property and the carbon fiber quality of coal-tar pitch.
Summary of the invention
In order to prepare high-strength carbon fiber, the present invention proposes the thinking of its presoma coal-tar pitch microtexture of modification, so provide a kind of method of chemical modification of simple catalysis coal-tar pitch auto-polymerization, promptly a kind of coal-tar pitch chemical modification method that is used for the carbon fiber preparation.
Realize that the above-mentioned purpose technical solution is such:
Coal-tar pitch is dried to constant weight in 110～120 ℃ of conditions of temperature, to remove moisture; By volume mass ratio 3～15:1 mixes stirring at room 5～15 hours with solvent quinoline and coal-tar pitch; Obtain mixing solutions; Filter mixing solutions, get filtrate; Pour filtrate into reaction vessel, heating under continuing logical nitrogen, stirring when being heated to 80～120 ℃, being pressed 1～16% of coal-tar pitch quality and is added catalyzer in filtrate.Primary Catalysts is a boron trifluoride diethyl etherate, and cocatalyst is oil of mirbane or 1-nitro-naphthalene or 2-nitro-naphthalene or o-dinitrobenzene or paradinitrobenzene.100～180 ℃ of down reactions 5～10 hours, heating distilling off solvent quinoline till waiting not have the quinoline solvent and distilling out, obtains the chemical modification coal-tar pitch; Adopting the described chemical modification coal-tar pitch of board-like rheometer test k value is 1000～3500Pas
The condition of test: adopt board-like rheometer to carry out temperature scanning, temperature rise rate is 5 ℃/min, and the test angles frequency is 6.3rad/s.Get the k value of 190 ℃ of correspondences on the flow curve, as the modification evaluation index.
The preparation of coal-tar pitch base carbon fibre generally comprises flow processs such as raw material abstraction, polycondensation, spinning, carbonization.The committed step of the synthetic carbon fiber of control is the coal-tar pitch polycondensation of carbon fiber precursor and the high temperature cabonization reaction of carbon fiber.Coal-tar pitch is complicated heterogeneous system, and aspects such as the aromatization degree of different solvents extract, composition, character, molecular structure are all different.Toluene, tetrahydrofuran (THF), quinoline etc. can be used as extraction solvent, and experiment finds that the quinoline extract is the fat coal pitch that relatively is fit to the preparation carbon fiber precursor.
Though the quinoline extract of coal-tar pitch can spin even successive pitch fibers, but because its aromaticity, phenyl ring degree of condensing are low, the carbon fiber strength that obtains of carbonization is not enough thus, thus need carry out the polycondensation modification to extract earlier, to form the higher condensed aromatics of condensation degree.Carry out polycondensation with catalyst pitch, optimize the bituminous microtexture, improve the bituminous spinning property, finally reach carbon content and the mechanical strength that improves coal-tar pitch base fiber.
The Primary Catalysts that the present invention uses is a boron trifluoride diethyl etherate, and cocatalyst mainly is oil of mirbane, paradinitrobenzene, Meta-dinitrobenzene, 1-nitro-naphthalene, 2-nitro-naphthalene.
The structure of catalyzer of the present invention has the Lewis acid feature of the electronic capability accepted, and this catalyzer can be regarded as and the atom of electron pair or the centrosome that atomic group can form coordinate bond are provided.
The catalysis coal-tar pitch polymeric principles of chemistry: the catalyzer boron trifluoride diethyl etherate can be accepted an electronics, forms a coordinate Electron Affinities active centre, and this is the initial substance that chemical reaction takes place.This active centre be with the coal-tar pitch component in the initial substance of aromatic ring generation chemical reaction, electrophilic substitution reaction takes place in activity site such as the α or the β position of it and aromatic ring, connects a group on aromatic ring.Obtain reaction if a plurality of close electricity take place, then on this aromatic ring, can form the group of a plurality of replacements at an aromatic ring.If an alkyl contains two active groups and the catalysis electrophilic substitution reaction takes place twice, then a kind of situation replaces at an aromatic ring generation secondary, and the result forms a hydrocarbon ring on an aromatic ring, and this is the basis that aromatic condensed ring forms; Another kind of situation replaces on two aromatic rings, and these two aromatic rings are connected as a result, impels the coal-tar pitch molecular weight to increase.If participating in the reactant of electrophilic substitution reaction is aromatic derivatives, then may form and and aromatic ring, again by further chemical reaction, then may form thick and aromatic ring.The logical high so greatly aromaticity of coal-tar pitch forms more mesophase pitch.
Aluminum trihalide (AlX
3) be a kind of common catalyzer with this catalyst structure feature.What need special instruction is with AlX
3When carrying out the modification of coal-tar pitch catalytic chemistry for catalyzer, can the auto-polymerization of catalysis coal-tar pitch, owing to do not participate in chemical reaction as catalyst themselves, it remains in, and there is disadvantageous effect in the following process to coal-tar pitch in the polymerisate, so the described catalyzer of the application's patent can not be analogized AlX is arranged
3Deng material.
With the boron trifluoride diethyl etherate is Primary Catalysts, and the polycondensation effect of coal-tar pitch is remarkable.With the condensation polymerization reaction that the collaborative above-mentioned Primary Catalysts of cocatalyst nitro-aromatic can improve coal-tar pitch more significantly, optimize the coal-tar pitch microtexture, strengthen the spinning property of intermediate phase coal-tar pitch, improve the mechanical property of coal-tar pitch base fiber.
With the boron trifluoride diethyl etherate is Primary Catalysts, and cocatalyst has oil of mirbane, paradinitrobenzene, o-dinitrobenzene, Meta-dinitrobenzene, 1-nitro-naphthalene, 2-nitro-naphthalene.Use cocatalyst to improve the coal-tar pitch modified effect effectively, improved the carbon content of coal-tar pitch carbon fiber and the tensile strength of final carbonizedfibres.
The Primary Catalysts boron trifluoride diethyl etherate is different with the cocatalyst consumption, to the modified effect difference of coal-tar pitch, and generalized case, along with the increase of catalyst levels, the corresponding rising of the softening temperature of modified coal pitch, viscosity increased.This show reaction medium pitch molecule through condensation, condense, cause the coal-tar pitch molecular change big, molecular weight improves.But there is dialectical nature in the use of catalyzer, and the catalyzer usage quantity is little, and the modified effect of coal-tar pitch is bad.The catalyzer usage quantity is big, causes the molecular change of modified coal pitch big, and softening temperature raises, and can giving subsequently so on the contrary, the spinning technique of coal-tar pitch causes difficulty.Simultaneously, assorted elements such as nitrogen, oxygen are introduced in the affiliation that adds of catalyzer, the too much intensity that adds affiliation reduction carbon fiber.Take all factors into consideration, should select the appropriate catalyst consumption, i.e. the effective modification of the coal-tar pitch of Bao Zhenging, the high carbon content of guarantee coal-tar pitch can make modified coal pitch have good flowing property again, is convenient to melt-spinning.
Modified coal pitch of the present invention is to reel off raw silk from cocoons to finish in 140-180 ℃ of following nitrogen atmosphere, can determine the diameter of coal pitch fibers according to the speed of reeling off raw silk from cocoons.
Carbonization is the key link of preparation carbon fiber; carbonization is exactly under nitrogen protection heating makes the inner chemical reactions such as crosslinked, cyclisation, polycondensation and aromizing that further take place of coal-tar pitch; the aromatic ring plane net is constantly grown up, form the cancellated process of mainly forming of aromatic ring two dimensional surface by carbon.Coal pitch fibers carbonization of the present invention is to finish under 1200 ℃.
The present invention is only using chemical reaction catalyst just can realize the chemical modification of coal-tar pitch smoothly, and technology is simple, and modified effect is good, and modified coal pitch of the present invention reaches easy spinning and easily carbonization, successfully realizes preparation carbon fiber precursor fat coal pitch purpose.
Embodiment
Below in conjunction with embodiment, the present invention is done to describe further.
Embodiment 1
Take by weighing softening point temperature and be 50 ℃ coal-tar pitch place 110 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 5:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 5 hours.After stirring end, liquid in the extraction container is carried out suction filtration, extract filtrate.Filtrate is poured in the reaction vessel, continuing logical nitrogen, constantly be heated to 100 ℃ under the agitation condition, 10 hours for some time of reaction.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.70 ℃ of viscosity through rheometer test are 80Pa.s.
Embodiment 2
Take by weighing softening temperature and be 50 ℃ coal-tar pitch place 120 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 3:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 15 hours.Stir and finish, liquid in the extraction container is carried out suction filtration, obtain filtrate.Filtrate is poured in the reaction vessel, add the catalyzer boron trifluoride diethyl etherate of coal-tar pitch quality 1% when under continuing logical nitrogen, stirring, being heated to 100 ℃.Reacted 5 hours down at 100 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.Through rheometer test, its viscosity is 600Pas in the time of 70 ℃.
Embodiment 3
Take by weighing softening temperature and be 50 ℃ coal-tar pitch place 120 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 5:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 10 hours.After stirring end, liquid in the extraction container is carried out suction filtration, extract filtrate.Filtrate is poured in the reaction vessel, add the catalyzer boron trifluoride diethyl etherate of coal-tar pitch quality 5% when under continuing logical nitrogen, the continuous stirring, being heated to 100 ℃.Reacted 8 hours down at 110 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.190 ℃ of viscosity through rheometer test are 1500Pa.s.
Embodiment 4
Take by weighing softening temperature and be 60 ℃ coal-tar pitch place 120 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 8:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 10 hours.After stirring end, liquid in the beaker is carried out suction filtration, extract filtrate.Suction filtration liquid is poured in the reaction vessel, added catalyzer, the 1-nitro-naphthalene of the boron trifluoride diethyl etherate of coal-tar pitch quality 4% and coal-tar pitch quality 4% when under continuing logical nitrogen, continuous stirring condition, being heated to 100 ℃.Reacted 10 hours down at 130 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.190 ℃ of viscosity through rheometer test are 1800Pa.s.
Embodiment 5
Take by weighing softening temperature and be 60 ℃ coal-tar pitch place 120 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 15:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 10 hours.After stirring end, liquid in the extraction container is carried out suction filtration, extract filtrate.Filtrate is poured in the reaction vessel, add catalyzer, the oil of mirbane of coal-tar pitch quality 5% boron trifluoride diethyl etherate and coal-tar pitch quality 5% when under continuing logical nitrogen, the continuous stirring, being heated to 100 ℃ respectively.Reacted 10 hours down at 140 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.190 ℃ of viscosity through rheometer test are 2400Pa.s.
Embodiment 6
Take by weighing softening temperature and be 70 ℃ coal-tar pitch place 110 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 5:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 10 hours.After stirring end, liquid in the extraction container is carried out suction filtration, extract filtrate.Filtrate is poured in the reaction vessel, continuing logical nitrogen, constantly stirring and add catalyzer, the i.e. paradinitrobenzene of the boron trifluoride diethyl etherate of coal-tar pitch quality 5% and coal-tar pitch quality 5% when being heated to 100 ℃ under the part respectively.React 10 hours for some time down at 140 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.190 ℃ of viscosity through rheometer test are 2500Pa.s.
Embodiment 7
Take by weighing softening temperature and be 70 ℃ coal-tar pitch place 110 ℃ of baking ovens to constant weight to remove moisture.With solvent quinoline mass ratio 10:1(solvent volume by volume: the coal-tar pitch quality) add and hold in the extraction container of coal-tar pitch stirring at room 10 hours.After stirring end, liquid in the extraction container is carried out suction filtration, extract filtrate.Filtrate is poured in the reaction vessel, continuing logical nitrogen, constantly stirring and add catalyzer, i.e. the 2-nitro-naphthalene of the boron trifluoride diethyl etherate of coal-tar pitch quality 6% and coal-tar pitch quality 6% when being heated to 100 ℃ under the part respectively.React 10 hours for some time down at 140 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.190 ℃ of viscosity through rheometer test are 2900Pa.s.
Embodiment 8
Take by weighing softening temperature and be 90 ℃ coal-tar pitch place 110 ℃ of baking ovens to constant weight to remove moisture.With the solvent quinoline in the 10:1(solvent volume: the ratio coal-tar pitch quality) adds and holds in the extraction container of coal-tar pitch stirring at room 5 hours.After stirring end, liquid in the extraction container is carried out suction filtration, extract filtrate.Filtrate is poured in the reaction vessel, continuing logical nitrogen, constantly stirring and add catalyzer, the i.e. o-dinitrobenzene of the boron trifluoride diethyl etherate of coal-tar pitch quality 8% and coal-tar pitch quality 8% when being heated to 100 ℃ under the part respectively.React 10 hours for some time down at 180 ℃.Heat the distilling off solvent quinoline then, till waiting not have the quinoline solvent and distilling out, reaction finishes.Get modified coal pitch.190 ℃ of viscosity through rheometer test are 3400Pa.s.
Claims (3)
1. one kind is used for the coal-tar pitch chemical modification method that carbon fiber prepares, and it is characterized in that operation steps is as follows:
1.1, coal-tar pitch is dried to constant weight in 110～120 ℃ of conditions of temperature, to remove moisture; By volume mass ratio 3～15:1 mixes stirring at room 5～15 hours with solvent quinoline and coal-tar pitch; Obtain mixing solutions; Filter mixing solutions, get filtrate;
1.2, pour filtrate into reaction vessel, heating under continuing logical nitrogen, stirring, when being heated to 80～120 ℃, in filtrate, press 1～16% of coal-tar pitch quality and add catalyzer, catalyzer is a boron trifluoride diethyl etherate, reacts 5～10 hours heating distilling off solvent quinoline down at 100～180 ℃, till waiting not have the quinoline solvent and distilling out, obtain the chemical modification coal-tar pitch; 190 ℃ of viscositys of described chemical modification coal-tar pitch are 1000～3400Pas.
2. a kind of coal-tar pitch chemical modification method that is used for the carbon fiber preparation according to claim 1, it is characterized in that: described catalyzer boron trifluoride diethyl etherate is a Primary Catalysts, also comprises cocatalyst, the consumption mass ratio of Primary Catalysts and cocatalyst is 1:1; Described cocatalyst is oil of mirbane or 1-nitro-naphthalene or 2-nitro-naphthalene or o-dinitrobenzene or paradinitrobenzene.
3. a kind of coal-tar pitch chemical modification method that is used for the carbon fiber preparation according to claim 1, it is characterized in that: the softening temperature of described coal-tar pitch is 50-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110179432XA CN102260513A (en) | 2011-06-30 | 2011-06-30 | Coal pitch chemical modification method for carbon fiber preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110179432XA CN102260513A (en) | 2011-06-30 | 2011-06-30 | Coal pitch chemical modification method for carbon fiber preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102260513A true CN102260513A (en) | 2011-11-30 |
Family
ID=45007364
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110179432XA Pending CN102260513A (en) | 2011-06-30 | 2011-06-30 | Coal pitch chemical modification method for carbon fiber preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102260513A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272754A (en) * | 2019-05-13 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of high purity aromatics asphalt production process for high-end carbon material |
| CN111004641A (en) * | 2019-12-27 | 2020-04-14 | 西安郎格飞博科技有限公司 | Spinnable asphalt and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4758326A (en) * | 1984-10-05 | 1988-07-19 | Kawasaki Steel Corporation | Method of producing precursor pitches for carbon fibers |
| US5601794A (en) * | 1991-12-25 | 1997-02-11 | Mitsubishi Chemical Corporation | Pitch type carbon fibers and process for their production |
| CN101294090A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Fine purification method for coal tar pitch |
| CN101525543A (en) * | 2009-04-07 | 2009-09-09 | 汝南县东旭碳材塑料有限公司 | Preparation method for intermediate phase asphalt |
| CN101580729A (en) * | 2009-06-11 | 2009-11-18 | 煤炭科学研究总院 | Method for preparing mesophase asphalt by coal liquefaction residue |
| CN101654619A (en) * | 2008-08-22 | 2010-02-24 | 中钢集团鞍山热能研究院有限公司 | Production process of coal raw material refined asphalt for carbon fibers |
-
2011
- 2011-06-30 CN CN201110179432XA patent/CN102260513A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4758326A (en) * | 1984-10-05 | 1988-07-19 | Kawasaki Steel Corporation | Method of producing precursor pitches for carbon fibers |
| US5601794A (en) * | 1991-12-25 | 1997-02-11 | Mitsubishi Chemical Corporation | Pitch type carbon fibers and process for their production |
| CN101294090A (en) * | 2007-04-25 | 2008-10-29 | 淄博矿业集团有限责任公司 | Fine purification method for coal tar pitch |
| CN101654619A (en) * | 2008-08-22 | 2010-02-24 | 中钢集团鞍山热能研究院有限公司 | Production process of coal raw material refined asphalt for carbon fibers |
| CN101525543A (en) * | 2009-04-07 | 2009-09-09 | 汝南县东旭碳材塑料有限公司 | Preparation method for intermediate phase asphalt |
| CN101580729A (en) * | 2009-06-11 | 2009-11-18 | 煤炭科学研究总院 | Method for preparing mesophase asphalt by coal liquefaction residue |
Non-Patent Citations (1)
| Title |
|---|
| KAP SEUNG YANG: "Preparations of Carbon Fibers from Precursor Pitches Synthesized with Coal Tar of Petroleum Residue Oil", 《FIBERS AND POLYMERS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272754A (en) * | 2019-05-13 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of high purity aromatics asphalt production process for high-end carbon material |
| CN111004641A (en) * | 2019-12-27 | 2020-04-14 | 西安郎格飞博科技有限公司 | Spinnable asphalt and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103265008B (en) | Nitrogen-doped porous carbon and preparation method thereof | |
| 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 | |
| CN111501134B (en) | Method for preparing general-purpose asphalt-based carbon fiber from coal liquefaction residues | |
| CN107720721B (en) | Mesocarbon microspheres and preparation method thereof | |
| CN102399563A (en) | Method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization | |
| CN111575037B (en) | Preparation method of high-modulus carbon fiber and precursor mesophase pitch thereof | |
| Liu et al. | Controllable synthesis of isotropic pitch precursor for general purpose carbon fiber using waste ethylene tar via bromination–dehydrobromination | |
| CN104087331A (en) | Mesophase pitch raw material as well as preparation method and application of mesophase pitch raw material in preparing high-performance carbon fiber | |
| CN103204501A (en) | Method for preparation of activated carbon from carbon-rich residue of high temperature coal tar or coal tar pitch | |
| CN108441244A (en) | A kind of preparation method of mesocarbon microspheres and mesophase pitch | |
| CN103359702A (en) | Preparation method of mesophase carbon microspheres with different particle sizes | |
| CN102899061B (en) | Method for preparing high-purity mesophase pitch and prepared high-purity mesophase pitch | |
| Lee et al. | Preparation and characterization of high-spinnability isotropic pitch from 1-methylnaphthalene-extracted low-rank coal by co-carbonization with petroleum residue | |
| Ni et al. | Chemical Modification of Asphaltene with SEBS as Precursor for Isotropic Pitch‐Based Carbon Fiber | |
| CN103740396B (en) | The method of modifying of modifying asphalt, DCL/Direct coal liquefaction hard pitch and application thereof | |
| CN105238431A (en) | Method for preparing mesophase pitch through catalytic cracking oil slurry hydrogenation reduction and co-carbonization | |
| Zhang et al. | Influence of Lignin units on the properties of Lignin/PAN‐derived carbon fibers | |
| Jiang et al. | Controlling spinning pitch property by tetrahydrofuran-soluble fraction of coal tar pitch co-carbonization with petrolatum | |
| Lou et al. | Structural modification of petroleum pitch induced by oxidation treatment and its relevance to carbonization behaviors | |
| CN102260513A (en) | Coal pitch chemical modification method for carbon fiber preparation | |
| CN103755926B (en) | Condensation multinuclear polyaromatic hydrocarbon resin and preparation method thereof | |
| CN108611113B (en) | Method for preparing mesophase pitch and carbon fiber by deep oxidation-catalytic polycondensation | |
| CN106544759A (en) | A kind of preparation method of petroleum pitch-based carbon fiber | |
| CN112852462B (en) | Continuous preparation method of oil-based raw material for mesophase pitch production | |
| CN110205157A (en) | A kind of method of solid catalyst in removing catalytic cracked oil pulp |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111130 |