CN102776014B - Preparation method of petroleum-based high softening point spinning pitch - Google Patents
Preparation method of petroleum-based high softening point spinning pitch Download PDFInfo
- Publication number
- CN102776014B CN102776014B CN2012102528431A CN201210252843A CN102776014B CN 102776014 B CN102776014 B CN 102776014B CN 2012102528431 A CN2012102528431 A CN 2012102528431A CN 201210252843 A CN201210252843 A CN 201210252843A CN 102776014 B CN102776014 B CN 102776014B
- Authority
- CN
- China
- Prior art keywords
- temperature
- pitch
- bottom oil
- ethylene bottom
- spinning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Working-Up Tar And Pitch (AREA)
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 preparation method with petroleum high softening-point spinning asphalt, particularly relate to a kind of preparation method of ethylene bottom oil high softening-point spinning asphalt, belong to the spinning asphalt technical field.
Background technology
Pitch-based carbon fiber research starts from the sixties in 20th century, by Japanese large space between muscles China fir youth, is sent out the manufacturing process that understands pitch-based carbon fiber.The then research of pitch-based carbon fiber obtains develop rapidly abroad.Along with China's expanding economy, 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 preparation method of CN101135074A general purpose grade charcoal fiber, the employing ethylene bottom oil is raw material, after first atmospheric oxidation again thermal polycondensation prepare the high softening-point spinning asphalt.In the method ethylene bottom oil, most of light constituent can not effectively utilize.It is raw material that the Liaoyang petrochemical industry adopts ethylene cracking tar, frequent, vacuum flashing, and the operations such as air lift, evaporation, prepare the high softening-point spinning asphalt, and the technological process step is more.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of petroleum high softening-point spinning asphalt, the method has the advantages that technical process is simple, operation is continuous, controllability is good.
The present invention realized by the following technical programs, and a kind of preparation method of petroleum high softening-point spinning asphalt is characterized in that comprising the following steps:
80 ~ 120 ℃ of the first preheatings of ethylene bottom oil, then in 220 ~ 280 ℃ of temperature and vacuum tightness 80 ~ 120Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 80 ~ 100 ℃, coking value is 40 ~ 50% ethylene bottom oil pitch, by in this ethylene bottom oil pitch dislocation reactor, with 2 ~ 5 ℃/min of temperature rise rate, be warming up to 330 ~ 360 ℃, constant temp. heating polycondensation 4 ~ 6 hours, make softening temperature and be the ethylene bottom oil pitch of 200 ~ 225 ℃, this ethylene bottom oil pitch is pulled out the part light constituent in 340 ~ 370 ℃ of temperature and vacuum tightness 80 ~ 120Pa wiped film vaporization, final acquisition softening temperature is the spinning asphalt of 270 ~ 285 ℃.
Advantage of the present invention and effect are as follows: the present invention first adopts ethylene bottom oil the wiped film vaporization technology to pull out the part light constituent, obtains ethylene bottom oil pitch, and the light constituent of extracting can be used as the high quality raw material that prepare carbon black.Then ethylene bottom oil pitch is carried out in reactor to thermal polycondensation, the softening temperature that improves ethylene bottom oil pitch is 200 ~ 225 ℃, then through luwa evaporator, pulling out the part light constituent, to make softening temperature be 270 ~ 285 ℃ of spinning asphalts.This method is continuous operation, and technical process is simple, and controllability is good, is applicable to suitability for industrialized production.Prepared spinning asphalt coking value is high, and the spinning properties excellence, more than continuous spinning length can reach ten thousand metres, even also fracture of wire can not occur in high rotating speed spinning.
Embodiment
Embodiment 1
After 110 ℃ of 350kg ethylene bottom oil preheatings, in 240 ℃ of temperature and vacuum tightness 90Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 85 ℃, coking value is 40% ethylene bottom oil pitch 130kg, then by ethylene bottom oil pitch dislocation reactor, with 3 ℃/min of temperature rise rate, be warming up to 340 ℃, constant temp. heating polycondensation 5 hours, the softening temperature that improves ethylene bottom oil pitch 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, string diameter is 16 μ m.
Embodiment 2
After 115 ℃ of 350kg ethylene bottom oil preheatings, in 245 ℃ of temperature and vacuum tightness 95Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 88 ℃, coking value is 43% ethylene bottom oil pitch 126kg, then by ethylene bottom oil pitch dislocation reactor, with 3 ℃/min of temperature rise rate, be warming up to 350 ℃, constant temp. heating polycondensation 4.5 hours, the softening temperature that improves ethylene bottom oil pitch 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, string diameter is 15 μ m.
Embodiment 3
After 110 ℃ of 350kg ethylene bottom oil preheatings, in 238 ℃ of temperature and vacuum tightness 85Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 80 ℃, coking value is 39% ethylene bottom oil pitch 135kg, then by ethylene bottom oil pitch dislocation reactor, with 4 ℃/min of temperature rise rate, be warming up to 360 ℃, constant temp. heating polycondensation 4.5 hours, the softening temperature that improves ethylene bottom oil pitch 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 350kg ethylene bottom oil preheatings, in 260 ℃ of temperature and vacuum tightness 105Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 95 ℃, coking value is 45% ethylene bottom oil pitch 124kg, then by ethylene bottom oil pitch dislocation reactor, with 4 ℃/min of temperature rise rate, be warming up to 350 ℃, constant temp. heating polycondensation 4 hours, the softening temperature that improves ethylene bottom oil pitch 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, string diameter is 15 μ m.
Embodiment 5
After 115 ℃ of 350kg ethylene bottom oil preheatings, in 250 ℃ of temperature and vacuum tightness 95Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 87 ℃, coking value is 43% ethylene bottom oil pitch 126kg, then by ethylene bottom oil pitch dislocation reactor, with 3 ℃/min of temperature rise rate, be warming up to 360 ℃, constant temp. heating polycondensation 5 hours, the softening temperature that improves ethylene bottom oil pitch 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, string diameter is 15 μ m.
Claims (1)
1. the preparation method of a petroleum high softening-point spinning asphalt, it is characterized in that comprising the following steps: ethylene bottom oil first is preheating to 80 ~ 120 ℃, then in 220 ~ 280 ℃ of temperature and vacuum tightness 80 ~ 120Pa wiped film vaporization, pull out light constituent, obtaining softening temperature is 80 ~ 100 ℃, coking value is 40 ~ 50% ethylene bottom oil pitch, by this softening temperature, it is 80 ~ 100 ℃, coking value is in 40 ~ 50% ethylene bottom oil pitch dislocation reactor, with 2 ~ 5 ℃/min of temperature rise rate, be warming up to 330 ~ 360 ℃, constant temp. heating polycondensation 4 ~ 6 hours, make softening temperature and be the ethylene bottom oil pitch of 200 ~ 225 ℃, this softening temperature is that the ethylene bottom oil pitch of 200 ~ 225 ℃ is pulled out the part light constituent in 340 ~ 370 ℃ of temperature and vacuum tightness 80 ~ 120Pa wiped film vaporization, final acquisition softening temperature is the spinning asphalt of 270 ~ 285 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102528431A CN102776014B (en) | 2012-07-20 | 2012-07-20 | Preparation method of petroleum-based high softening point spinning pitch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102528431A CN102776014B (en) | 2012-07-20 | 2012-07-20 | Preparation method of petroleum-based high softening point spinning pitch |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102776014A CN102776014A (en) | 2012-11-14 |
| CN102776014B true CN102776014B (en) | 2013-11-27 |
Family
ID=47121127
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102528431A Active CN102776014B (en) | 2012-07-20 | 2012-07-20 | Preparation method of petroleum-based high softening point spinning pitch |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102776014B (en) |
Families Citing this family (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 |
| CN111925818B (en) * | 2020-08-14 | 2021-03-12 | 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 |
| CN114149819B (en) * | 2021-12-01 | 2022-12-09 | 中国矿业大学(北京) | Method for increasing softening point temperature of asphalt and asphalt obtained by method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1245141A (en) * | 1998-08-18 | 2000-02-23 | 中国石油化工集团公司 | Process for preparing spinning asphalt used for high-performance carbon fibre |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5876523A (en) * | 1981-10-29 | 1983-05-09 | Nippon Oil Co Ltd | Preparation of pitch carbon fiber |
| US4497789A (en) * | 1981-12-14 | 1985-02-05 | Ashland Oil, Inc. | Process for the manufacture of carbon fibers |
| JPS60202189A (en) * | 1984-03-26 | 1985-10-12 | Idemitsu Kosan Co Ltd | Pitch for carbonaceous material and its preparation |
| JPS6234985A (en) * | 1985-08-08 | 1987-02-14 | Idemitsu Kosan Co Ltd | Production of pitch for carbonaceous material |
| US4996037A (en) * | 1985-09-13 | 1991-02-26 | Berkebile Donald C | Processes for the manufacture of enriched pitches and carbon fibers |
| US5429739A (en) * | 1992-08-25 | 1995-07-04 | Ashland Inc. | Pitch precursor production by distillation |
| CN1158415C (en) * | 2000-12-06 | 2004-07-21 | 辽阳石油化纤公司亿方化工实验二厂 | Prepn of petroleum asphalt-base common carbon fiber material |
| CN102391885A (en) * | 2011-09-22 | 2012-03-28 | 天津大学 | Coal tar pitch-based high-softening point spinning pitch and preparation method thereof |
-
2012
- 2012-07-20 CN CN2012102528431A patent/CN102776014B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1245141A (en) * | 1998-08-18 | 2000-02-23 | 中国石油化工集团公司 | Process for preparing spinning asphalt used for high-performance carbon fibre |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102776014A (en) | 2012-11-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102776014B (en) | Preparation method of petroleum-based high softening point spinning pitch | |
| CN102391885A (en) | Coal tar pitch-based high-softening point spinning pitch and preparation method thereof | |
| CN101838542B (en) | Manufacturing method of ultra-temperature pitch | |
| CN105887245B (en) | A kind of preparation method of continuous high-performance Mesophase Pitch-based Carbon Fibers | |
| CN105567275B (en) | A kind of production method for preparing high-purity high softening point bitumen | |
| WO2013104092A8 (en) | Process for producing mesophase pitch by hydrogenation of high-temperature coal tar | |
| Li et al. | Preparation of carbon fibers from low-molecular-weight compounds obtained from low-rank coal and biomass by solvent extraction | |
| CN103014919B (en) | Preparation method of general purpose pitch-based carbon fiber | |
| CN103122503A (en) | Preparation method of high-strength and high-modulus pitch-based fiber | |
| CN111718740B (en) | Spinnable mesophase pitch prepared by solvent synergistic hydrogenation, preparation method and application | |
| CN104946289B (en) | High-softening-point asphalt, and preparation method and application thereof | |
| CN103361096B (en) | Preparation method of high-softening-point asphalt for producing general-grade carbon fibers | |
| CN104388109B (en) | The preparation method of a kind of solvable mesophase pitch | |
| CN108611701A (en) | Graphene oxide modified pitch base carbon fibre production method | |
| CN107163971A (en) | A kind of continuous production method of pitch base carbon material feedstock | |
| CN103014918A (en) | Method for preparing coal-series general asphalt carbon fiber | |
| CN102839008A (en) | Purification method for coal tar soft pitch | |
| CN103184062A (en) | Preparation method of high softening point spinning pitch | |
| CN103952168A (en) | Method for preparing high-softening-point asphalt for general grade asphalt carbon fiber from coal tar pitch | |
| CN109504415B (en) | Production method of needle coke | |
| CN108221089A (en) | A kind of preparation method of asphalt base carbon fiber | |
| CN103965932A (en) | Treatment method for mixed asphalt as raw material for preparing needle coke | |
| CN110578188B (en) | Method for preparing spinnable asphalt by co-thermal polycondensation of acid anhydride modified coal asphalt and kerosene co-refining residue | |
| CN108048958A (en) | A kind of preparation method of coal tar pitch carbon fiber | |
| Yoo et al. | Properties of coal tar pitch modified with acid and oxidation treatment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |