CN105905883A - Mesocarbon microbead and preparation method thereof - Google Patents
Mesocarbon microbead and preparation method thereof Download PDFInfo
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- CN105905883A CN105905883A CN201610237690.1A CN201610237690A CN105905883A CN 105905883 A CN105905883 A CN 105905883A CN 201610237690 A CN201610237690 A CN 201610237690A CN 105905883 A CN105905883 A CN 105905883A
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- 239000002931 mesocarbon microbead Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000003245 coal Substances 0.000 claims abstract description 57
- 239000000295 fuel oil Substances 0.000 claims abstract description 42
- 238000005406 washing Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000010426 asphalt Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 230000006911 nucleation Effects 0.000 claims abstract description 13
- 238000010899 nucleation Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 7
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 22
- 239000003921 oil Substances 0.000 claims description 14
- 239000011302 mesophase pitch Substances 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000003599 detergent Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 208000035985 Body Odor Diseases 0.000 claims 1
- 206010055000 Bromhidrosis Diseases 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000011325 microbead Substances 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000004005 microsphere Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000007600 charging Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 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
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Working-Up Tar And Pitch (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a mesocarbon microbead and its preparation method. The method comprises the following steps: S1, heating coal liquefied asphalt; S2, distilling the heated coal liquefied asphalt to obtain liquefied heavy oil and an asphalt substance; S3, adding a nucleation promoter into the liquefied heavy oil and reacting to obtain a mixture containing mesophase microbeads; and S4, washing the mixture with a washing agent, filtering and drying to obtain the mesocarbon microbeads. The whole technological process is simple and has strong operability and good economy. By using coal to directly liquefy liquefied heavy oil in residue for preparation of the mesocarbon microbeads, it is beneficial to formation of the mesocarbon microbeads with uniform size and good degree of sphericity. Meanwhile, the application range of coal liquefied residue is broadened, and waste of residue resources is avoided. The invention is of great practical significance for boosting general economical benefits of a coal liquefaction plant.
Description
Technical field
The present invention relates to coal deep processing field, in particular to a kind of MCMB and preparation method thereof.
Background technology
Coal liquefaction residue be the outward appearance under a kind of high charcoal, high ash and the material of high-sulfur, room temperature be solid asphalt shape, softening point should be
About 190 DEG C, solid content about 50%.Liquefied heavy oil content about about 20% in coal liquefaction residue, this part heavy coal liquids is not
Can be only used for back adapted and do DCL/Direct coal liquefaction circulating solvent, be also highly suitable for as the raw material preparing carbon material.Intermediate-phase carbon
Microsphere is a kind of novel charcoal material approximating graphite-structure, the layer structure having uniqueness due to it and ball nature, thus at lithium
Ion battery cathode material, prepare the aspects such as high-specific surface area ball shape active carbon and obtained fine application.
The patent that relevant coal liquefaction residue prepares MCMB is less, and Chinese patent CN102225755A discloses a kind of base
It is the method that MCMB prepared by raw material in coal liquefaction residue.But this patent uses the heavy liquid in coal liquefaction residue
Carburetion is the MCMB that raw material prepares with the mixture of bitumen.And, the molecular weight distribution of this mixture
Wider range, the partial reaction activity high in course of reaction middle-molecular-weihydroxyethyl is the highest, can be converted into mesophase in relatively low temperature,
And molecular weight low long period of reaction at relatively high temperatures also is difficult to be converted into mesophase, cause preparing MCMB
During, hardly result in size than more uniform MCMB.
Summary of the invention
It is desirable to provide a kind of MCMB and preparation method thereof, to provide in a kind of size uniformity and good sphericity
Between phase carbon microspheres.
To achieve these goals, according to an aspect of the invention, it is provided the preparation method of a kind of MCMB.Should
Method comprises the following steps: S1, is heated by coal liquefaction Colophonium；S2, distills the coal liquefaction Colophonium after heating, obtains liquid
Change heavy oil and bitumen；S3, adds nucleation accelerating agent in liquefaction heavy oil, obtains the mixing containing mesophase ball after reaction
Thing；S4, uses detergent to wash in mixture, through filtering, obtaining MCMB after drying.
Further, S1 specifically includes: coal liquefaction asphalt powder is broken to particle diameter ＜ 3mm, is then added in heating tank be heated to
300～320 DEG C.
Further, S2 specifically includes: will heating after coal liquefaction Colophonium join in membrane evaporator, 300～370 DEG C,
Distill under the conditions of negative pressure of vacuum 10～20Pa, obtain liquefy heavy oil and bitumen.
Further, the softening point < 110 DEG C of liquefaction heavy oil.
Further, S3 specifically includes: add liquefied heavy oil quality 5～the nucleation accelerating agent of 10% in liquefaction heavy oil, with
10～15 DEG C of heating rates, from room temperature to 300 DEG C, stop 120min and are sufficiently mixed uniformly, then with 7～10 DEG C of heating rates
Being warming up to 420～460 DEG C, at inert gas atmosphere, stir speed (S.S.) is 200～600r/min and pressure is normal pressure or certainly rises pressure,
Constant temperature 4～10h.
Further, nucleation accelerating agent is prepared by following steps: 1) be mixed and stirred for extractant by coal liquefaction residue,
Extract, be centrifugally separating to obtain extract；2) extract is carried out normal pressure or decompression distillation, is extracted refined thing；3)
By extracting and refining thing under 400 DEG C～450 DEG C, inert gas atmosphere and 0.1～3.0MPa, constant voltage constant temperature 5～16h occurs
Polyreaction, obtains mesophase pitch；4) < 1 micron obtains nucleation accelerating agent mesophase pitch to be crushed to granularity.
Further, S4 specifically includes: the mixture obtained by S3 is 200～300 DEG C in temperature and carries out once washing, filters
After, filtering residue is carried out secondary washing again, obtains MCMB after drying.
Further, once washing agent be boiling range scope be 300～400 DEG C normal one line oil, first vacuum side stream or stabilized hydrogenation oil.
Further, the detergent of secondary washing be boiling range be < the coal liquefaction light oil of 110 DEG C.
According to a further aspect in the invention, it is provided that a kind of MCMB.This MCMB uses any of the above-described kind of system
Preparation Method prepares.
The liquefaction heavy oil obtained by the inventive method is by coal liquefaction Colophonium (bitumen and the mixture of liquefaction heavy oil) warp
Crossing what distillation obtained, whole technical process is simple, workable, has good economy.Additionally, utilize the direct liquid of coal
Liquefaction heavy oil in change residue is prepared MCMB and is advantageously formed the MCMB of size uniformity and good sphericity, with
The Shi Tuokuan application of coal liquefaction residue, it is to avoid the waste of residue resource, to the whole economic efficiency improving coal liquefaction plant
There is very important realistic meaning.
Accompanying drawing explanation
The Figure of description of the part constituting the application is used for providing a further understanding of the present invention, and the present invention's is schematic real
Execute example and illustrate for explaining the present invention, being not intended that inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 shows the polarizing microscope picture of the MCMB that the embodiment of the present invention 1 obtains；
Fig. 2 shows the polarizing microscope picture of the MCMB that the embodiment of the present invention 2 obtains；
Fig. 3 shows the polarizing microscope picture of the MCMB that the embodiment of the present invention 3 obtains；
Fig. 4 shows the polarizing microscope picture of the MCMB that comparative example 1 obtains；
Fig. 5 shows the SEM figure of the MCMB that embodiment 1 obtains；And
Fig. 6 shows the SEM figure of the MCMB that comparative example 1 obtains.
Detailed description of the invention
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can be mutually combined.
Describe the present invention below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
According to a kind of typical embodiment of the present invention, it is provided that the preparation method of a kind of MCMB.This preparation method includes
Following steps: S1, heats coal liquefaction Colophonium；S2, will heating after coal liquefaction Colophonium distill, obtain liquefy heavy oil and
Bitumen；S3, adds nucleation accelerating agent in liquefaction heavy oil, obtains the mixture containing mesophase ball after reaction；S4,
Detergent is used to wash in mixture, through filtering, obtaining MCMB after drying.
Wherein, coal liquefaction Colophonium is the mixture of bitumen and liquefaction heavy oil.Such as, China's Firing Shenhua Coal liquefaction chemical industry is limited
The graduate coal liquefaction in company Shanghai Colophonium (bitumen and the mixture of liquefaction heavy oil), the softening point one of this coal liquefaction Colophonium
As at 120～160 DEG C.
Coal liquefaction Colophonium is obtained by the liquefaction heavy oil obtained by the inventive method through distillation, and whole technical process is simple,
Workable, there is good economy.Additionally, it is micro-to utilize the liquefaction heavy oil in coal directly-liquefied residue to prepare intermediate-phase carbon
Ball advantageously forms the MCMB of size uniformity and good sphericity, has widened the application of coal liquefaction residue simultaneously, has kept away
Exempt from the waste of residue resource, the whole economic efficiency improving coal liquefaction plant has been had very important realistic meaning.
Preferably, S1 specifically includes: coal liquefaction asphalt powder is broken to particle diameter ＜ 3mm, is then added in heating tank be heated to
300-320℃.Wherein, coal liquefaction asphalt powder is broken to particle diameter ＜ 3mm both convenient chargings, Colophonium can be made soft in relatively short period of time again
Change melted.
Preferably, S2 specifically includes: join in membrane evaporator by the coal liquefaction Colophonium after heating, 300～370 DEG C, true
Distill under the conditions of idling pressure 10～20Pa, obtain liquefy heavy oil and bitumen.Technical process is simple, workable,
There is good economy.The softening point < 110 DEG C of liquefaction heavy oil.
Preferably, S3 specifically includes: add liquefied heavy oil quality 5～the nucleation accelerating agent of 10%, with 10～15 DEG C in liquefaction heavy oil
Heating rate, from room temperature to 300 DEG C, stops 120min and is sufficiently mixed uniformly, be then warming up to 7～10 DEG C of heating rates
420～460 DEG C, at inert gas atmosphere, stir speed (S.S.) is 200～600r/min and pressure is normal pressure or certainly rises pressure, constant temperature 4～
10h.It is basically unchanged in view of liquefied heavy oil chemical property before 300 DEG C, for saving the time, uses the mode being rapidly heated.And work as
When temperature is higher than 300 DEG C, liquefaction heavy oil starts to occur thermal decomposition and heat polymerization, but mitigation is compared in reaction, can use very fast
Speed, but the speed lower than before 300 DEG C heats up.
According to a kind of typical embodiment of the present invention, nucleation accelerating agent is prepared by following steps: 1) by coal liquefaction residue
It is mixed and stirred for extractant, extracts, be centrifugally separating to obtain extract；2) extract is carried out normal pressure or decompression distillation,
It is extracted refined thing；3) by extracting and refining thing under 400 DEG C～450 DEG C, inert gas atmosphere and 0.1～3.0MPa, permanent
There is polyreaction in pressure constant temperature 5～16h, obtains mesophase pitch；4) < 1 micron is become mesophase pitch to be crushed to granularity
Core accelerator.According to a kind of typical embodiment of the present invention, the preparation of nucleation accelerating agent can be found in patent 201310153232.6
The mesophase pitch prepared.
Preferably, S4 specifically includes: the mixture obtained by S3 is 200～300 DEG C in temperature and carries out once washing, after filtration,
Filtering residue is the most repeatedly washed, obtains MCMB after drying.The purpose of once washing is in order in higher temperature
Lower by the Colophonium wash clean on MCMB surface, and repeatedly washing is to remain in MCMB by after once washing
The solvent on surface is thoroughly washed off.
Preferably, once washing agent be boiling range scope be 300～400 DEG C normal one line oil, first vacuum side stream or stabilized hydrogenation oil.Phase
Extractant for other has detersive efficiency height, is easily recycled advantage.
Preferably, the detergent repeatedly washed be boiling range be < the coal liquefaction light oil of 110 DEG C.The light oil using this boiling range is because many
Even if MCMB surface residual fraction light oil after secondary washing, but can volatilize owing to its boiling range is relatively low easily or evaporate
Fall.
According to a kind of typical embodiment of the present invention, it is provided that a kind of MCMB.This MCMB uses above-mentioned system
Preparation Method prepares.
Beneficial effects of the present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
20kg granularity is joined in heating tank less than the coal liquefaction Colophonium of 3 millimeters and adds heat fusing in 300 DEG C, will former after heating
Material joins in membrane evaporator, 300 DEG C, distill under the conditions of negative pressure of vacuum 10Pa, after distillation 4h, respectively obtain liquid
Change heavy oil and bitumen.Add in liquefaction heavy oil and account for liquefied heavy oil quality 5% mesophase pitch (< 1 micron), with 15 DEG C
/ min, from room temperature to 300 DEG C, stops 120min and is sufficiently mixed uniformly, be then warming up to 420 DEG C with 7 DEG C/min, at nitrogen
Gas atmosphere, stir speed (S.S.) is 200r/min, and pressure is under normal pressure, constant temperature 10h；
The mixture above-mentioned condition obtained uses two wires, 300～400 DEG C of normal sides oil to carry out once washing, uses after filtering, separating
< liquefied coal coil of 110 degree carries out secondary washing, through filtering, separate, being dried to obtain MCMB.
Embodiment 2
20kg granularity is joined in heating tank less than the coal liquefaction Colophonium of 3 millimeters and adds heat fusing in 320 DEG C, will former after heating
Material joins in membrane evaporator, 320 DEG C, distill under the conditions of negative pressure of vacuum 20Pa, after distillation 6h, respectively obtain liquid
Change heavy oil and bitumen.Add in liquefaction heavy oil and account for liquefied heavy oil quality 10% mesophase pitch, with 10 DEG C/min from room
Temperature is warming up to 300 DEG C, stops 120min and is sufficiently mixed uniformly, is then warming up to 460 DEG C with 10 DEG C/min, at nitrogen atmosphere, stirs
Mixing speed is 600r/min, and pressure is under normal pressure, constant temperature 4h；
The mixture above-mentioned condition obtained uses 300～400 DEG C of first vacuum side streams to carry out once washing, with < 110 after filtering, separating
The liquefied coal coil of degree carries out secondary washing, through filtering, separate, being dried to obtain MCMB.
Embodiment 3
20kg granularity is joined in heating tank less than the coal liquefaction Colophonium of 3 millimeters and adds heat fusing in 300 DEG C, will former after heating
Material joins in membrane evaporator, 350 DEG C, distill under the conditions of negative pressure of vacuum 15Pa, after distillation 5h, respectively obtain liquid
Change heavy oil and bitumen.Add in liquefaction heavy oil and account for liquefied heavy oil quality 8% mesophase pitch, with 12 DEG C/min from room temperature
It is warming up to 300 DEG C, stops 120min and be sufficiently mixed uniformly, be then warming up to 440 DEG C with 9 DEG C/min, in nitrogen atmosphere, stirring
Speed is 400r/min, and pressure is under normal pressure, constant temperature 6h；
The mixture above-mentioned condition obtained uses 300～400 DEG C of stabilized hydrogenation side line oil to carry out once washing, through filtering, separating
Afterwards with < liquefied coal coil of 110 degree carries out secondary washing, through filtering, separate, being dried to obtain MCMB.
The polarizing microscope picture of the MCMB that embodiment 1-3 obtains the most as Figure 1-3, can be seen that from picture
MCMB size uniformity, good sphericity, SEM (scanning electron microscope) figure of embodiment 1 as it is shown in figure 5, from
Can be seen that in picture that the particle size distribution ratio of MCMB is more uniform, the comparison of surface washing is clean.
Comparative example 1
With coal liquefaction Colophonium as raw material, with 15 DEG C/min from room temperature to 300 DEG C, stop 120min and be sufficiently mixed uniformly, so
After be warming up to 420 DEG C with 7 DEG C/min, at nitrogen atmosphere, stir speed (S.S.) is 200r/min, and pressure is under normal pressure, constant temperature 10h；
The mixture above-mentioned condition obtained uses 300～400 DEG C of normal line oil to carry out once washing, uses after filtering, separating
< liquefied coal coil of 110 DEG C carries out secondary washing, through filtering, separate, being dried to obtain MCMB.
The polarizing microscope figure of the MCMB that comparative example 1 obtains as shown in Figure 4, can be seen that intermediate-phase carbon from picture
Microsphere Size heterogeneity, the SEM of comparative example 1 schemes as shown in Figure 6, can be seen that the particle diameter of MCMB divides from picture
Cloth is wider, and after washing, mesophase ball adhesion is more, and has some beads to split.
As can be seen from the above description, the above embodiments of the present invention achieve following technique effect:
Utilize the preparation method that the present invention provides, with coal liquefaction Colophonium as raw material, carried out membrane distillation, molecule can be obtained
The liquefaction heavy oil that amount distribution is narrower.Prepare MCMB with this liquefaction heavy oil, advantageously form size uniformity and spherical
The MCMB spent.This coal liquefaction Colophonium is as the solvent extraction product of coal liquefaction residue, it is possible to prepare better performances
MCMB, for widening the application of coal liquefaction residue, avoiding the waste of resource, the entirety warp of raising coal liquefaction plant
Ji benefit has important practical significance.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for those skilled in the art
For, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any amendment of being made, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. the preparation method of a MCMB, it is characterised in that comprise the following steps:
S1, heats coal liquefaction Colophonium；
S2, distills the described coal liquefaction Colophonium after heating, obtains liquefy heavy oil and bitumen；
S3, adds nucleation accelerating agent in described liquefaction heavy oil, obtains the mixture containing mesophase ball after reaction；
S4, washs described mixture employing detergent, through filtering, obtaining described MCMB after drying.
Preparation method the most according to claim 1, it is characterised in that described S1 specifically includes: by described coal liquefaction asphalt powder
It is broken to particle diameter ＜ 3mm, is then added in heating tank be heated to 300～320 DEG C.
Preparation method the most according to claim 1, it is characterised in that described S2 specifically includes: by the described coal liquid after heating
Change Colophonium and join in membrane evaporator, 300～370 DEG C, distill under the conditions of negative pressure of vacuum 10～20Pa, obtain
Described liquefaction heavy oil and described bitumen.
Preparation method the most according to claim 3, it is characterised in that the softening point of described liquefaction heavy oil < 110 DEG C.
Preparation method the most according to claim 1, it is characterised in that described S3 specifically includes: add in described liquefaction heavy oil
Enter described liquefied heavy oil quality 5～the nucleation accelerating agent of 10%, with 10～15 DEG C of heating rates from room temperature to 300 DEG C,
Stop 120min and be sufficiently mixed uniformly, be then warming up to 420～460 DEG C with 7～10 DEG C of heating rates, at indifferent gas bromhidrosis
Atmosphere, stir speed (S.S.) is 200～600r/min and pressure is normal pressure or certainly rises pressure, constant temperature 4～10h.
Preparation method the most according to claim 5, it is characterised in that described nucleation accelerating agent is prepared by following steps:
1) coal liquefaction residue is mixed and stirred for extractant, extracts, be centrifugally separating to obtain extract；
2) described extract is carried out normal pressure or decompression distillation, is extracted refined thing；
3) by described extracting and refining thing under 400 DEG C～450 DEG C, inert gas atmosphere and 0.1～3.0MPa, constant pressure and constant
There is polyreaction in temperature 5～16h, obtains mesophase pitch；
4) < 1 micron obtains described nucleation accelerating agent described mesophase pitch to be crushed to granularity.
Preparation method the most according to claim 1, it is characterised in that described S4 specifically includes: the institute that described S3 is obtained
State mixture to be 200～300 DEG C in temperature and carry out once washing, after filtration, filtering residue is carried out secondary washing, drying again
After obtain described MCMB.
Preparation method the most according to claim 7, it is characterised in that described once washing agent be boiling range scope be 300～400 DEG C
Normal one line oil, first vacuum side stream or stabilized hydrogenation oil.
Preparation method the most according to claim 7, it is characterised in that the detergent of described secondary washing be boiling range be < 110 DEG C
Coal liquefaction light oil.
10. a MCMB, it is characterised in that use as in claim 1 to 9, any one preparation method prepares.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610237690.1A CN105905883A (en) | 2016-04-15 | 2016-04-15 | Mesocarbon microbead and preparation method thereof |
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| CN201610237690.1A CN105905883A (en) | 2016-04-15 | 2016-04-15 | Mesocarbon microbead and preparation method thereof |
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| CN201610237690.1A Pending CN105905883A (en) | 2016-04-15 | 2016-04-15 | Mesocarbon microbead and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108455558A (en) * | 2018-03-27 | 2018-08-28 | 中国科学院过程工程研究所 | A kind of preparation method of novel mesocarbon microspheres |
| CN113667506A (en) * | 2020-05-15 | 2021-11-19 | 中国石油化工股份有限公司 | Preparation method and preparation system of mesophase pitch |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005050819A (en) * | 2004-08-04 | 2005-02-24 | Osaka Gas Co Ltd | Meso carbon micro beads |
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