CN108264915A - A kind of preparation method for spinning mesophase pitch - Google Patents
A kind of preparation method for spinning mesophase pitch Download PDFInfo
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- CN108264915A CN108264915A CN201810233342.6A CN201810233342A CN108264915A CN 108264915 A CN108264915 A CN 108264915A CN 201810233342 A CN201810233342 A CN 201810233342A CN 108264915 A CN108264915 A CN 108264915A
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- mesophase pitch
- carbonization
- spinning
- preparation
- pressure
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/04—Working-up pitch, asphalt, bitumen by chemical means reaction by blowing or oxidising, e.g. air, ozone
-
- 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
Abstract
The invention discloses a kind of preparation methods for spinning mesophase pitch.The invention mainly includes steps：Using catalytic cracking slurry oil as raw material, to catalyze and synthesize naphthalene oligomerization asphalt as Co carbonization agent and for hydrogen reagent, Co carbonization pressure polymerization is carried out under 380 ~ 450 DEG C of temperature condition, under the pressure of 0.5 ~ 6MPa and reacts 3 ~ 12h, is then unloaded to normal pressure and is obtained Co carbonization polymerbitumen；Co carbonization polymerbitumen is subjected to nitrogen bubbling with the tolerance of 3 ~ 10L/ (minKg) under normal pressure and 370 ~ 440 DEG C of temperature condition again and purges 1 ~ 20h, room temperature is down to the end of reaction can obtain and high-quality spin mesophase pitch；Continuous spinnings more than 500 hole 5000m can be realized through melt spinning using this mesophase pitch as raw material.The present invention has technique and equipment is simple, reaction condition is mild, and prepared mesophase pitch softening point is relatively low, good spinnability, at low cost, it is easy to accomplish the features such as industrialized production.
Description
Technical field
The invention belongs to high-performance pitch based carbon fiber spinning method for preparing raw material technical fields, and in particular to Yi Zhongke
Spin the preparation method of mesophase pitch.
Background technology
Mesophase pitch is prepare the advanced Carbon Materials such as high-performance pitch Carbon fibe, needle coke and C/C composite materials excellent
Good presoma.As high-performance carbonaceous presoma generally require mesophase pitch have hetero atom is few, ash content is low, aromaticity is high,
The features such as low and neat molecules align of condensation degree, high carbon yield, preferable mobility.And for being used to prepare high-performance
The presoma mesophase pitch of pitch based carbon fiber has higher requirement to its rheological property and purity.
Research shows that the presence of the short alkyl branches and cycloalkane structure in mesophase pitch molecular structure can effectively improve
The solubility of mesophase pitch improves its rheological property, so as to better spinnability.
Catalytic cracking slurry oil is to prepare a kind of common raw material that oil is mesophase pitch, is individually carried out in thermal polymerization preparation
Between during asphalt phase, with the progress of polymerisation and the removing of alkyl branches, H/C molar ratios significantly drop in pitch
It is low so that the mesophase pitch softening point of preparation is relatively high therefore is preparing interphase drip by raw material of catalytic cracking slurry oil
It generally requires to carry out hydrotreating in green process, main path includes high-pressure hydrogenation processing and reagent adds two class of hydrogen.Mochida
Deng using catalytic cracking slurry oil pitch as raw material, two-step process is purged by pressure polymerization and vacuum it is prepared for 100% interphase and drip
Blueness, and carried out spinning in higher temperature.It looks into celebrating virtue to wait using catalytic cracking slurry oil richness aromatic component as raw material, be cut by solvent
It is prepared for that mesophase pitch can be spun with thermal polymerization process.Chinese patent CN106544758A adds using catalytic slurry as raw material through high pressure
After hydrogen pretreatment and the classification charing of two one-step polycondensations obtain interphase product, it is fine that high modulus pitch-based carbon is prepared through melt spinning
Dimension.Chinese patent CN105238430A is prepared for by hydroisomerizing and thermal polycondensation two-step process with the Gao Pin compared with low softening point
Matter mesophase pitch.Generally speaking, the mesophase pitch H/C that prepared by individual thermal polycondensation process is relatively low, and softening point is high, spinning condition
It is more harsh.Although and solvent cutting and add hydrogen-thermal polymerization process can be prepared compared with low softening point mesophase pitch, these
Preparation process production cost is higher, limits its further popularization and application.
Currently used Co carbonization reagent is divided into two classes.The first kind is the pure materials such as naphthalene, naphthane, decahydronaphthalene, such common
Charring reagent adds hydrogen with obvious effects, can effectively reduce interphase softening point, but can be substantially reduced mesophase pitch yield, simultaneously altogether
The dosage of carbonized agent is larger, and hydrogenation reaction pressure is higher, and there are the problems such as Co carbonization reagent abjection difficulty.Another kind of Co carbonization examination
Agent is the more complicated petroleum industry by-product of component, and I.Mochida is passed through using catalytic cracked oil pulp and decompression residuum as raw material
Co carbonization technique prepares needle coke.Li Xuejun etc. has studied the Co carbonization of catalytic cracked oil pulp aromatic rich cut and ethylene bottom oil
Behavior simultaneously prepares the streamlined interphase of wide area, and then can prepare needle coke.China University Of Petroleum Beijing Wang Liang is with catalytic cracked oil pulp
Co carbonization is carried out under normal pressure with coal tar asphalt for raw material mesophase pitch is prepared and to prepare needle coke.In summary
Decompression residuum, ethylene bottom oil and coal tar are due to its own complicated component, although can effectively improve catalysis by Co carbonization technique
The optical characteristics of cracking slurry oil mesophase pitch and coking performance, but be difficult to prepare spinning mesophase pitch.And naphthalene oligomerization asphalt
As a kind of catalytic polymerization pitch, compared to other Co carbonization agent, its molecular structure is relatively controllable, while can turn in naphthalene oligomerization asphalt
The presence of hydrogen is moved, the liquid carbonized reaction rate of catalytic cracked oil pulp and the structure composition of interphase can be changed；Co carbonization is anti-
Transferable hydrogen during answering in naphthalene oligomerization asphalt carries out hydrogenating reduction to catalytic cracked oil pulp and forms hydrogenation of aromatics and cycloalkanes
Structure so as to effectively improve mesophase pitch H/C molar ratios, reduce mesophase pitch softening point, improves mesophase pitch
Soluble and rheological property.
Invention content
Present invention is generally directed to it is existing prepare mesophase pitch method as raw material using catalytic cracking slurry oil there are techniques to answer
Miscellaneous, the problems such as equipment requirement is high, mesophase pitch softening point is higher, spinning is unstable, it is intended to which exploitation is a kind of with catalytic pyrolysis oil
It starches as primary raw material, naphthalene oligomerization asphalt prepares the high-quality new method for spinning mesophase pitch for auxiliary material.This method passes through Co carbonization
Polymerization technique, thermal polymerization process and two kinds of Co carbonization raw material different ratios realize prepared mesophase pitch softening point compared with
It is low, H/C moles higher, can continuous fusion spinning up to more than 5000m.
The present invention to achieve the above object, adopts the following technical scheme that：
A kind of preparation method for spinning mesophase pitch, flow mainly include：Catalytic cracking slurry oil is used as raw material, to
It wherein adds in and catalyzes and synthesizes naphthalene oligomerization asphalt as Co carbonization agent and for hydrogen reagent, under 360~450 DEG C of temperature condition, 0.5
Co carbonization pressure polymerization is carried out under the pressure of~6MPa and reacts 3~12h, then unloads to normal pressure and obtains Co carbonization polymerbitumen；Again will
Co carbonization polymerbitumen carries out nitrogen under normal pressure and 350~440 DEG C of temperature condition with the tolerance of 3~10L/ (minKg)
Bubbling purges or 1~20h of vacuum distillation, and room temperature is down to the end of reaction can obtain that softening point is relatively low, H/C moles higher excellent
Matter can spin mesophase pitch.
The catalytic cracking slurry oil mole H/C is 0.80~1.6.
The naphthalene oligomerization asphalt softening point that catalyzes and synthesizes is 40~180 DEG C, and mole H/C is 0.60~0.79.
Naphthalene oligomerization asphalt use quality is catalyzed and synthesized as catalytic cracking slurry oil 0.05~1 times.
The vacuum distillation pressure is -0.1~0MPa.
Mesophase pitch softening point prepared by this method is 250~290 DEG C, and interphase content 95~100%, H/C rubs
Your score ratio is 0.50~0.65, and quinoline insolubles content is less than 26wt%, and it is continuous that more than 5000m can be prepared through melt spinning
Long filament, string diameter is up to 10~15 μm.
Present invention advantageous effect compared with existing preparation method is：
The use of catalytic cracked oil pulp is primary raw material, naphthalene oligomerization asphalt prepares intermediate as Co carbonization agent, the two Co carbonization
The linear combination for preparing mesophase pitch yield, interphase prepared by Co carbonization process is polymerized alone higher than the two in asphalt phase yield
Asphaltene molecule extent of polymerization is relatively higher.
It adds in the naphthalene oligomerization asphalt for containing cycloalkane structure to be used as hydrogen reagent, improves the composition structure of reaction system, make
System rheological performance is improved, and is easy to regulate and control product molecule structure, is conducive to prepare and good is spun mesophase pitch.
Mesophase pitch softening point is H/C moles higher down to 250~290 DEG C, and soluble good, viscosity is low, after being conducive to
It is continuous to carry out melt spinning.
Production process of the present invention is simple, and reaction condition is mild, low for equipment requirements, easy to spread to realize industrialization.
Specific embodiment
Being further discussed below provided by the present invention prepared using catalytic cracking slurry oil as primary raw material with reference to embodiment can
The method for spinning mesophase pitch, but the scope of protection of present invention is not limited to the range described in embodiment, it is specific real
It applies " part " of expression amount, " content " etc. in example and represents mass fraction.
Embodiment 1
Take H/C molar ratios are 1.0, xylene solubles content is 100% 80 parts of catalytic cracking slurry oil and to catalyze and synthesize
Softening point be 85 DEG C, 20 parts of the naphthalene oligomerization asphalts of H/C molar ratios 0.73 is stirred, and be passed through in ordinary high pressure reaction kettle
Air in nitrogen purging kettle, is warming up to 420 DEG C with 5 DEG C/min heating rates and keeps the temperature 6h, insulating process system pressure is
2.2MPa, Temperature fall after heat preservation unload system pressure to normal pressure, obtain Co carbonization polymerbitumen.
By Co carbonization polymerbitumen under an inert atmosphere in 400 DEG C under normal pressure bubbling blow away except light component, gas flow
For 3L/ (min.Kg), persistently stirred in purge, reaction 10h obtain softening point be 260 DEG C, carbon yield 87.3%, H/C
The mesophase pitch for being 98% for 0.574, quinoline insolubles 20.5%, anisotropy constituent content.
Embodiment 2
Take H/C molar ratios are 1.0, xylene solubles content is 100% 50 parts of catalytic cracking slurry oil and to catalyze and synthesize
Softening point be 85 DEG C, 50 parts of the naphthalene oligomerization asphalts of H/C molar ratios 0.73 is stirred, and be passed through in ordinary high pressure reaction kettle
Air in nitrogen purging kettle, is warming up to 420 DEG C with 5 DEG C/min heating rates and keeps the temperature 6h, insulating process system pressure is
1.8MPa, Temperature fall after heat preservation unload system pressure to normal pressure, obtain Co carbonization polymerbitumen.
By Co carbonization polymerbitumen under an inert atmosphere in 400 DEG C of vacuum distillation purgings, pressure is -0.05MPa gas streams
Measure as 3L/ (min.Kg), persistently stirred in purge, reaction 10h obtain softening point be 252 DEG C, carbon yield 85.7%, H/
The mesophase pitch that C is 0.600, quinoline insolubles 18.4%, anisotropy constituent content are 100%.
Embodiment 3
Take H/C molar ratios are 1.2, xylene solubles content is 100% 80 parts of catalytic cracking slurry oil and to catalyze and synthesize
Softening point be 93 DEG C, 20 parts of the naphthalene oligomerization asphalt that H/C molar ratios are 0.76 is stirred, and lead in ordinary high pressure reaction kettle
Enter nitrogen and be forced into 2MPa, 430 DEG C are warming up to 5 DEG C/min heating rates and keep the temperature 3h, insulating process system pressure is
5.3MPa, Temperature fall after heat preservation unload system pressure to normal pressure, obtain Co carbonization polymerbitumen.
By Co carbonization polymerbitumen under an inert atmosphere in 410 DEG C under normal pressure bubbling blow away except light component, gas flow
It for 3L/ (min.Kg), is persistently stirred in purge, reaction 3h obtains that softening point is 262 DEG C, carbon yield 86.0%, H/C are
0.610th, the mesophase pitch that quinoline insolubles 20.0%, anisotropy constituent content are 100%.
Embodiment 4
Take H/C molar ratios are 0.8, xylene solubles content is 100% 80 parts of catalytic cracking slurry oil and to catalyze and synthesize
Softening point be 150 DEG C, 50 parts of the naphthalene oligomerization asphalt that H/C molar ratios are 0.72 is stirred in ordinary high pressure reaction kettle, and
It is passed through nitrogen and is forced into 2MPa, 410 DEG C are warming up to 5 DEG C/min heating rates and keep the temperature 9h, insulating process system pressure is
5.0MPa, Temperature fall after heat preservation unload system pressure to normal pressure, obtain Co carbonization polymerbitumen.
By Co carbonization polymerbitumen under an inert atmosphere in 395 DEG C under normal pressure bubbling blow away except light component, gas flow
For 10L/ (min.Kg), persistently stirred in purge, reaction 14h obtain softening point be 280 DEG C, carbon yield 87.7%, H/C
The mesophase pitch for being 100% for 0.558, quinoline insolubles 24.3%, anisotropy constituent content.
Embodiment 5
Take H/C molar ratios are 0.8, xylene solubles content is 100% 80 parts of catalytic cracking slurry oil and to catalyze and synthesize
Softening point be 150 DEG C, 50 parts of the naphthalene oligomerization asphalt that H/C molar ratios are 0.68 is stirred in ordinary high pressure reaction kettle, and
It is passed through nitrogen and is forced into 2MPa, 410 DEG C are warming up to 5 DEG C/min heating rates and keep the temperature 9h, insulating process system pressure is
5.0MPa, Temperature fall after heat preservation unload system pressure to normal pressure, obtain Co carbonization polymerbitumen.
By Co carbonization polymerbitumen under an inert atmosphere in 395 DEG C vacuum distillation purging, pressure be -0.09MPa, gas stream
Measure as 10L/ (min.Kg), persistently stirred in purge, reaction 3h obtain softening point be 280 DEG C, carbon yield 88.2%, H/
C is 0.540, quinoline insolubles 25.0%, and anisotropy constituent content is 100% mesophase pitch.
Claims (7)
1. a kind of preparation method for spinning mesophase pitch, it is characterised in that including following steps：
Step (1) uses catalytic cracking slurry oil as raw material, thereto add in catalyze and synthesize naphthalene oligomerization asphalt as Co carbonization agent with
For hydrogen reagent, carried out under 380~450 DEG C of temperature condition, under the pressure of 0.5~6MPa Co carbonization pressure polymerization reaction 3~
Then 12h is unloaded to normal pressure and is obtained Co carbonization polymerbitumen；
Step (2) again by Co carbonization polymerbitumen under normal pressure and 370~440 DEG C of temperature condition with 3~10L/ (minKg)
Tolerance carry out 1~20h of nitrogen bubbling purging or vacuum distillation, be down to room temperature to the end of reaction and can spin mesophase pitch to obtain the final product.
2. a kind of preparation method for spinning mesophase pitch according to claim 1, it is characterised in that：The step (1)
In catalytic cracking slurry oil be slurry oil after purification, H/C is 0.7~1.6, and molecular weight distribution is 250~1500.
3. a kind of preparation method for spinning mesophase pitch according to claim 1, it is characterised in that：The step (1)
In catalyze and synthesize naphthalene oligomerization asphalt softening point as 40~180 DEG C, H/C is 0.60~0.79.
4. a kind of preparation method for spinning mesophase pitch according to claim 1, it is characterised in that：The step (1)
In the naphthalene oligomerization asphalt use quality that catalyzes and synthesizes be 0.05~1 times of catalytic cracking slurry oil.
5. a kind of preparation method for spinning mesophase pitch according to claim 1, it is characterised in that：The step (2)
In vacuum distillation pressure be -0.1~0MPa.
6. a kind of preparation method for spinning mesophase pitch according to claim 1, it is characterised in that：The step (2)
In the prepared mesophase pitch softening point that spins be 250~300 DEG C, interphase content is 95~100%, H/C molar fractions
Than being 0.50~0.65, quinoline insolubles content is less than 25wt%.
7. a kind of preparation method for spinning mesophase pitch according to claim 1, it is characterised in that：The step (2)
In the prepared mesophase pitch that spins can realize more than 500 hole 5000m continuous spinning through melt spinning, string diameter is up to 10~15
μm。
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| CN108264915B CN108264915B (en) | 2020-12-04 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110272755A (en) * | 2019-05-13 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of high thermal stability spinning asphalt preparation method and its dedicated unit |
| CN111439741A (en) * | 2020-05-29 | 2020-07-24 | 中国石油大学(华东) | Method for improving atmospheric pyrolysis carbonization carbon formation rate of ethylene tar and application thereof |
| CN113621130A (en) * | 2021-08-02 | 2021-11-09 | 武汉科技大学 | Preparation method of high-quality spinning asphalt, product and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110272755A (en) * | 2019-05-13 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of high thermal stability spinning asphalt preparation method and its dedicated unit |
| CN110272755B (en) * | 2019-05-13 | 2021-02-23 | 湖南东映碳材料科技有限公司 | Preparation method of spinning asphalt with high thermal stability and special device thereof |
| CN111439741A (en) * | 2020-05-29 | 2020-07-24 | 中国石油大学(华东) | Method for improving atmospheric pyrolysis carbonization carbon formation rate of ethylene tar and application thereof |
| CN113621130A (en) * | 2021-08-02 | 2021-11-09 | 武汉科技大学 | Preparation method of high-quality spinning asphalt, product and application thereof |
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| CN108264915B (en) | 2020-12-04 |
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