CN102776014A - Preparation method of petroleum-based high softening point spinning pitch - Google Patents
Preparation method of petroleum-based high softening point spinning pitch Download PDFInfo
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- CN102776014A CN102776014A CN2012102528431A CN201210252843A CN102776014A CN 102776014 A CN102776014 A CN 102776014A CN 2012102528431 A CN2012102528431 A CN 2012102528431A CN 201210252843 A CN201210252843 A CN 201210252843A CN 102776014 A CN102776014 A CN 102776014A
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Abstract
The invention discloses a preparation method of petroleum-based high softening point spinning pitch and belongs to the technical field of spinning pitch. The preparation method includes the steps of preheating ethylene tar, performing wiped film vaporization to remove light components at the temperature of 220-280 DEG C under the vacuum degree of 80-120Pa so as to obtain ethylene tar pitch, transferring the ethylene tar pitch into a reactor, heating to 330-360 DEG C, performing constant-temperature thermal polycondensation to obtain ethylene tar pitch softening at 200-225 DEG C, performing wiped film vaporization to the ethylene tar pitch to remove part of the light components at the temperature of 340-370 DEG C under the vacuum degree of 80-120Pa so as to finally obtain spinning pitch which softens at 270-285 DEG C. The preparation method has the advantages of continuity in operation, simplicity in process flow, high controllability and suitability for industrial production. The prepared spinning pitch is high in coking value, excellent in spinning performance, and available for continuous spinning more than 10000m in length.
Description
Technical field
The present invention relates to a kind of is the preparation method of high softening-point spinning asphalt with oil, particularly relates to a kind of preparation method of ethylene bottom oil high softening-point spinning asphalt, belongs to the spinning asphalt technical field.
Background technology
Pitch-based carbon fiber research starts from the sixties in 20th century, is sent out the ME of clear pitch-based carbon fiber by Japanese large space between muscles China fir youth.The research of pitch-based carbon fiber then obtains develop rapidly abroad.Along with Chinese economic development, the diversification of charcoal fiber applications development in recent years, its Application Areas is constantly widened.Also obtain certain achievement in research, but also do not formed throughput.
In the CN101135074A general purpose grade charcoal fiber preparation method, the employing ethylene bottom oil is a raw material, after the first atmospheric oxidation again thermal polycondensation prepare the high softening-point spinning asphalt.Most of light constituent can not effectively utilize in this method ethylene bottom oil.It is raw material that the Liaoyang petrochemical industry adopts ethylene cracking tar, frequent, vacuum flashing, and operations such as gas is carried, evaporation, preparation high softening-point spinning asphalt, the technological process step is more.
Summary of the invention
The object of the present invention is to provide a kind of oil is the preparation method of high softening-point spinning asphalt, and this method has the advantages that technical process is simple, operation is continuous, controllability is good.
The present invention realizes that through following technical scheme a kind of oil is the preparation method of high softening-point spinning asphalt, it is characterized in that may further comprise the steps:
80 ~ 120 ℃ of ethylene bottom oil elder generation preheatings; Pull out light constituent in 220 ~ 280 ℃ of temperature and vacuum tightness 80 ~ 120Pa wiped film vaporization then; Obtain softening temperature and be 80 ~ 100 ℃, coking value and be 40 ~ 50% ethylene bottom oil pitch, in this ethylene bottom oil pitch dislocation reaction kettle, be warming up to 330 ~ 360 ℃ with 2 ~ 5 ℃/min of temperature rise rate; Constant temperature thermal polycondensation 4 ~ 6 hours; Make softening temperature and be 200 ~ 225 ℃ ethylene bottom oil pitch, this ethylene bottom oil pitch is pulled out the part light constituent 340 ~ 370 ℃ of temperature with vacuum tightness 80 ~ 120Pa wiped film vaporization, finally obtains softening temperature and be 270 ~ 285 ℃ spinning asphalt.
Advantage of the present invention and effect are following: the present invention adopts the wiped film vaporization technology to pull out the part light constituent ethylene bottom oil earlier, obtains ethylene bottom oil pitch, and the light constituent of extracting can be used as preparation sooty high quality raw material.Then ethylene bottom oil pitch is carried out thermal polycondensation in reaction kettle, improving ethylene bottom oil bituminous softening temperature is 200 ~ 225 ℃, and pulling out the part light constituent through luwa evaporator again, to make softening temperature be 270 ~ 285 ℃ of spinning asphalts.This method is a continuous operation, and technical process is simple, and controllability is good, is fit to suitability for industrialized production.Prepared spinning asphalt coking value is high, and spinning properties is excellent, and continuous spinning length can reach more than the ten thousand metres, even also fracture of wire can not take place in high rotating speed spinning.
Embodiment
Embodiment 1
After 110 ℃ of the 350kg ethylene bottom oil preheatings; Pull out light constituent in 240 ℃ of temperature and vacuum tightness 90Pa wiped film vaporization, obtaining softening temperature is 85 ℃, and coking value is 40% ethylene bottom oil pitch 130kg; Then with in the ethylene bottom oil pitch dislocation reaction kettle; Be warming up to 340 ℃ with 3 ℃/min of temperature rise rate, constant temperature thermal polycondensation 5 hours, improving ethylene bottom oil bituminous softening temperature is 225 ℃; This ethylene bottom oil pitch is pulled out the part light constituent in 350 ℃ of temperature and vacuum tightness 110Pa wiped film vaporization, obtains high softening-point spinning asphalt 70kg.Adopting ring and ball method to test softening temperature is 275 ℃, and adopting GB 8727-88 test coking value is 80.7%.With 15000 meters of this spinning asphalt continuous spinnings, the silk footpath is 16 μ m.
Embodiment 2
After 115 ℃ of the 350kg ethylene bottom oil preheatings; Pull out light constituent in 245 ℃ of temperature and vacuum tightness 95Pa wiped film vaporization, obtaining softening temperature is 88 ℃, and coking value is 43% ethylene bottom oil pitch 126kg; Then with in the ethylene bottom oil pitch dislocation reaction kettle; Be warming up to 350 ℃ with 3 ℃/min of temperature rise rate, constant temperature thermal polycondensation 4.5 hours, improving ethylene bottom oil bituminous softening temperature is 220 ℃; This ethylene bottom oil pitch is pulled out the part light constituent in 345 ℃ of temperature and vacuum tightness 110Pa wiped film vaporization, obtains high softening-point spinning asphalt 75kg.Adopting ring and ball method to test softening temperature is 271 ℃, and adopting GB 8727-88 test coking value is 80.1%.With 13000 meters of this spinning asphalt continuous spinnings, the silk footpath is 15 μ m.
Embodiment 3
After 110 ℃ of the 350kg ethylene bottom oil preheatings; Pull out light constituent in 238 ℃ of temperature and vacuum tightness 85Pa wiped film vaporization, obtaining softening temperature is 80 ℃, and coking value is 39% ethylene bottom oil pitch 135kg; Then with in the ethylene bottom oil pitch dislocation reaction kettle; Be warming up to 360 ℃ with 4 ℃/min of temperature rise rate, constant temperature thermal polycondensation 4.5 hours, improving ethylene bottom oil bituminous softening temperature is 227 ℃; This ethylene bottom oil pitch is pulled out the part light constituent in 360 ℃ of temperature and vacuum tightness 115Pa wiped film vaporization, obtains high softening-point spinning asphalt 72kg.Adopting ring and ball method to test softening temperature is 280 ℃, and adopting GB 8727-88 test coking value is 82.4%.With 15000 meters of this spinning asphalt continuous spinnings, filament diameter is 14 μ m.
Embodiment 4
After 120 ℃ of the 350kg ethylene bottom oil preheatings; Pull out light constituent in 260 ℃ of temperature and vacuum tightness 105Pa wiped film vaporization, obtaining softening temperature is 95 ℃, and coking value is 45% ethylene bottom oil pitch 124kg; Then with in the ethylene bottom oil pitch dislocation reaction kettle; Be warming up to 350 ℃ with 4 ℃/min of temperature rise rate, constant temperature thermal polycondensation 4 hours, improving ethylene bottom oil bituminous softening temperature is 231 ℃; This ethylene bottom oil pitch is pulled out the part light constituent in 360 ℃ of temperature and vacuum tightness 120Pa wiped film vaporization, obtains high softening-point spinning asphalt 67kg.Adopting ring and ball method to test softening temperature is 285 ℃, and adopting GB 8727-88 test coking value is 82.9%.With 16000 meters of this spinning asphalt continuous spinnings, the silk footpath is 15 μ m.
Embodiment 5
After 115 ℃ of the 350kg ethylene bottom oil preheatings; Pull out light constituent in 250 ℃ of temperature and vacuum tightness 95Pa wiped film vaporization, obtaining softening temperature is 87 ℃, and coking value is 43% ethylene bottom oil pitch 126kg; Then with in the ethylene bottom oil pitch dislocation reaction kettle; Be warming up to 360 ℃ with 3 ℃/min of temperature rise rate, constant temperature thermal polycondensation 5 hours, improving ethylene bottom oil bituminous softening temperature is 230 ℃; This ethylene bottom oil pitch is pulled out the part light constituent in 350 ℃ of temperature and vacuum tightness 115Pa wiped film vaporization, obtains high softening-point spinning asphalt 72kg.Adopting ring and ball method to test softening temperature is 279 ℃, and adopting GB 8727-88 test coking value is 81.9%.With 15000 meters of this spinning asphalt continuous spinnings, the silk footpath is 15 μ m.
Claims (1)
1. preparation method that oil is the high softening-point spinning asphalt; It is characterized in that may further comprise the steps: 80 ~ 120 ℃ of ethylene bottom oil elder generation preheatings; Pull out light constituent in 220 ~ 280 ℃ of temperature and vacuum tightness 80 ~ 120Pa wiped film vaporization then; Obtain softening temperature and be 80 ~ 100 ℃, coking value and be 40 ~ 50% ethylene bottom oil pitch, in this ethylene bottom oil pitch dislocation reaction kettle, be warming up to 330 ~ 360 ℃ with 2 ~ 5 ℃/min of temperature rise rate; Constant temperature thermal polycondensation 4 ~ 6 hours; Make softening temperature and be 200 ~ 225 ℃ ethylene bottom oil pitch, this ethylene bottom oil pitch is pulled out the part light constituent 340 ~ 370 ℃ of temperature with vacuum tightness 80 ~ 120Pa wiped film vaporization, finally obtains softening temperature and be 270 ~ 285 ℃ spinning asphalt.
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| CN2012102528431A CN102776014B (en) | 2012-07-20 | 2012-07-20 | Preparation method of petroleum-based high softening point spinning pitch |
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| CN2012102528431A CN102776014B (en) | 2012-07-20 | 2012-07-20 | Preparation method of petroleum-based high softening point spinning pitch |
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| CN102776014B CN102776014B (en) | 2013-11-27 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184062A (en) * | 2013-04-03 | 2013-07-03 | 天津大学 | Preparation method of high softening point spinning pitch |
| CN103305942A (en) * | 2013-06-06 | 2013-09-18 | 天津大学 | Spinneret plate and method for preparing mesophase pitch-based strip carbon fibers |
| CN107163971A (en) * | 2017-05-22 | 2017-09-15 | 新疆中碳科技有限责任公司 | A kind of continuous production method of pitch base carbon material feedstock |
| CN111925818A (en) * | 2020-08-14 | 2020-11-13 | 辽宁信德新材料科技股份有限公司 | Carbon fiber spinnable asphalt and preparation method and application thereof |
| CN112592734A (en) * | 2020-11-24 | 2021-04-02 | 新疆中碳新材料科技有限责任公司 | Continuous production method of lithium ion battery cathode coating material |
| CN114149819A (en) * | 2021-12-01 | 2022-03-08 | 中国矿业大学(北京) | Method for increasing softening point temperature of asphalt and asphalt obtained by method |
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2012
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103184062A (en) * | 2013-04-03 | 2013-07-03 | 天津大学 | Preparation method of high softening point spinning pitch |
| CN103305942A (en) * | 2013-06-06 | 2013-09-18 | 天津大学 | Spinneret plate and method for preparing mesophase pitch-based strip carbon fibers |
| CN107163971A (en) * | 2017-05-22 | 2017-09-15 | 新疆中碳科技有限责任公司 | A kind of continuous production method of pitch base carbon material feedstock |
| CN111925818A (en) * | 2020-08-14 | 2020-11-13 | 辽宁信德新材料科技股份有限公司 | Carbon fiber spinnable asphalt and preparation method and application thereof |
| CN112592734A (en) * | 2020-11-24 | 2021-04-02 | 新疆中碳新材料科技有限责任公司 | Continuous production method of lithium ion battery cathode coating material |
| CN114149819A (en) * | 2021-12-01 | 2022-03-08 | 中国矿业大学(北京) | Method for increasing softening point temperature of asphalt and asphalt obtained by method |
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