CN107934934A - A kind of method for efficiently preparing asphalt base mesocarbon microspheres - Google Patents
A kind of method for efficiently preparing asphalt base mesocarbon microspheres Download PDFInfo
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- CN107934934A CN107934934A CN201810025992.1A CN201810025992A CN107934934A CN 107934934 A CN107934934 A CN 107934934A CN 201810025992 A CN201810025992 A CN 201810025992A CN 107934934 A CN107934934 A CN 107934934A
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- mesocarbon microspheres
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Abstract
The invention discloses a kind of method for efficiently preparing asphalt base mesocarbon microspheres.First in certain temperature, N2Asphalt and additive are sufficiently mixed under flow and mixing speed and the pre-heat treatment, the micromolecular compound for being difficult to polymerize with removing；Afterwards in N2Under the conditions of protection, 0.5~2.0MPa of pressure, 380~420 DEG C of temperature, 2~6h of constant temperature carries out heat polymerization, obtains the polymerbitumen containing mesocarbon microspheres；Thermosol, filtering are further carried out to polymerbitumen with the washing oil of 245~290 DEG C of boiling range, after filter cake is extracted through organic solvents such as pyridine, toluene, vacuum drying, that is, obtain asphalt base mesocarbon microspheres.Asphalt used in the present invention and additive abundance and cost is relatively low, by the mass fraction for controlling additive, the mesocarbon microspheres that even particle size distribution, size are controllable, yield is of a relatively high can be prepared, lithium ion battery negative material can be used as after carbonization, graphitization.
Description
Technical field
The invention belongs to carbon material field, and in particular to a kind of to prepare mesocarbon microspheres by raw material of asphalt
Method.
Background technology
Mesocarbon microspheres (MCMB) is as a kind of new Carbon Materials, in 1973 first by Japanese scholars Yamada etc.
Separated from mesophase pitch, since it has unique lamellar structure and good physicochemical characteristic, become and prepare lithium
The first choice of ion battery cathode material, catalyst carrier, active carbon with high specific surface area material, performance liquid chromatographic column filler etc. is former
One of material.
At present, preparing the method for mesocarbon microspheres has thermal polycondensation process, suspension method, emulsion process, chemical vapour deposition technique etc..
Wherein using the mesocarbon microspheres that emulsion process or suspension method are prepared with spherical rounding is smooth, particle diameter distribution is controllable, yield
The advantages that high.But the technical process that mesocarbon microspheres is prepared using both approaches is cumbersome, and to the requirement of raw material
It is high, it is difficult to realize large-scale industrial production.Since thermal polycondensation process reaction process is easily controllable, and technique is simple, so mesh
Preceding industrial preparation mesocarbon microspheres is mainly based on thermal polycondensation process.
Patent CN1057319C " a kind of preparation method of mesocarbon microspheres ", first passes through the method removing coal tar of heat filtering
A pyridine insoluble obtains clean coal tar in oil, then coal tar is mixed according to a certain percentage with clean coal tar, aggregated point
From the mesocarbon microspheres for afterwards, obtaining uniform sphere diameter distribution." prepared by the copolycondensation of mesocarbon microspheres by patent CN1308113A
Method ", using medium temperature coal pitch and asphalt as raw material, uses copolycondensation method to prepare yield as 20~30% intermediate-phase carbon
Microballoon.Patent CN101920956A " a kind of method of highly-efficiently preparing asphalt-based mesocarbon microspheres ", with medium temperature coal pitch or height
Warm coal tar pitch is raw material, and rosin and disproportionated rosin are additive, and it is micro- to prepare the uniform intermediate-phase carbon of high income, particle diameter distribution
Ball.Patent CN102491307A " a kind of method of preparing mesocarbon microbeads by copolycondensation ", it is residual with coal tar asphalt and coal liquefaction
Slag carries out copolycondensation and prepares the mesocarbon microspheres that particle diameter distribution is relatively narrow, yield is 30%.Patent CN103274395A
" a kind of synthetic method of controllable grain size mesocarbon microspheres ", using coal tar pitch as raw material, graphite is the chemical combination such as additive, iron, cobalt
Thing goes out the mesocarbon microspheres of controllable grain size for catalyst preparation, but the subtractive process of catalyst is more complicated.Patent
CN103420358A " preparation method of mesocarbon microspheres ", by adding the additive of static electrification lotus in reactant, prepares
Go out that good sphericity, particle be big, the mesocarbon microspheres of high income.A kind of patent CN103833007A " coal tar pitch base intermediate-phase carbons
The preparation method of microballoon ", coal tar pitch raw material is re-mixed with itself the heavy phase pitch obtained by pretreatment, is obtained containing difference
The pitch of ratio quinoline insolubles, prepares the controllable mesocarbon microspheres of high income, granularity under appropriate conditions.Work at present
It is more using coal tar pitch as raw material that mesocarbon microspheres is prepared in industry, such as China Tianjin Bei Terui and China fir Taxodiaceae skill etc. are with coal tar pitch
Mesocarbon microspheres is prepared for raw material.And asphalt is since raw material quinoline insolubles itself is relatively low, prepared centre
Phase carbon microspheres yield is low, size distribution is uneven, industrially compares and is difficult to apply.Therefore, explore a kind of using asphalt as original
Material, particle diameter distribution is uniform, yield is of a relatively high, the simple mesocarbon microspheres preparation method of technical process is of great significance,
The application field of asphalt is widened.
For above present Research, the present invention is suitable by handling raw material preheating and adding using asphalt as raw material
Suitable additive carries out heat polymerization, can prepare the higher mesocarbon microspheres of controllable sphericity, epigranular, yield.
The content of the invention
The object of the present invention is to provide a kind of method for efficiently preparing asphalt base mesocarbon microspheres, at preheating
Manage some component characteristics of feed change or add additive, it is micro- to solve directly using asphalt to prepare intermediate-phase carbon at present
The problems such as yield is low during ball, size distribution is uneven, makes to prepare mesocarbon microspheres with good by raw material of asphalt
Commercial application prospect.
A kind of method for efficiently preparing asphalt base mesocarbon microspheres according to the present invention, is mainly arranged by following
Apply realization.
A kind of method for efficiently preparing asphalt base mesocarbon microspheres, mainly includes the following steps that：
(1) by asphalt and additive, high-temperature high-pressure reaction kettle is added to by additive mass fraction 0.5~10%
In.The toluene insolubles of the asphalt is 0.1%, and quinoline insolubles is less than 0.05%；Additive includes rosin or carbon black
One or two kinds of mixture in N110；
(2) by reaction kettle of the step (1) equipped with asphalt and additive agent mixture, heated up with the speed of 3~6 DEG C/min
To 250~300 DEG C, in N2Under the conditions of 40~80mL/min of flow, 100~200r/min of mechanical agitation speed, 1~2h of constant temperature into
Row the pre-heat treatment, obtain asphalt and additive is sufficiently mixed thing；
(3) be sufficiently mixed thing by what step (2) obtained asphalt and additive, 100~200r/min of stir speed (S.S.),
0.5~2.0MPa of pressure, 4~6 DEG C/min heating rate under be warming up to 380~420 DEG C, and 2~6h of constant temperature carries out thermal polymerization
Reaction, that is, obtain the polymerbitumen containing mesocarbon microspheres.The polymerisation protective atmosphere is N2；
(4) polymerbitumen for obtaining step (3) and washing oil in mass ratio 1:1~1:3, under conditions of 170~200 DEG C
Be stirred, thermosol, filtering, the filter cake after filtering is stripped to phegma to be colourless with organic solvent.The washing oil
Boiling range is 245~290 DEG C, and the filtrate containing washing oil is distilled by heating, you can realizes that washing oil recycles；The organic solvent
Including a kind of or two of which mixture in pyridine, toluene, quinoline, tetrahydrofuran, can repeatedly be used to extract；
(5) filter cake after being extracted to step (4), under the conditions of 60~150 DEG C, vacuum are 0.09MPa, vacuum drying 6
~24h removes solvent, that is, obtains final products mesocarbon microspheres.
Mesocarbon microspheres prepared by the above method, 1.8~10um of particle size range, the yield of mesocarbon microspheres for 8~
12%.
Compared with prior art, advantage for present invention and have the beneficial effect that：
(1) asphalt and additive rosin and carbon black N110 abundances, and it is cheap.
(2) by asphalt and additive premix the pre-heat treatment, in order to make additive with asphalt poly-
It is sufficiently mixed before closing reaction, in addition can effectively removes the micromolecular compound for being difficult to polymerize in raw material, obtain fragrance
Spend the asphalt of higher.
(3) by controlling the mass fraction of additive, heat polymerization is carried out to asphalt, size distribution can be prepared
Uniformly, the preferable mesocarbon microspheres of sphericity.
(4) particle size range for the mesocarbon microspheres that the present invention is prepared using asphalt is 1.8~10um, intermediate-phase carbon
The yield of microballoon is 8~12%.
Embodiment
The embodiment of the present invention is described in further detail with reference to embodiments.The present invention is not limited to following
Embodiment, in the range of the front and rear objective is not departed from, all modifications and variation based on basic thought of the present invention, belong to
In the claimed technical scope of the present invention.
Embodiment 1：
Asphalt is mixed with the carbon black N110 that mass fraction is 2% and is placed in reaction kettle, then the heating with 4 DEG C/min
Speed is warming up to 300 DEG C, in N2Under the conditions of flow 60mL/min, mechanical agitation rotating speed 150r/min, constant temperature 2h the pre-heat treatments, i.e.,
Obtain asphalt and the carbon black N110 of removing small molecule is sufficiently mixed thing.Afterwards in N2Under protection, with the speed of 5 DEG C/min
It is warming up to 400 DEG C, under conditions of pressure 1MPa and mechanical agitation rotating speed 200r/min, constant temperature 4h carries out polymerisation, to obtain the final product
To the polymeric petroleum pitch containing mesocarbon microspheres.With the washing oil of 2 times of quality to above-mentioned polymeric petroleum pitch in 190 DEG C of conditions
Lower stirring, thermosol, filtering, the filter cake after filtering are stripped with pyridine colourless to phegma.Afterwards by the filter cake after extracting
Under the conditions of 80 DEG C, vacuum are 0.09MPa, vacuum drying 12h removing solvents, obtain mesocarbon microspheres.Among petroleum base
The particle mean size of phase carbon microspheres is 8.93um, yield 10.2%.
Embodiment 2：
Asphalt is mixed with the rosin that mass fraction is 2%, then 300 DEG C are warming up to the speed of 4 DEG C/min, in N2
Under the conditions of flow 40mL/min, mechanical agitation rotating speed 200r/min, constant temperature 2h the pre-heat treatments, that is, obtain removing small molecule oil
Pitch and rosin are sufficiently mixed thing.Afterwards in N2Under protection, 410 DEG C are warming up to the speed of 5 DEG C/min, pressure 1MPa,
Under conditions of mechanical agitation rotating speed 200r/min, constant temperature 5h carries out polymerisation, that is, obtains the polymerization containing mesocarbon microspheres
Asphalt.With the washing oil of 3 times of quality machinery, thermosol, filtering under the conditions of 180 DEG C to above-mentioned polymeric petroleum pitch, will filter
Filter cake afterwards is stripped colourless to phegma with toluene.It is afterwards 0.09MPa bars in 60 DEG C, vacuum by the filter cake after extracting
Under part, vacuum drying 12h removing solvents, obtain mesocarbon microspheres.The particle mean size of petroleum base mesocarbon microspheres is
5.88um, yield 8.83%.
Embodiment 3：
Asphalt is mixed with the rosin that mass fraction is 5%, then 280 DEG C are warming up to the heating rate of 5 DEG C/min,
In N2Under the conditions of flow 80mL/min, mechanical agitation rotating speed 200r/min, constant temperature 2h the pre-heat treatments, that is, obtain removing small molecule
Asphalt and rosin are sufficiently mixed thing.Afterwards in N2Under protection, 410 DEG C are warming up to the heating rate of 6 DEG C/min, is being pressed
Under conditions of power 1MPa, mechanical agitation rotating speed 200r/min, constant temperature 4h carries out polymerisation, that is, obtains containing mesocarbon microspheres
Polymeric petroleum pitch.Again with the washing oil of 2 times of quality to above-mentioned polymeric petroleum pitch stirring, thermosol, mistake under the conditions of 170 DEG C
Filter, the filter cake after filtering is stripped with tetrahydrofuran colourless to phegma.Afterwards by the filter cake after extracting in 90 DEG C, vacuum
Spend under the conditions of 0.09MPa, vacuum drying 24h removing solvents, obtain mesocarbon microspheres.Petroleum base mesocarbon microspheres is put down
Equal granularity is 2.66um, yield 9.79%.
Embodiment 4：
Asphalt is mixed with the carbon black N110 that mass fraction is 0.5% and is placed in reaction kettle, then the liter with 5 DEG C/min
Warm speed is warming up to 290 DEG C, in N2Under the conditions of flow 50mL/min, mechanical agitation rotating speed 150r/min, constant temperature 2h the pre-heat treatments,
Obtain asphalt and the carbon black N110 of removing small molecule is sufficiently mixed thing.Afterwards in N2Under protection, with the speed of 6 DEG C/min
Rate is warming up to 390 DEG C, and under conditions of pressure 0.5MPa and mechanical agitation rotating speed 200r/min, constant temperature 6h carries out polymerisation,
Obtain the polymeric petroleum pitch containing mesocarbon microspheres.With the washing oil of 3 times of quality to above-mentioned polymeric petroleum pitch at 200 DEG C
Under the conditions of stirring, thermosol, filtering, the filter cake after filtering is stripped with pyridine colourless to phegma.Afterwards by after extracting
For filter cake under the conditions of 80 DEG C, vacuum are 0.09MPa, vacuum drying 18h removing solvents, obtain mesocarbon microspheres.Petroleum base
The particle mean size of mesocarbon microspheres is 9.88um, yield 8.0%.
Embodiment 5：
Rosin that asphalt and mass fraction are 2%, 1% carbon black N110 are mixed and be placed in reaction kettle, then with 4
DEG C/heating rate of min is warming up to 300 DEG C, in N2Under the conditions of flow 80mL/min, mechanical agitation rotating speed 200r/min, constant temperature
2h the pre-heat treatments, that is, obtain the removing asphalt of small molecule, carbon black N110 and rosin is sufficiently mixed thing.Afterwards in N2Protection
Under, 400 DEG C are warming up to the speed of 4 DEG C/min, under conditions of pressure 1.0MPa and mechanical agitation rotating speed 200r/min, constant temperature
4.5h carries out polymerisation, that is, obtains the polymeric petroleum pitch containing mesocarbon microspheres.With the washing oil of 2 times of quality to above-mentioned poly-
Close asphalt stirring, thermosol, filtering under the conditions of 180 DEG C, by the filter cake after filtering with toluene be stripped to phegma without
Color.Afterwards by the filter cake after extracting under the conditions of 60 DEG C, vacuum are 0.09MPa, vacuum drying 24h removing solvents, in acquisition
Between phase carbon microspheres.The particle mean size of petroleum base mesocarbon microspheres is 3.96um, yield 10.8%.
Embodiment 6：
Asphalt is mixed with the rosin that mass fraction is 10% and is placed in reaction kettle, then the heating speed with 4 DEG C/min
Rate is warming up to 300 DEG C, in N2Under the conditions of flow 60mL/min, mechanical agitation rotating speed 200r/min, constant temperature 1.5h the pre-heat treatments, i.e.,
The asphalt and rosin for obtaining removing small molecule are sufficiently mixed thing.Afterwards in N2Under protection, heated up with the speed of 5 DEG C/min
To 400 DEG C, under conditions of pressure 1.0MPa and mechanical agitation rotating speed 200r/min, constant temperature 4h carries out polymerisation, that is, obtains
Polymeric petroleum pitch containing mesocarbon microspheres.With the washing oil of 2 times of quality to above-mentioned polymeric petroleum pitch under the conditions of 180 DEG C
Stirring, thermosol, filtering, the filter cake after filtering are stripped with pyridine colourless to phegma.Afterwards by the filter cake 90 after extracting
DEG C, vacuum be 0.09MPa under the conditions of, vacuum drying 20h removing solvent, obtain mesocarbon microspheres.Petroleum base intermediate-phase carbon
The particle mean size of microballoon is 1.82um, yield 11.4%.
Claims (8)
- A kind of 1. method for efficiently preparing asphalt base mesocarbon microspheres, it is characterised in that following steps：(1) asphalt and additive are mixed in a certain ratio, are added in high-temperature high-pressure reaction kettle；(2) by the reaction kettle equipped with asphalt and additive agent mixture, 250~300 DEG C are warming up to certain speed, in N2 The lower mechanical agitation of protection, 1~2h of constant temperature carry out the pre-heat treatment, and obtain asphalt and additive is sufficiently mixed thing；(3) asphalt and additive are sufficiently mixed thing, 100~200r/min of stir speed (S.S.), pressure 0.5~ 2.0MPa, 4~6 DEG C/min heating rate under be warming up to 380~420 DEG C, and 2~6h of constant temperature carries out heat polymerization, to obtain the final product To the polymerbitumen containing mesocarbon microspheres；(4) polymerbitumen and washing oil are stirred by certain mass ratio, under conditions of 170~200 DEG C, thermosol, filtering, will It is colourless that filter cake after filtering is stripped to phegma with organic solvent；(5) under the conditions of 60~150 DEG C, vacuum are 0.09MPa, 6~24h of vacuum drying takes off filter cake after being extracted to step (4) Except solvent, that is, obtain final products mesocarbon microspheres.
- A kind of 2. method for efficiently preparing asphalt base mesocarbon microspheres according to claim 1, it is characterised in that (1) asphalt described in, its toluene insolubles are 0.1%, and quinoline insolubles is less than 0.05%；The additive includes pine One or two kinds of mixture in fragrant or carbon black N110, additive mass fraction are 0.5~10%.
- A kind of 3. method for efficiently preparing asphalt base mesocarbon microspheres according to claim 1, it is characterised in that (2) heating rate is 3~6 DEG C/min, N240~80mL/min of flow, 100~200r/min of mechanical agitation speed.
- A kind of 4. method for efficiently preparing asphalt base mesocarbon microspheres according to claim 1, it is characterised in that (3) heat polymerization, its protective atmosphere are N2。
- A kind of 5. method for efficiently preparing asphalt base mesocarbon microspheres according to claim 1, it is characterised in that (4) the washing oil boiling range used in is 245~290 DEG C, and the mass ratio of polymerbitumen and washing oil is 1:1~1:3；Filtrate containing washing oil Distilled by heating, you can realize that washing oil recycles.
- A kind of 6. method for efficiently preparing asphalt base mesocarbon microspheres according to claim 1, it is characterised in that (4) organic solvent used in is a kind of or two of which mixture in pyridine, toluene, quinoline, tetrahydrofuran, and can be with Repeatedly it is used to extract.
- 7. the asphalt base mesocarbon microspheres obtained according to any methods of claim 1-6, it is characterised in that system Standby mesocarbon microspheres, 1.8~10um of particle size range, the yield of mesocarbon microspheres is 8~12%.
- 8. a kind of lithium ion battery negative material, it is characterised in that the asphalt base intermediate-phase carbon described in claim 7 is micro- Ball, is prepared through carbonization, graphitization.
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| CN109179371A (en) * | 2018-10-24 | 2019-01-11 | 武汉科技大学 | A kind of mesocarbon microspheres and the method using pitch hot tearing oil preparation mesocarbon microspheres |
| CN110803693A (en) * | 2019-11-13 | 2020-02-18 | 溧阳紫宸新材料科技有限公司 | Anthracene oil-based mesocarbon microbeads and preparation method and application thereof |
| CN111392707A (en) * | 2020-03-25 | 2020-07-10 | 中国科学院化学研究所 | Method for preparing mesocarbon microbeads by direct coal liquefaction |
| CN112011383A (en) * | 2020-07-31 | 2020-12-01 | 吉诺润滑技术(苏州)有限公司 | Carbon microsphere lubricating fluid antiwear agent and antiwear lubricating fluid |
| CN112758916A (en) * | 2020-12-25 | 2021-05-07 | 西安交通大学 | Active graphene and method for preparing active graphene through mesophase pitch |
| CN113247878A (en) * | 2021-06-30 | 2021-08-13 | 北京化工大学 | Preparation method and application of asphalt-based carbon microspheres |
| CN114477126A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Mesocarbon microbeads and preparation method thereof |
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| CN109179371A (en) * | 2018-10-24 | 2019-01-11 | 武汉科技大学 | A kind of mesocarbon microspheres and the method using pitch hot tearing oil preparation mesocarbon microspheres |
| CN110803693A (en) * | 2019-11-13 | 2020-02-18 | 溧阳紫宸新材料科技有限公司 | Anthracene oil-based mesocarbon microbeads and preparation method and application thereof |
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| CN114477126A (en) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | Mesocarbon microbeads and preparation method thereof |
| CN112758916A (en) * | 2020-12-25 | 2021-05-07 | 西安交通大学 | Active graphene and method for preparing active graphene through mesophase pitch |
| CN113247878A (en) * | 2021-06-30 | 2021-08-13 | 北京化工大学 | Preparation method and application of asphalt-based carbon microspheres |
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