CN108795466A - A kind of method that FCC clarified oils induction polycondensation prepares mesophase pitch - Google Patents
A kind of method that FCC clarified oils induction polycondensation prepares mesophase pitch Download PDFInfo
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- CN108795466A CN108795466A CN201810594195.5A CN201810594195A CN108795466A CN 108795466 A CN108795466 A CN 108795466A CN 201810594195 A CN201810594195 A CN 201810594195A CN 108795466 A CN108795466 A CN 108795466A
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- mesophase pitch
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- 239000011302 mesophase pitch Substances 0.000 title claims abstract description 60
- 239000003921 oil Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000006068 polycondensation reaction Methods 0.000 title claims abstract description 23
- 230000006698 induction Effects 0.000 title claims abstract description 8
- 241001597008 Nomeidae Species 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000009835 boiling Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- 238000009987 spinning Methods 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 230000016507 interphase Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 4
- 239000010620 bay oil Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 239000011294 coal tar pitch Substances 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 241000772415 Neovison vison Species 0.000 description 2
- 150000001491 aromatic compounds Chemical class 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000011329 calcined coke Substances 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- 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
- C10C3/002—Working-up pitch, asphalt, bitumen by thermal means
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Working-Up Tar And Pitch (AREA)
- Inorganic Fibers (AREA)
Abstract
The present invention provides the methods that a kind of induction polycondensation of FCC clarified oils prepares mesophase pitch.This method is that the group with naphthenic base FCC clarified oil mid-boiling points less than 530 DEG C is divided into raw material, at 390~450 DEG C of temperature, pressure 2MPa, reacts 2~10h, obtains low softening point mesophase pitch.The mesophase pitch settles 1h at 180~300 DEG C of temperature, cuts lower layer's anisotropy and is mutually used as derivant.Raw material and a certain proportion of derivant are uniformly mixed, and at 380~450 DEG C of temperature, pressure 2MPa, are reacted 2~12h, are obtained high-quality mesophase pitch.Present invention process is simple, and production cost is low, and obtained mesophase pitch anisotropic structure content is high (> 97%), and crystal characteristic size is big, and molecular arrangement and orientation degree is high, has large watershed type optical texture, and spinning properties are good.
Description
Technical field
The present invention relates to a kind of naphthenic base FCC clarified oils by inducing polycondensation process to prepare the side of spinnability mesophase pitch
Method, belongs to mink cell focus processing and carbon materials material precursor prepares interleaving techniques field.
Background technology
It is original that Carbonaceous mesophase pitch, which is with coal tar pitch, mink cell focus, high molecular polymer and other aromatic compounds etc.,
Material, a kind of nematic crystal substance obtained by the methods of thermal polycondensation, catalyzed polycondensation, it is a variety of flat plate-like condensed-nuclei aromatics groups
At mixture.It is excellent since mesophase pitch derives from a wealth of sources, have excellent performance, cheap, carbon yield is high and machinability is strong etc.
Point is acknowledged as many advanced function material (such as high-strength high-modules carbon fibre, highly heat-conductive material, electrode material, superhigh specific surface areas
Activated carbon etc.) outstanding parent, these functional materials the fields such as national defense industry, aerospace, high-end science and technology, civilian industry send out
Wave great function.
The starting material structure and preparation process of mesophase pitch be determine mesophase pitch anisotropic structure content and
The key factor of liquid crystal structure.The FCC clarified oils that catalytic cracking (FCC) technique generates are rich in polycyclic aromatic hydrocarbon compounds, carbon content
It is higher, and abundance, it is cheap, theoretically prepare the desirable feedstock of mesophase pitch.But containing certain in clarified oil
The catalyst fines of amount, this has a major impact the quality of mesophase pitch.Catalyst content has to be lower than 10 μ g/ in clarified oil
It can be only achieved the requirement for preparing high-quality carbon material when g.It is generally removed at present by the methods of electrostatic separation, filtering or vacuum distillation
Catalyst in FCC clarified oils.
Domestic Institutes Of Technology Of Taiyuan Cao Qing improves charing by the way that carbonaceous mesophase spherules are added to the method in coal tar pitch
The content of anisotropic structure in product mesophase pitch, and the liquid crystal structure of mesophase pitch is improved, by gained interphase
Pitch is further calcined, and needle coke that is structurally ordered, haveing excellent performance has been obtained.In this course, carbonaceous mesophase spherules play
The effect of derivant, induction coal tar pitch molecule polycondensation form structurally ordered mesophase pitch and subsequent product.University Of Tianjin king
At raising the influence for having investigated carbonaceous mesophase spherules and primary quinoline insolubles to coal tar asphalt thermal polycondensation reaction process, it is believed that add
The carbonaceous mesophase spherules entered can promote increasing for anisotropic structure content in system, together as the core of diauxic growth
When make generate carbonaceous mesophase spherules size increase;And seed of the quinoline insolubles as mesophase pitch, that is, it is intermediate
The core of phase carbosphere growth to reduce the high-energy barrier that anisotropy mutually generates, and then reduces the work of interphase generation
Change energy, but the mesophase pitch generated mosaic texture under polarisation is in the majority.In addition, the rivers Beijing University of Chemical Technology Song Huai to ferrocene with
The process that petroleum residual oil Co-carbonization reaction prepares mesophase pitch is studied, it is found that the presence of ferrocene can significantly improve
The thermal polycondensation rate of petroleum residual oil, and the mesophase pitch for melting simultaneously build is more readily formed, the reason is that the crystallite aligned orderly of iron,
Layer of charcoal ordered arrangement can be induced so that intermediate phase molecule lamella shows higher order.But this method products obtained therefrom
In metallic iron is difficult to remove, thus during preparing follow-up high-performance carbon fibre, mesophase pitch spinning effect is bad.
For the FCC clarified oils of composed structure complexity, only be difficult to reach by the simple technological operation of a step prepare it is high-strength
Therefore two or more process combinings are to prepare high-quality centre by the purpose for spending high modulus carbon fiber presoma mesophase pitch
The effective and feasible method of asphalt phase.The present invention is first removed the impurity such as catalyst in FCC clarified oils by reduced pressure distillation process
It goes, then by derivant synthesis and mesophase pitch induction polycondensation synthesis, two-step process is compound prepares mesophase pitch, can reach
Product anisotropic structure content is improved, improves interphase molecular structure, improves the purpose of spinning properties.
Invention content
The purpose of the present invention is being directed to the problems such as petroleum base mesophase pitch spinning properties are poor, preparation process is complicated, provide
One kind using naphthenic base FCC clarified oils mid-boiling point in 530 DEG C of distillates below as raw material, through induction pyrocondensation polymerizing technology prepare in
Between asphalt phase method.This raw low, simple for process, prepared mesophase pitch anisotropic structure content of the method production
Height, crystal characteristic size is big, and molecular arrangement and orientation degree is high, and spinning properties are good, is the excellent forerunner for producing high modulus carbon fiber
Body.
The method that a kind of FCC clarified oils induction polycondensation of the present invention prepares mesophase pitch, includes the following steps:
(1) distillate using naphthenic base FCC clarified oil mid-boiling points less than 530 DEG C is raw material;(2) raw material is in 390~450 DEG C of temperature, pressure
Under power 2MPa, 1~10h is reacted, low softening point mesophase pitch is obtained;(3) low softening point mesophase pitch temperature 180~
1h is settled at 300 DEG C, lower layer's anisotropy is cut and is mutually used as derivant;(4) FCC clarified oils and the mixing of a certain proportion of derivant
Uniformly, at 380~450 DEG C of temperature, pressure 2MPa, 2~12h is reacted, high-quality mesophase pitch is obtained.
In the step (1), naphthenic base FCC clarified oils are less than 530 DEG C by the distillate boiling point that vacuum distillation obtains.
In the step (2), reaction temperature is 415~435 DEG C, and the softening point of prepared mesophase pitch is 190~220
℃。
In the step (3), settling temperature is 210~260 DEG C, and the softening point of prepared derivant is 195~225 DEG C.
Reaction temperature is 420~440 DEG C in the step (4), and mass ratio when derivant is mixed with FCC clarified oils is
0.01~0.10:1.
It is raw material that the present invention, which chooses FCC clarified oils through being evaporated under reduced pressure distillate of the obtained boiling point less than 530 DEG C, in temperature
390~450 DEG C, under pressure 2MPa, 2~10h is reacted, low softening point mesophase pitch is obtained.The mesophase pitch is in temperature 180
1h is settled at~300 DEG C, lower layer's anisotropy is cut and is mutually used as derivant.The molecular arrangement and orientation degree of the derivant is high, has
Preferable liquid crystal structure.Then raw material and a certain proportion of derivant are uniformly mixed, in 380~450 DEG C of temperature, pressure 2MPa
Under, 2~12h is reacted, high-quality mesophase pitch is obtained.During thermal polycondensation, the derivant disperseed in the reaction system rises
To the effect of interphase incipient nucleus, the intermediate phase molecule generated in mother liquor is guided to be arranged according to incipient nucleus structure growth, Jin Ersheng
At the mesophase pitch product of molecular structure aligned orderly.
Compared with the prior art the method for the present invention has the following advantages:
1, the raw material that the present invention uses is less than 530 DEG C of distillate for naphthenic base FCC clarified oil mid-boiling points, is rich in 2-4 rings
Aromatic compound, and it is miscellaneous to have cut off catalyst for influencing that mesophase structure is formed etc. after reduced pressure distillation process for FCC clarified oils
Matter.
2, derivant used in the present invention is by Material synthesis, and non-corrosive to equipment, synthesis technology is simple, in preparation
Between asphalt phase anisotropic structure content it is high, crystal characteristic size is big, and molecular arrangement and orientation degree is high, and spinning properties are good.
3, the present invention is with short production cycle, and the introducing of derivant accelerates carbonization reaction rate, reduces reaction activity,
Be conducive to the quick formation of high-quality mesophase pitch.
Specific implementation mode
With reference to embodiment be further discussed below it is provided by the present invention with naphthenic base FCC clarified oil mid-boiling points be less than 530
DEG C distillate be raw material through inducing the polycondensation process method for preparing mesophase pitch.
The anisotropic structure content and optical texture type of mesophase pitch are measured by reflection-type petrographic microscope;It is soft
Change point to measure using conventional needling method;The crystal characteristic size of mesophase pitch is calculated using Raman spectrometer analysis;It adopts
Interphase molecular arrangement and orientation degree is calculated with X-ray diffractometer characterization;Product spinning properties pass through domestic single screw rod spinning
Machine measures.
Embodiment 1:
300mL is added not in vacuum distillate 160g by the naphthenic base FCC clarified oil mid-boiling points of Bohai Bay Oil less than 530 DEG C
It becomes rusty in steel autoclave, purges air in discharge kettle with high pure nitrogen, be warming up to 390 DEG C, it is permanent under the stirring of 500r/min
It presses 2MPa thermal polycondensations to react 11.5h, obtains the mesophase pitch that softening point is 197 DEG C, which settles at 210 DEG C
1h cuts lower layer's anisotropy and is mutually used as derivant, and the softening point of the derivant is 201 DEG C.Then, by FCC clarified oils and
The derivant of 1wt.% is uniformly mixed, and under 420 DEG C of reaction temperature, pressure 2MPa, thermal polycondensation reacts 10h, obtains anisotropy
Structural content is the 97%, mesophase pitch of large watershed type structure, and softening point is 237 DEG C, crystal characteristic size is 1.29 ×
10-2, molecular arrangement and orientation degree is 0.946, when spinning temperature is 330 DEG C, tensile strength 2.76GPa.
Embodiment 2:
300mL stainless steel autoclaves are added in the vacuum distillate 160g of the naphthenic base FCC clarified oils of Bohai Bay Oil
In, air in discharge kettle is purged with high pure nitrogen, is warming up to 450 DEG C, under the stirring of 500r/min, constant pressure 2MPa thermal polycondensations are anti-
2h is answered, the mesophase pitch that softening point is 215 DEG C is obtained, which settles 1h at 230 DEG C, cut lower layer respectively to different
Property to be mutually used as derivant, the softening point of the derivant be 221 DEG C.Then, the derivant of FCC clarified oils and 10wt.% are mixed
Uniformly, under 440 DEG C of reaction temperature, pressure 2MPa, thermal polycondensation reacts 8h, obtains anisotropic structure content and is 98%, flows greatly
The mesophase pitch of domain type structure, softening point are 263 DEG C, and crystal characteristic size is 1.32 × 10-2, molecular arrangement and orientation degree is
0.957, when spinning temperature is 340 DEG C, tensile strength 2.83GPa.
Embodiment 3:
300mL stainless steel autoclaves are added in the vacuum distillate 160g of the naphthenic base FCC clarified oils of Bohai Bay Oil
In, air in discharge kettle is purged with high pure nitrogen, is warming up to 430 DEG C, under the stirring of 500r/min, constant pressure 2MPa thermal polycondensations are anti-
7h is answered, the mesophase pitch that softening point is 201 DEG C is obtained, which settles 1h at 215 DEG C, cut lower layer respectively to different
Property to be mutually used as derivant, the softening point of the derivant be 205 DEG C.Then, the derivant of FCC clarified oils and 5wt.% are mixed equal
Even, under 440 DEG C of reaction temperature, pressure 2MPa, thermal polycondensation reacts 8h, and it is 99%, large watershed to obtain anisotropic structure content
The mesophase pitch of type structure, softening point are 241 DEG C, and crystal characteristic size is 1.37 × 10-2, molecular arrangement and orientation degree is
0.977, when spinning temperature is 338 DEG C, tensile strength 2.88GPa.
Embodiment 4:
300mL stainless steel autoclaves are added in the vacuum distillate 160g of the naphthenic base FCC clarified oils of Bohai Bay Oil
In, air in discharge kettle is purged with high pure nitrogen, is warming up to 435 DEG C, under the stirring of 500r/min, constant pressure 2MPa thermal polycondensations are anti-
7h is answered, the mesophase pitch that softening point is 208 DEG C is obtained, which settles 1h at 225 DEG C, cut lower layer respectively to different
Property to be mutually used as derivant, the softening point of the derivant be 214 DEG C.Then, the derivant of FCC clarified oils and 5wt.% are mixed equal
Even, under 430 DEG C of reaction temperature, pressure 2MPa, thermal polycondensation reacts 9h, and it is 99%, large watershed to obtain anisotropic structure content
The mesophase pitch of type structure, softening point are 248 DEG C, and crystal characteristic size is 1.41 × 10-2, molecular arrangement and orientation degree is
0.985, when spinning temperature is 338 DEG C, tensile strength 2.97GPa.
Claims (6)
1. a kind of method that FCC clarified oils induction polycondensation prepares mesophase pitch, it is characterised in that include the following steps:(1) with
Group of the naphthenic base FCC clarified oil mid-boiling points less than 530 DEG C is divided into raw material;(2) raw material is in 390~450 DEG C of temperature, pressure 2MPa
Under, 2~10h is reacted, low softening point mesophase pitch is obtained;(3) low softening point mesophase pitch is at 180~300 DEG C of temperature
1h is settled, lower layer's anisotropy is cut and is mutually used as derivant;(4) FCC clarified oils and a certain proportion of derivant are uniformly mixed,
380~450 DEG C of temperature under pressure 2MPa, reacts 2~12h, obtains high-quality mesophase pitch.
2. the preparation method of mesophase pitch as described in claim 1, it is characterised in that:In the step (1), by naphthenic base
FCC clarified oils obtain low boiling point in 530 DEG C of component as raw material by vacuum distillation.
3. the preparation method of mesophase pitch as described in claim 1, it is characterised in that:The preparation process of the mesophase pitch
The combination of polycondensation two processes of synthesis is induced for derivant synthesis and mesophase pitch.
4. the preparation method of mesophase pitch as described in claim 1, it is characterised in that:In the step (2), reaction temperature
It it is 415~435 DEG C, the softening point of prepared mesophase pitch is 190~220 DEG C.
5. the preparation method of mesophase pitch as described in claim 1, it is characterised in that:In the step (3), settling temperature
It it is 210~260 DEG C, the softening point of prepared derivant is 195~225 DEG C.
6. the preparation method of mesophase pitch as described in claim 1, it is characterised in that:Reaction temperature in the step (4)
It it is 420~440 DEG C, mass ratio when derivant is mixed with FCC clarified oils is 0.01~0.1:1.
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Cited By (2)
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---|---|---|---|---|
CN112920827A (en) * | 2021-01-21 | 2021-06-08 | 青岛农业大学 | Method for preparing mesophase pitch by seed induction |
CN114106863A (en) * | 2022-01-27 | 2022-03-01 | 克拉玛依市先进能源技术创新有限公司 | Spinning mesophase pitch and preparation method thereof |
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CN103265966A (en) * | 2013-05-18 | 2013-08-28 | 中国石油大学(华东) | Preparation method of mesophase pitch with high mesophase content |
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CN106435840A (en) * | 2016-10-21 | 2017-02-22 | 中国石油大学(华东) | Preparation method of asphalt based carbon fiber |
CN107201248A (en) * | 2017-07-17 | 2017-09-26 | 青岛科技大学 | A kind of method that FCC slurry component cutting sedimentation separation prepares mesophase pitch |
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2018
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CN103265966A (en) * | 2013-05-18 | 2013-08-28 | 中国石油大学(华东) | Preparation method of mesophase pitch with high mesophase content |
CN103923682A (en) * | 2014-04-29 | 2014-07-16 | 神华集团有限责任公司 | Intermediate-phase asphalt and method for preparing intermediate-phase asphalt from coal liquefaction refined asphalt |
CN106435840A (en) * | 2016-10-21 | 2017-02-22 | 中国石油大学(华东) | Preparation method of asphalt based carbon fiber |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112920827A (en) * | 2021-01-21 | 2021-06-08 | 青岛农业大学 | Method for preparing mesophase pitch by seed induction |
CN114106863A (en) * | 2022-01-27 | 2022-03-01 | 克拉玛依市先进能源技术创新有限公司 | Spinning mesophase pitch and preparation method thereof |
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Application publication date: 20181113 |