CN114477132A - Mesocarbon microbeads and preparation method thereof - Google Patents
Mesocarbon microbeads and preparation method thereof Download PDFInfo
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- CN114477132A CN114477132A CN202210086436.1A CN202210086436A CN114477132A CN 114477132 A CN114477132 A CN 114477132A CN 202210086436 A CN202210086436 A CN 202210086436A CN 114477132 A CN114477132 A CN 114477132A
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- 239000002931 mesocarbon microbead Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004005 microsphere Substances 0.000 claims abstract description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 68
- 238000010438 heat treatment Methods 0.000 claims abstract description 61
- 239000002028 Biomass Substances 0.000 claims abstract description 24
- 239000010426 asphalt Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000011294 coal tar pitch Substances 0.000 claims abstract description 17
- 239000011269 tar Substances 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 239000011317 mixed pitch Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000010000 carbonizing Methods 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 15
- 239000004744 fabric Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000011336 carbonized pitch Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000011302 mesophase pitch Substances 0.000 abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000011295 pitch Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 238000006068 polycondensation reaction Methods 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011325 microbead Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
Abstract
The invention discloses a mesocarbon microbead and a preparation method thereof, wherein the preparation method comprises the following steps: (1) after centrifugal filtration, mixing the biomass tar with coal tar pitch according to the mass ratio of 0.1-0.2: 1 to obtain mixed pitch; (2) placing the mixed asphalt in an inert gas atmosphere, heating for 6-9 h at 400-420 ℃, and then cooling to room temperature to obtain carbonized asphalt; (3) extracting and separating the carbonized asphalt to obtain carbon microspheres; (4) and (3) washing and drying the carbon microspheres, and then heating and carbonizing the carbon microspheres in stages in an inert gas atmosphere to obtain the carbon microspheres. The method for preparing the mesophase pitch by using the biomass tar mixed coal tar pitch effectively improves the yield of the mesophase carbon microspheres and realizes the effective utilization of the biomass tar.
Description
Technical Field
The invention belongs to the technical field of coking, and particularly relates to a mesophase carbon microsphere and a preparation method thereof.
Background
The mesocarbon microbeads are the intermediate-temp liquid-phase thermolysis product of polycyclic aromatic hydrocarbon. It can be prepared from coal or petroleum derived pitches, naphthalene isotropic pitches, heavy oils, and coal tar. Mesocarbon microbeads have been extensively studied as precursors for the preparation of carbon fibers, foams and other advanced functional materials. In recent years, more research has been focused on the use of mesocarbon microbeads as electrode materials, such as lithium ion secondary batteries and sodium ion batteries.
The preparation method of the mesocarbon microbeads mainly comprises a thermal polycondensation method, an emulsification method, a suspension method and other preparation methods. Compared with the emulsification method and the suspension method, the thermal polycondensation method has the advantages of simple process, easy control of preparation conditions, easy realization of continuous production and the like, and is widely adopted by carbon microsphere production enterprises at present. However, the polycondensation method generally has the defects of wide diameter distribution of mesophase carbon microspheres, low yield, high cost and the like.
Disclosure of Invention
Aiming at the prior art, the invention provides a mesophase carbon microsphere and a preparation method thereof, aiming at solving the problem of low yield of the existing preparation method.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation method of the mesocarbon microbeads is provided and comprises the following steps:
(1) after centrifugal filtration, mixing the biomass tar with coal tar pitch according to the mass ratio of 0.1-0.2: 1 to obtain mixed pitch;
(2) placing the mixed asphalt in an inert gas atmosphere, heating for 6-9 h at 400-420 ℃, and then cooling to room temperature to obtain carbonized asphalt;
(3) extracting and separating the carbonized asphalt to obtain carbon microspheres;
(4) and (3) washing and drying the carbon microspheres, and then heating and carbonizing the carbon microspheres in stages in an inert gas atmosphere to obtain the carbon microspheres.
According to the invention, the biomass tar is mixed with the coal tar pitch, the composition and the structure of the coal tar pitch are adjusted, the defect of low hydrogen content in the medium-temperature coal tar pitch is overcome, and meanwhile, a naphthenic structure can be introduced. Under the condition of high-temperature co-carbonization, the system viscosity of the mesophase pitch is reduced, and the dispersion and formation of the mesophase carbon microspheres in a reaction system are facilitated; the medium-temperature coal tar pitch and biomass tar co-carbonization also provide more nucleation areas of the mesophase carbon microspheres, so that the yield of the mesophase carbon microspheres can be effectively improved, and is increased from 15-20% to 30-40% in the traditional method.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the centrifugation is carried out for 30min at 4000-4300 r/min.
Further, the filtration was performed with 200 mesh filter cloth.
Further, the extraction and separation of the carbonized asphalt in the step (3) comprises the following steps: mixing the carbonized asphalt and the quinoline solvent, stirring for 1h at 150 ℃, centrifuging, standing for layering, taking the solute of the lower layer, performing suction filtration and washing, and drying to obtain the finished product.
Further, the washing was conducted by sequentially washing with quinoline, toluene and acetone.
Further, the washing in the step (4) is washing with toluene.
Further, the drying in the step (4) is drying for 2 hours at 120 ℃.
Further, the staged heating includes the steps of: the mixture was heated from ambient temperature to 300 ℃ at a heating rate of 5 ℃/min, then to 720 ℃ at a heating rate of 1 ℃/min, then to 1100 ℃ at a heating rate of 5 ℃/min, and then to 1100 ℃ for 1 h.
The invention also provides the mesocarbon microbeads prepared by the preparation method.
The invention has the beneficial effects that:
1. the mesophase pitch is prepared by mixing the biomass tar with the coal tar pitch, the biomass tar is residue obtained by pyrolyzing biomass materials at high temperature, the biomass materials comprise tree sawdust, crop straws and the like, and the mesophase pitch has the advantages of being renewable, low in cost, low in nitrogen, low in sulfur, sufficient in global supply and the like.
2. The yield of the mesocarbon microbeads is effectively improved and is improved to 30-40% from 15-20% in the traditional method.
3. Compared with the mesocarbon microbeads prepared from coal tar pitch, the mesocarbon microbeads prepared by the method have larger interlayer spacing and more defect points.
Drawings
FIG. 1 shows polarization micrographs of carbonized asphalts in examples 1 to 3 of the present invention and comparative example 1 (wherein a: PB-0, b: PB-10, c: PB-15, and d: PB-20).
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention.
Example 1
The preparation method of the mesocarbon microbeads MCMB-10 comprises the following steps:
(1) placing the biomass tar in a centrifugal filter, centrifuging for 30min at 4100r/min, wherein the filter cloth is 200-mesh filter cloth, and mixing the filtered biomass tar with coal tar pitch according to the mass ratio of 0.1:1 to obtain mixed pitch;
(2) placing the mixed asphalt in a pressurized reaction kettle, filling nitrogen for purging, heating to 300 ℃ from room temperature at the heating rate of 5 ℃/min in the nitrogen atmosphere, heating to 410 ℃ at the heating rate of 1 ℃/min, carrying out carbonization thermal polycondensation at 410 ℃ for 7h, and naturally cooling to room temperature to obtain carbonized asphalt PB-10;
(3) placing carbonized asphalt PB-10 and a quinoline solvent in a high-temperature reaction kettle, heating to 150 ℃ in a sealed manner, stirring for 1h at 150 ℃, centrifuging, standing for layering, taking a lower-layer solute, performing suction filtration and washing on the lower-layer solute by using quinoline, toluene and acetone, and drying to obtain carbon microspheres;
(4) washing the carbon microspheres with toluene, then placing the carbon microspheres into a vacuum drying oven to be dried for 2h at 120 ℃, then placing the carbon microspheres into a tube furnace, heating the carbon microspheres to 300 ℃ from the ambient temperature at a heating rate of 5 ℃/min in the first stage, heating the carbon microspheres to 720 ℃ at a heating rate of 1 ℃/min in the second stage, heating the carbon microspheres to 1100 ℃ at a heating rate of 5 ℃/min in the third stage, then heating the carbon microspheres for 1h at 1100 ℃, and cooling the carbon microspheres to room temperature to obtain the mesocarbon microspheres MCMB-10.
Example 2
The preparation method of the mesocarbon microbeads MCMB-15 comprises the following steps:
(1) placing the biomass tar in a centrifugal filter, centrifuging for 30min at 4000r/min, wherein the filter cloth is 200-mesh filter cloth, and mixing the filtered biomass tar with coal tar pitch according to the mass ratio of 0.15:1 to obtain mixed pitch;
(2) placing the mixed asphalt in a pressurized reaction kettle, filling nitrogen for purging, heating to 300 ℃ from room temperature at the heating rate of 5 ℃/min in the nitrogen atmosphere, heating to 420 ℃ at the heating rate of 1 ℃/min, performing copolycarbonate thermal polycondensation at 420 ℃ for 6h, and naturally cooling to room temperature to obtain carbonized asphalt PB-15;
(3) placing carbonized asphalt PB-15 and a quinoline solvent in a high-temperature reaction kettle, heating to 150 ℃ in a sealed manner, stirring for 1h at 150 ℃, centrifuging, standing for layering, taking a lower-layer solute, performing suction filtration and washing on the lower-layer solute by using quinoline, toluene and acetone, and drying to obtain carbon microspheres;
(4) washing the carbon microspheres with toluene, then placing the carbon microspheres into a vacuum drying oven to be dried for 2h at 120 ℃, then placing the carbon microspheres into a tube furnace, heating the carbon microspheres to 300 ℃ from the ambient temperature at a heating rate of 5 ℃/min in the first stage, heating the carbon microspheres to 720 ℃ at a heating rate of 1 ℃/min in the second stage, heating the carbon microspheres to 1100 ℃ at a heating rate of 5 ℃/min in the third stage, then heating the carbon microspheres for 1h at 1100 ℃, and cooling the carbon microspheres to room temperature to obtain the mesocarbon microspheres MCMB-15.
Example 3
The preparation method of the mesocarbon microbeads MCMB-20 comprises the following steps:
(1) placing the biomass tar in a centrifugal filter, centrifuging for 30min at 4300r/min, wherein the filter cloth is 200-mesh filter cloth, and mixing the filtered biomass tar with coal tar pitch according to the mass ratio of 0.2:1 to obtain mixed pitch;
(2) placing the mixed asphalt in a pressurized reaction kettle, filling nitrogen for purging, heating to 300 ℃ from room temperature at the heating rate of 5 ℃/min in the nitrogen atmosphere, heating to 400 ℃ at the heating rate of 1 ℃/min, carrying out carbonization thermal polycondensation at 400 ℃ for 9h, and naturally cooling to room temperature to obtain carbonized asphalt PB-20;
(3) placing carbonized asphalt PB-20 and a quinoline solvent in a high-temperature reaction kettle, heating to 150 ℃ in a sealed manner, stirring for 1h at 150 ℃, centrifuging, standing for layering, taking a lower-layer solute, performing suction filtration and washing on the lower-layer solute by using quinoline, toluene and acetone, and drying to obtain carbon microspheres;
(4) washing the carbon microspheres with toluene, then placing the carbon microspheres into a vacuum drying oven to be dried for 2h at 120 ℃, then placing the carbon microspheres into a tube furnace, heating the carbon microspheres to 300 ℃ from the ambient temperature at a heating rate of 5 ℃/min in the first stage, heating the carbon microspheres to 720 ℃ at a heating rate of 1 ℃/min in the second stage, heating the carbon microspheres to 1100 ℃ at a heating rate of 5 ℃/min in the third stage, then heating the carbon microspheres for 1h at 1100 ℃, and cooling the carbon microspheres to room temperature to obtain the mesocarbon microspheres MCMB-20.
Comparative example 1
The preparation method of the mesocarbon microbeads MCMB-0 comprises the following steps:
(1) putting coal tar pitch into a pressurized reaction kettle, introducing nitrogen for purging, heating to 300 ℃ from room temperature at the heating rate of 5 ℃/min in the nitrogen atmosphere, heating to 410 ℃ at the heating rate of 1 ℃/min, reacting at 410 ℃ for 7h, and naturally cooling to room temperature to obtain carbonized pitch PB-0;
(2) separating the carbon microspheres from the carbonized asphalt PB-0 by Soxhlet extraction with a quinoline solvent to obtain carbon microspheres;
(3) washing the carbon microspheres with toluene, then placing the carbon microspheres into a vacuum drying oven to be dried for 2h at 120 ℃, then placing the carbon microspheres into a tube furnace, heating the carbon microspheres to 300 ℃ from the ambient temperature at a heating rate of 5 ℃/min in the first stage, heating the carbon microspheres to 720 ℃ at a heating rate of 1 ℃/min in the second stage, heating the carbon microspheres to 1100 ℃ at a heating rate of 5 ℃/min in the third stage, then heating the carbon microspheres for 1h at 1100 ℃, and cooling the carbon microspheres to room temperature to obtain the mesocarbon microspheres MCMB-0.
Then, the optical structure of the mesophase carbon microspheres in the mother liquor pitch in examples 1 to 3 and comparative example 1 was observed with a polarization microscope, the particle size distribution and the average particle size of the carbon microspheres were analyzed with a laser particle size analyzer, the crystallite structure of the carbon microspheres was analyzed with X-ray diffraction, and the defects and the disorder degree of the carbon microspheres were analyzed with raman spectroscopy. The results are shown in fig. 1, table 1, and table 2.
TABLE 1 yield and particle size of mesophase carbon microbeads
As can be seen from Table 1, the mean particle size of the Mesophase Carbon Microbeads (MCMB) decreases as the pitch content of the biomass in the co-carbonized pitch decreases. The biomass asphalt added to the MCMB-0, MCMB-10, MCMB-15 and MCMB-20 is 0%, 10%, 15% and 20% in sequence, and the average particle diameters are 22.18 μm, 18.24 μm, 12.31 μm and 10.14 μm respectively. It can be seen from table 1 that, as the content of the biomass pitch increases, the yield thereof increases, and the yield of the mesophase carbon microspheres added with the biomass pitch mass ratio of 15% is the highest, and is 42.8 wt%.
TABLE 2 calculation of XRD Spectroscopy microstructure and calculation of degree of disorder of Raman Spectroscopy of MCMBs
As can be seen from Table 2, the interlayer spacing (d)002) Increases with increasing biomass pitch ratio. The interlayer distance of the mesocarbon microbeads prepared from the coal tar pitch is 0.3323nm, and the interlayer distances of the mesocarbon microbeads prepared from the biomass pitches with 10%, 15% and 20% of added substances are 0.3458nm, 0.3485nm and 0.3516nm respectively. Relative intensity I of D peak and G peak in Raman spectrum data analysisD/IGCan reflect the degree of carbon disordered structure in the carbon material. Mesophase carbon microsphere prepared from coal tar pitch ID/IG0.21, added with 10%, 15% and 20% of mesophase carbon microspheres prepared from biomass pitchD/IGRespectively 2.63, 2.67 and 3.29. Compared with the mesocarbon microbeads prepared from the coal tar pitch, the prepared mesocarbon microbeads have larger interlayer spacing and more defect points.
While the present invention has been described in detail with reference to the embodiments, it should not be construed as limited to the scope of the patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (9)
1. The preparation method of the mesocarbon microbeads is characterized by comprising the following steps:
(1) after centrifugal filtration, mixing the biomass tar with coal tar pitch according to the mass ratio of 0.1-0.2: 1 to obtain mixed pitch;
(2) placing the mixed asphalt in an inert gas atmosphere, heating for 6-9 h at 400-420 ℃, and then cooling to room temperature to obtain carbonized asphalt;
(3) extracting and separating the carbonized asphalt to obtain carbon microspheres;
(4) and (3) washing and drying the carbon microspheres, and then heating and carbonizing the carbon microspheres in stages in an inert gas atmosphere to obtain the carbon microspheres.
2. The method of claim 1, wherein: the centrifugation is carried out for 30min at 4000-4300 r/min.
3. The method of claim 1, wherein: the filtration is performed by using 200-mesh filter cloth.
4. The preparation method according to claim 1, wherein the extraction and separation of the carbonized pitch in the step (3) comprises the steps of: mixing the carbonized asphalt and the quinoline solvent, stirring for 1h at 150 ℃, centrifuging, standing for layering, taking the solute of the lower layer, performing suction filtration and washing, and drying to obtain the finished product.
5. The method of claim 4, wherein: the washing is sequentially washing with quinoline, toluene and acetone.
6. The method of claim 1, wherein: the washing in the step (4) is washing with toluene.
7. The method of claim 1, wherein: in the step (4), the drying is carried out for 2 hours at the temperature of 120 ℃.
8. The method of claim 1, wherein the staged heating comprises the steps of: the mixture was heated from ambient temperature to 300 ℃ at a heating rate of 5 ℃/min, then to 720 ℃ at a heating rate of 1 ℃/min, then to 1100 ℃ at a heating rate of 5 ℃/min, and then to 1100 ℃ for 1 h.
9. Mesophase carbon microspheres produced by the production method according to any one of claims 1 to 8.
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CN112812801A (en) * | 2021-01-13 | 2021-05-18 | 中国石油大学(华东) | Preparation process of mesophase pitch and pitch-based carbon fiber |
CN113636538A (en) * | 2021-09-18 | 2021-11-12 | 中国矿业大学(北京) | Mesocarbon microbeads and preparation method thereof |
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CN108840331A (en) * | 2018-07-03 | 2018-11-20 | 贵州格瑞特新材料有限公司 | A kind of high interlamellar spacing artificial graphite material and preparation method thereof |
CN112645304A (en) * | 2021-01-13 | 2021-04-13 | 中国石油大学(华东) | Method for preparing high-performance mesocarbon microbeads from heavy oil |
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Non-Patent Citations (1)
Title |
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LEI LI ET AL.: ""Preparation of mesocarbon microbeads from coal tar pitch with blending of biomass tar pitch"", 《JOURNAL OF ANALYTICAL AND APPLIED PYROLYSIS》 * |
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