CN109181733A - A kind of method that coal tar pitch preparation can spin pitch - Google Patents
A kind of method that coal tar pitch preparation can spin pitch Download PDFInfo
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- CN109181733A CN109181733A CN201811160012.5A CN201811160012A CN109181733A CN 109181733 A CN109181733 A CN 109181733A CN 201811160012 A CN201811160012 A CN 201811160012A CN 109181733 A CN109181733 A CN 109181733A
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- pitch
- coal tar
- tar pitch
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- vaseline
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/08—Working-up pitch, asphalt, bitumen by selective extraction
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/026—Working-up pitch, asphalt, bitumen by chemical means reaction with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/04—Working-up pitch, asphalt, bitumen by chemical means reaction by blowing or oxidising, e.g. air, ozone
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- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
- Inorganic Fibers (AREA)
Abstract
The method that a kind of preparation of coal tar pitch can spin pitch is that middle low temperature pitch powder is broken to 20 mesh hereinafter, obtaining refined bitumen after soluble constituent recycles tetrahydrofuran solvent with the soluble constituent that tetrahydrofuran extraction filters out middle low temperature coal tar pitch；It is put into reactor after refined bitumen is mixed with vaseline, normal pressure is passed through nitrogen, 180-220 DEG C of temperature is warming up to 1-10 DEG C/min heating rate, then switch air and reactor is passed through with 10-60mL/ming rate, and it is heated to 280-350 DEG C of reaction temperature with 1-10 DEG C/min heating rate, pitch can be spun by being made after stopping 1-10 hours.The advantages of present invention has high income, cheap, thermal polycondensation moderate temperature.
Description
Technical field
The invention belongs to asphalt base carbon fiber technical fields, and in particular to a kind of method that coal tar pitch preparation can spin pitch.
Technical background
The 1980s, carbon fiber manufacturing industry is fast-developing, since it is with excellent electricity, thermodynamics
Can, it is widely used in the various fields such as national defense industry, aerospace, hard-core technology, daily life.Foreign countries have had commercialization
The ability of production, but China is also in development and trial production stage.Since beauty, day, moral are as strategic materials control, seriously
Restrict the development of the related fieldss such as China's national defense.Therefore, accelerate the research and development to carbon fiber that there is strategic importance.
General purpose grade asphalt-based carbon fiber technology is prepared to realize, has strict demand to raw material.It should meet claimed below: 1, grey
Point, content of heteroatoms it is few；2, softening point is high, usually >=210 DEG C；3, good spinnability (narrow molecular weight distribution, indissoluble object be few,
Light component is few) and thermal stability；4, high carbon yield.The raw materials for production of asphalt base carbon fiber be generally asphalt, coal tar pitch,
Pitch and ethylene bottom oil pitch etc. obtained by naphthalene oligomerisation.But that there are softening points is low for the pitch through coal tar or petroleum residual oil distillation preparation
The characteristics of (70-100 DEG C).Therefore it needs to pre-process asphalt stock before spinning, to improve its softening point.
The method for improving green softening point mainly has constant-pressure and high-temperature hot polymerization, pressurized high-temperature hot polymerization, vacuum high-temperature hot polymerization, the heat of oxidation
The methods such as polymerization, crosslinking synthetic method, catalysis synthesis process and hydrogenation modification thermal polymerization.Wherein high temperature thermopolymerization to coal tar pitch modification at
Reason amplitude is big, easy to operate, but asphalt softening point improves asphalt softening point distribution width, yield after unobvious and its polymerization
Low, poor fluidity, is unfavorable for melt spinning；Direct oxidation thermal polymerization can effectively improve the softening point of spinning asphalt, asphalt yield
Height, but there are a large amount of fixed gases to carry glance coal discharge, severe operational environment and reaction interval not easy to control after being passed through air or oxygen
Degree；And catalysis synthesis process and crosslinking synthetic method reaction temperature are violent, are difficult to control, custom catalysts are corrosive to equipment, instead
Remaining catalyst also influences subsequent spinning and carbonization technique after answering；Hydrogenation modification thermal polymerization can usually prepare good spinning
Pitch, but currently used hydrogen supply dissolvent is that naphthane holds since its boiling point is lower (207.2 DEG C) in high temperature thermopolymerization
When being easily lost by gas entrainment, hydrogen supply deficiency when causing to polymerize, and using the high polymers such as PVC, PS as hydrogen supply substance, pyrolysis
Temperature is high, and when low temperature can not generate free radicals reacts with pitch.Therefore using a kind of moderate boiling point and the hyperergic confession of pitch
It is very necessary that the modified preparation of hydrogen reagent can spin pitch.
Summary of the invention
Cheap the object of the present invention is to provide a kind of high income, the coal tar pitch preparation of thermal polycondensation moderate temperature can be spun
The method of pitch.
The present invention is using petrochemical industry by-product vaseline as the modified purified coal tar pitch of hydrogen supply dissolvent, and this method not only may be used
To effectively improve the softening point of raw material coal tar pitch, and the softening point of modified coal tar pitch is high, and melting range is narrow, and good fluidity, light component is few,
Have excellent spinning properties.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of coal tar pitch of the present invention prepares the method that can spin pitch, comprising the following steps:
Step 1: middle low temperature pitch powder is broken to 20 mesh hereinafter, filtering out middle low temperature coal tar pitch with tetrahydrofuran extraction
Soluble constituent, soluble constituent recycle tetrahydrofuran solvent after, obtain refined bitumen；
Step 2: putting into reactor after refined bitumen is mixed with vaseline, it is 10-60mL/min that normal pressure, which is passed through flow,
The nitrogen of g is warming up to 180-220 DEG C of temperature with 1-10 DEG C/min heating rate, switches air and then with 10-60mL/min
G rate is passed through reactor, and is heated to 280-350 DEG C of reaction temperature with 1-10 DEG C/min heating rate, after stopping 1-10 hours
Pitch can be spun by being made.
Above-mentioned method, the weight ratio of middle low temperature coal tar pitch and tetrahydrofuran described in step 1 are 1:4-1:10, in
The ash content of low temperature coal tar pitch is≤0.2wt%, and softening point is 70-90 DEG C.
Above-mentioned method, purification coal tar pitch described in step 1, Ash weight ratio≤0.03%, molecular weight distribution
For 200-350, softening point is 70-90 DEG C.
Above-mentioned method, vaseline described in step 2 are from the residual oil that crude oil leaves after normal pressure and vacuum distillation
The slack wax of abjection is the mixture of a kind of methane series hydrocarbon that hydrogen content is high or saturated hydrocarbons semi liquid state.Its density is 0.80-0.88g/
cm3, fusing point is 70-80 DEG C, and boiling point is 310-335 DEG C.
Ash weight ratio≤0.03% of purification coal tar pitch as described above, molecular weight distribution 200-350, softening point model
Enclose is 70-90 DEG C.
Refine coal tar pitch in step 2 as described above: vaseline weight ratio is 100:2-20.
Above-mentioned method, it is characterised in that the evaluation criterion of pitch spinnability is spun described in step 2 as single hole melting
Spin processes, each feeding quantity are that 5-30g can spin pitch, and spinning temperature is higher than 30-50 DEG C of softening point temperature, spinning pressure 0.3-
1MPa, spinning nozzle diameter are 0.3 μm, speed of wrap 200m/min.Compared with the prior art, the present invention has the following advantages:
The advantages of present invention incorporates high temperature thermopolymerization, oxidation thermal polymerization and hydrogenation modification thermal polymerizations, has processing amplitude
Greatly, short processing time, Asphalt Smoke Emission be few, easy to operate, modified effect clear advantage.And vaseline used is at low cost,
Safety is non-corrosive, hydrogen supply capacity is strong, the extent of reaction is big, so that the mobility for excessively polymerizeing and keeping pitch of pitch is avoided,
To improve the spinning properties of pitch.The melting range for spinning pitch after polymerization is narrow (≤32 DEG C), total recovery height (27-32%), soft
Change point high (212-270 DEG C), H/C atom is relatively low (0.52-0.56), and aromaticity is higher (0.76-0.82), and good spinnability is (single
Hole melt spinning length > 3.1km)；Pitch can be spun through melt spinning, the monofilament tension of asphalt-based carbon fiber is strong after pre-oxidation and carbonization
Degree is 882-981MPa, and single wire fracture elongation is 2.06-2.38%.
Below by subordinate list and example, technical scheme of the present invention will be described in further detail.
Specific embodiment
Embodiment 1
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.2wt%, softening point are 70 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:4 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design tetrahydrofuran, obtain essence
Pitch (ash content 0.03wt%, molecular weight distribution 200-350, softening point 72) processed；Coal tar pitch and vaseline will be refined with weight
Measure the ratio mixing than 50:1.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 20mL/ming
It purges and is heated to 180 DEG C with the heating rate of 5 DEG C/min.Stop being passed through nitrogen and the speed with 40mL/ming at 180 DEG C
Rate is continually fed into air, is heated to 310 DEG C with the heating rate of 5 DEG C/min, stops being passed through air and being cooled to after stopping 4 hours
Room temperature, which is made, can spin pitch, total recovery 27%.Pitch can be spun through 255 DEG C, spinning pressure 0.3MPa, spinning nozzle diameter is
0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 2
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.15wt%, softening point are 80 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:5 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen (ash
It is divided into 0.02wt%, molecular weight distribution 210-350, softening point 83)；By purification coal tar pitch and vaseline with weight ratio 50:1's
Ratio mixing.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 20mL/ming
It purges and is heated to 180 DEG C with the heating rate of 3 DEG C/min.Stop being passed through nitrogen and the speed with 20mL/ming at 180 DEG C
Rate is continually fed into air, is heated to 310 DEG C with the heating rate of 6 DEG C/min, stops being passed through air and being cooled to after stopping 4 hours
Room temperature, which is made, can spin pitch, total recovery 29%.Pitch can be spun through 242 DEG C, spinning pressure 0.5MPa, spinning nozzle diameter is
0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 3
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.1wt%, softening point are 90 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:9 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen (ash
It is divided into 0.01wt%, molecular weight distribution 240-350, softening point 90)；By purification coal tar pitch and vaseline with weight ratio 10:1's
Ratio mixing.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 25mL/ming
It purges and is heated to 210 DEG C with the heating rate of 4 DEG C/min.Stop being passed through nitrogen and the speed with 45mL/ming at 210 DEG C
Rate is continually fed into air, is heated to 320 DEG C with the heating rate of 5 DEG C/min, stops being passed through air and being cooled to after stopping 4 hours
Room temperature, which is made, can spin pitch, total recovery 32%.Pitch can be spun through 278 DEG C, spinning pressure 0.4MPa, spinning nozzle diameter is
0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 4
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.1wt%, softening point are 75 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:6 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen (ash
It is divided into 0.01wt%, molecular weight distribution 220-350, softening point 76)；By purification coal tar pitch and vaseline with weight ratio 20:1's
Ratio mixing.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 30mL/ming
It purges and is heated to 180 DEG C with the heating rate of 1 DEG C/min.Stop being passed through nitrogen and the speed with 30mL/ming at 180 DEG C
Rate is continually fed into air, is heated to 320 DEG C with the heating rate of 10 DEG C/min, stops being passed through air and cooling after stopping 5 hours
Pitch, total recovery 28% can be spun by being made to room temperature.Pitch can be spun through 264 DEG C, spinning pressure 0.6MPa, spinning nozzle diameter
It is 0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 5
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.2wt%, softening point are 85 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:8 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen (ash
It is divided into 0.015wt%, molecular weight distribution 210-340, softening point 83)；By purification coal tar pitch and vaseline with weight ratio 5:1's
Ratio mixing.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 20mL/ming
It purges and is heated to 200 DEG C with the heating rate of 8 DEG C/min.Stop being passed through nitrogen and the speed with 40mL/ming at 200 DEG C
Rate is continually fed into air, is heated to 330 DEG C with the heating rate of 2 DEG C/min, stops being passed through air and being cooled to after stopping 4 hours
Room temperature, which is made, can spin pitch, total recovery 30%.Pitch can be spun through 270 DEG C, spinning pressure 0.8MPa, spinning nozzle diameter is
0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 6
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.12wt%, softening point are 80 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:5 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen (ash
It is divided into 0.01wt%, molecular weight distribution 220-330, softening point 81)；By purification coal tar pitch and vaseline with weight ratio 5:1's
Ratio mixing.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 24mL/ming
It purges and is heated to 200 DEG C with the heating rate of 2 DEG C/min.Stop being passed through nitrogen and the speed with 38mL/ming at 200 DEG C
Rate is continually fed into air, is heated to 330 DEG C with the heating rate of 6 DEG C/min, stops being passed through air and cooling after stopping 10 hours
Pitch, total recovery 29% can be spun by being made to room temperature.Pitch can be spun through 284 DEG C, spinning pressure 1.0MPa, spinning nozzle diameter
It is 0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 7
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.18wt%, softening point are 81 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:10 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen
(ash content 0.011wt%, molecular weight distribution 210-350, softening point 80)；Coal tar pitch and vaseline will be refined with weight ratio
The ratio of 10:1 mixes.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 28mL/ming
It purges and is heated to 220 DEG C with the heating rate of 5 DEG C/min.Stop being passed through nitrogen and the speed with 55mL/ming at 220 DEG C
Rate is continually fed into air, is heated to 350 DEG C with the heating rate of 5 DEG C/min, stops being passed through air and being cooled to after stopping 7 hours
Room temperature, which is made, can spin pitch, total recovery 30%.Pitch can be spun through 276 DEG C, spinning pressure 0.7MPa, spinning nozzle diameter is
0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
Embodiment 8
The preparation method of the present embodiment vaseline modified pitch the following steps are included:
Step 1: middle low temperature coal tar pitch (ash content 0.17wt%, softening point are 78 DEG C) is crushed to 20 mesh hereinafter, with four
Hydrogen furans mass ratio 1:7 mixing, extraction filter out the soluble constituent of medium temperature coal pitch, after recycling design, obtain refined bitumen (ash
It is divided into 0.013wt%, molecular weight distribution 220-340, softening point 80)；Coal tar pitch and vaseline will be refined with weight ratio 20:1
Ratio mixing.
Step 2: mixed material described in step 1 is put into reactor, it is passed through the nitrogen normal pressure of 30mL/ming
It purges and is heated to 180 DEG C with the heating rate of 10 DEG C/min.Stop being passed through nitrogen and with 60mL/ming's at 180 DEG C
Rate is continually fed into air, is heated to 310 DEG C with the heating rate of 1 DEG C/min, stops being passed through air and cooling after stopping 7 hours
Pitch, total recovery 27% can be spun by being made to room temperature.Pitch can be spun through 271 DEG C, spinning pressure 0.5MPa, spinning nozzle diameter
It is 0.3 μm, speed of wrap 200m/min melt spinning, pitch good spinning property.
The Specifications of the vaseline modified pitch of each embodiment preparation of table
It is available by above table, it is produced within the scope of the present invention to spin before pitch is excellent asphalt-based carbon fiber
Drive body.
The preferred embodiment of the present invention has been described above in detail, but during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, these
Simple modification all belongs to the scope of protection of the present invention.
In addition, various embodiments of the present invention can be combined randomly, without departing from this hair
Bright thought should be considered as content disclosed in this invention.
Claims (8)
1. a kind of coal tar pitch prepares the method that can spin pitch, it is characterised in that include the following steps:
Step 1: middle low temperature pitch powder is broken to 20 mesh hereinafter, with tetrahydrofuran extraction filter out middle low temperature coal tar pitch can
Molten component obtains refined bitumen after soluble constituent recycles tetrahydrofuran solvent；
Step 2: putting into reactor after refined bitumen is mixed with vaseline, it is 10-60mL/ming's that normal pressure, which is passed through flow,
Nitrogen is warming up to 180-220 DEG C of temperature with 1-10 DEG C/min heating rate, switches air and then with 10-60mL/ming
Rate is passed through reactor, and is heated to 280-350 DEG C of reaction temperature with 1-10 DEG C/min heating rate, after stopping 1-10 hours
Pitch can be spun by being made.
2. a kind of coal tar pitch as described in claim 1 prepares the method that can spin pitch, it is characterised in that the middle low temperature of step 1
The weight ratio of coal tar pitch and tetrahydrofuran is 1:4-1:10.
3. a kind of coal tar pitch as described in claim 1 prepares the method that can spin pitch, it is characterised in that middle low temperature coal tar pitch
Ash content is≤0.2wt%, and softening point is 70-90 DEG C.
4. a kind of coal tar pitch as described in claim 1 prepares the method that can spin pitch, it is characterised in that the refining coal drip
Blueness, Ash weight ratio≤0.03%, molecular weight distribution 200-350, softening point are 70-90 DEG C.
5. a kind of coal tar pitch as described in claim 1 prepares the method that can spin pitch, it is characterised in that vaseline in step 2
Density is 80-0.88g/cm3, fusing point is 70-80 DEG C, and boiling point is 310-335 DEG C.
6. benefit require 5 described in a kind of coal tar pitch prepare the method that can spin pitch, it is characterised in that vaseline described in step 2
It is a kind of methane series hydrocarbon that hydrogen content is high or full for the slack wax deviate from from the residual oil that crude oil leaves after normal pressure and vacuum distillation
With the mixture of hydro carbons semi liquid state.
7. a kind of coal tar pitch as described in claim 1 prepares the method that can spin pitch, it is characterised in that smart in the step 2
Coal tar pitch processed: vaseline weight ratio is 100:2-20.
8. spinning pitch such as any one of claim 1-7 the method preparation, it is characterised in that the melting range that can spin pitch is≤
32 DEG C, softening point is 212-270 DEG C, and relatively low H/C atom is 0.52-0.56, aromaticity 0.76-0.82.
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| CN201811160012.5A CN109181733B (en) | 2018-09-30 | 2018-09-30 | Method for preparing spinnable asphalt from coal tar pitch |
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| CN201811160012.5A CN109181733B (en) | 2018-09-30 | 2018-09-30 | Method for preparing spinnable asphalt from coal tar pitch |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540853A (en) * | 2019-08-12 | 2019-12-06 | 中国科学院山西煤炭化学研究所 | Method for preparing spinnable asphalt from pyromellitic dianhydride and polystyrene modified coal pitch |
| CN110578188A (en) * | 2019-08-12 | 2019-12-17 | 中国科学院山西煤炭化学研究所 | Method for preparing spinnable asphalt by co-thermal polycondensation of acid anhydride modified coal asphalt and kerosene co-refining residue |
| CN111363577A (en) * | 2020-03-12 | 2020-07-03 | 中国科学院山西煤炭化学研究所 | Spinnable asphalt for coal-based general-grade asphalt carbon fibers and preparation method thereof |
| CN111501134A (en) * | 2020-05-28 | 2020-08-07 | 陕西师范大学 | Method for preparing general-purpose asphalt-based carbon fiber from coal liquefaction residues |
| CN112442385A (en) * | 2019-09-03 | 2021-03-05 | 中国石油化工股份有限公司 | Process for preparing spinnable pitch |
| CN113718374A (en) * | 2021-09-06 | 2021-11-30 | 山东瑞城宇航碳材料有限公司 | Preparation method of low-cost asphalt-based carbon fiber for composite material |
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