CN103184062A - Preparation method of high softening point spinning pitch - Google Patents
Preparation method of high softening point spinning pitch Download PDFInfo
- Publication number
- CN103184062A CN103184062A CN2013101146472A CN201310114647A CN103184062A CN 103184062 A CN103184062 A CN 103184062A CN 2013101146472 A CN2013101146472 A CN 2013101146472A CN 201310114647 A CN201310114647 A CN 201310114647A CN 103184062 A CN103184062 A CN 103184062A
- Authority
- CN
- China
- Prior art keywords
- spinning
- temperature
- pitch
- preparation
- high softening
- 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.)
- Pending
Links
Landscapes
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a preparation method of high softening point spinning pitch, and belongs to the technical field of spinning pitch. The preparation method comprises the following steps: knifing, evaporating and cutting part of light components of coal tar pitch subjected to primary quinoline insoluble removal under the conditions that the temperature is 370-410 DEG C, and the vacuum degree is 10-40 Pa to obtain refined pitch; rising the temperature to be 380-420 DEG C at the temperature rising rate of 1-2 DEG C/min, polycondensing the obtained refined pitch for 3-7 hours in a reaction kettle at a constant temperature; and knifing, evaporating and removing the light components of the polycondensed coal tar pitch under the conditions that the temperature is 350-370 DEG C, an the vacuum degree is 90-130 Pa, and cooling to the room temperature to obtain the spinning pitch with high softening point of 260-275 DEG C. The preparation method has the advantages as follows: the method is in continuous operation, simple in technological process, good in controllability, and suitable for industrial production. The spinning pitch prepared is excellent in spinning performance, and yarn break is not caused in the process of spinning at a high rotating speed, and the continuous spinning length can reach more than 15,000 m.
Description
Technical field
The present invention relates to a kind of preparation method of 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, is sent out the manufacturing process of understanding 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.Obtained certain achievement in research, but pitch-based carbon fiber does not still form throughput yet.
In the production method of patent CN101624730A coal-tar pitch based carbon fiber, it directly is raw material with the coal, make spinning asphalt through pulverized coal preparation workshop section, pitch extracting workshop section, pitch filtration workshop section, hair pitch evaporation desolventizing workshop section, hydrofining workshop section, the technical process complexity, higher to equipment requirements.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high softening-point spinning asphalt, this method has the advantages that technical process is simple, operation is continuous, controllability is good, be fit to suitability for industrialized production.
The present invention is realized that by the following technical programs a kind of preparation method of high softening-point spinning asphalt is characterized in that may further comprise the steps:
The coal-tar pitch wiped film vaporization cut-out light constituent under 370 ~ 410 ℃ of temperature and vacuum tightness 10 ~ 40Pa condition that removes primary quinoline insolubles is obtained refined asphaltic bitumen, again with the refined asphaltic bitumen that obtains in reactor, be that 1 ~ 2 ℃/min is warmed up to 380 ~ 420 ℃ with temperature rise rate, constant temperature thermal polycondensation 3 ~ 7 hours, then the wiped film vaporization under 350 ~ 370 ℃ of temperature and vacuum tightness 90 ~ 130Pa condition of the coal-tar pitch after the polycondensation is pulled out light constituent, being cooled to room temperature, to obtain high softening-point be 260 ~ 275 ℃ spinning asphalt.
Advantage of the present invention and effect are as follows: the present invention is that the coal-tar pitch that will remove primary quinoline insolubles is earlier made with extra care through wiped film vaporization, improve the softening temperature (200 ~ 230 ℃) of coal-tar pitch then by thermal polycondensation, and do not destroy the spinning property of coal-tar pitch, and then to pull out softening temperature through luwa evaporator be that to make softening temperature be 260 ~ 275 ℃ of spinning asphalts for the light constituent of 200 ~ 230 ℃ of coal-tar pitches.This method is continuous operation, and technical process is simple, and controllability is good, is fit to suitability for industrialized production.Fracture of wire can not take place in high rotating speed spinning in prepared spinning asphalt spinning properties excellence yet, and continuous spinning length can reach more than 15000 meters.
Embodiment
Embodiment 1
With remove primary quinoline insolubles reach contain 0.1% coal-tar pitch 1000g wiped film vaporization cut-out light constituent under 380 ℃ of temperature and vacuum tightness 15Pa condition and obtain 78 ℃ of refined asphaltic bitumen 800g(softening temperatures, coking value 53.6%).Get refined asphaltic bitumen 400g and put into reactor, to be 1.5 ℃/min be warmed up to 400 ℃ of constant temperature with reactor carried out thermal polycondensation in 4 hours and handle with temperature rise rate, then the coal-tar pitch after the polycondensation is pulled out the part light constituent in 350 ℃ of temperature and vacuum tightness 110Pa wiped film vaporization, obtain high softening-point spinning asphalt 160g.Softening temperature is 273 ℃.Carry out spinning with this spinning asphalt, the spinning rotating speed is 1450r/min, long 15500 meters of continuous spinning, and the silk footpath is 14 μ m.
Embodiment 2
With remove primary quinoline insolubles reach contain 0.1% coal-tar pitch 1000g wiped film vaporization cut-out light constituent under 385 ℃ of temperature and vacuum tightness 25Pa condition and obtain 80 ℃ of refined asphaltic bitumen 790g(softening temperatures, coking value 56.8%).Get refined asphaltic bitumen 400g and put into reactor, to be 2 ℃/min be warmed up to 400 ℃ of constant temperature with reactor carried out thermal polycondensation in 6 hours and handle with temperature rise rate, then the coal-tar pitch after the polycondensation is pulled out the part light constituent in 360 ℃ of temperature and vacuum tightness 117Pa wiped film vaporization, obtain high softening-point spinning asphalt 150g.Softening temperature is 278 ℃.Carry out spinning with this spinning asphalt, the spinning rotating speed is 1450r/min, long 15200 meters of continuous spinning, and the silk footpath is 15 μ m.
Embodiment 3
With remove primary quinoline insolubles reach contain 0.1% coal-tar pitch 1000g wiped film vaporization cut-out light constituent under 400 ℃ of temperature and vacuum tightness 15Pa condition and obtain 84 ℃ of refined asphaltic bitumen 770g(softening temperatures, coking value 58.1%).Get refined asphaltic bitumen 400g and put into reactor, to be 1.5 ℃/min be warmed up to 405 ℃ of constant temperature with reactor carried out thermal polycondensation in 5.5 hours and handle with temperature rise rate, then the coal-tar pitch after the polycondensation is pulled out the part light constituent in 365 ℃ of temperature and vacuum tightness 112Pa wiped film vaporization, obtain high softening-point spinning asphalt 155g.Softening temperature is 270 ℃.Carry out spinning with this spinning asphalt, the spinning rotating speed is 1350r/min, long 14000 meters of continuous spinning, and the silk footpath is 14 μ m.
Embodiment 4
With remove primary quinoline insolubles reach contain 0.1% coal-tar pitch 1000g wiped film vaporization cut-out light constituent under 390 ℃ of temperature and vacuum tightness 25Pa condition and obtain 82 ℃ of refined asphaltic bitumen 786g(softening temperatures, coking value 57.4%).Get refined asphaltic bitumen 400g and put into reactor, to be 2.0 ℃/min be warmed up to 400 ℃ of constant temperature with reactor carried out thermal polycondensation in 5.5 hours and handle with temperature rise rate, then the coal-tar pitch after the polycondensation is pulled out the part light constituent in 360 ℃ of temperature and vacuum tightness 110Pa wiped film vaporization, obtain high softening-point spinning asphalt 157g.Softening temperature is 275 ℃.Carry out spinning with this spinning asphalt, the spinning rotating speed is 1350r/min, long 14500 meters of continuous spinning, and the silk footpath is 15 μ m.
Embodiment 5
With remove primary quinoline insolubles reach contain 0.1% coal-tar pitch 1000g wiped film vaporization cut-out light constituent under 405 ℃ of temperature and vacuum tightness 10Pa condition and obtain 82 ℃ of refined asphaltic bitumen 790g(softening temperatures, coking value 58.1%).Get refined asphaltic bitumen 400g and put into reactor, to be 1.5 ℃/min be warmed up to 405 ℃ of constant temperature with reactor carried out thermal polycondensation in 4 hours and handle with temperature rise rate, then the coal-tar pitch after the polycondensation is pulled out the part light constituent in 365 ℃ of temperature and vacuum tightness 95Pa wiped film vaporization, obtain high softening-point spinning asphalt 160g.Softening temperature is 268 ℃.Carry out spinning with this spinning asphalt, the spinning rotating speed is 1450r/min, long 15500 meters of continuous spinning, and the silk footpath is 15 μ m.
Embodiment 6
With remove primary quinoline insolubles reach contain 0.1% coal-tar pitch 1000g wiped film vaporization cut-out light constituent under 390 ℃ of temperature and vacuum tightness 12Pa condition and obtain 79 ℃ of refined asphaltic bitumen 796g(softening temperatures, coking value 54.1%).Get refined asphaltic bitumen 400g and put into reactor, to be 1.5 ℃/min be warmed up to 410 ℃ of constant temperature with reactor carried out thermal polycondensation in 4 hours and handle with temperature rise rate, then the coal-tar pitch after the polycondensation is pulled out the part light constituent in 355 ℃ of temperature and vacuum tightness 100Pa wiped film vaporization, obtain high softening-point spinning asphalt 156g.Softening temperature is 270 ℃.Carry out spinning with this spinning asphalt, the spinning rotating speed is 1300r/min, long 14000 meters of continuous spinning, and the silk footpath is 14 μ m.
Claims (1)
1. the preparation method of a high softening-point spinning asphalt, it is characterized in that may further comprise the steps: coal-tar pitch wiped film vaporization cut-out light constituent under 370 ~ 410 ℃ of temperature and vacuum tightness 10 ~ 40Pa condition that will remove primary quinoline insolubles obtains refined asphaltic bitumen, again with the refined asphaltic bitumen that obtains in reactor, be that 1 ~ 2 ℃/min is warmed up to 380 ~ 420 ℃ with temperature rise rate, constant temperature thermal polycondensation 3 ~ 7 hours, then the wiped film vaporization under 350 ~ 370 ℃ of temperature and vacuum tightness 90 ~ 130Pa condition of the coal-tar pitch after the polycondensation is pulled out light constituent, being cooled to room temperature, to obtain high softening-point be 260 ~ 275 ℃ spinning asphalt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101146472A CN103184062A (en) | 2013-04-03 | 2013-04-03 | Preparation method of high softening point spinning pitch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101146472A CN103184062A (en) | 2013-04-03 | 2013-04-03 | Preparation method of high softening point spinning pitch |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103184062A true CN103184062A (en) | 2013-07-03 |
Family
ID=48675513
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101146472A Pending CN103184062A (en) | 2013-04-03 | 2013-04-03 | Preparation method of high softening point spinning pitch |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103184062A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593033A (en) * | 2015-01-12 | 2015-05-06 | 中钢集团鞍山热能研究院有限公司 | Preparation method of high-performance environment-friendly asphalt |
| CN104790069A (en) * | 2015-04-24 | 2015-07-22 | 中国科学院山西煤炭化学研究所 | Pre-processing method for asphalt stock for spinning |
| CN114410331A (en) * | 2022-03-09 | 2022-04-29 | 中国石油大学(华东) | Method for preparing spinnable mesophase pitch with low cost |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4606808A (en) * | 1983-04-22 | 1986-08-19 | Director-General Of The Agency Of Industrial Science & Technology | Method for the preparation of pitches for spinning carbon fibers |
| CN1030799A (en) * | 1987-07-21 | 1989-02-01 | 迪迪尔工程有限公司 | The production method of anisotropy carbon fiber and device |
| 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 |
| CN102776014A (en) * | 2012-07-20 | 2012-11-14 | 天津大学 | Preparation method of petroleum-based high softening point spinning pitch |
-
2013
- 2013-04-03 CN CN2013101146472A patent/CN103184062A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4606808A (en) * | 1983-04-22 | 1986-08-19 | Director-General Of The Agency Of Industrial Science & Technology | Method for the preparation of pitches for spinning carbon fibers |
| CN1030799A (en) * | 1987-07-21 | 1989-02-01 | 迪迪尔工程有限公司 | The production method of anisotropy carbon fiber and device |
| 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 |
| CN102776014A (en) * | 2012-07-20 | 2012-11-14 | 天津大学 | Preparation method of petroleum-based high softening point spinning pitch |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104593033A (en) * | 2015-01-12 | 2015-05-06 | 中钢集团鞍山热能研究院有限公司 | Preparation method of high-performance environment-friendly asphalt |
| CN104593033B (en) * | 2015-01-12 | 2018-05-08 | 中钢集团鞍山热能研究院有限公司 | A kind of preparation method of high-performance environment-friendly pitch |
| CN104790069A (en) * | 2015-04-24 | 2015-07-22 | 中国科学院山西煤炭化学研究所 | Pre-processing method for asphalt stock for spinning |
| CN114410331A (en) * | 2022-03-09 | 2022-04-29 | 中国石油大学(华东) | Method for preparing spinnable mesophase pitch with low cost |
| CN114410331B (en) * | 2022-03-09 | 2022-10-25 | 中国石油大学(华东) | Method for preparing spinnable mesophase pitch with low cost |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102391885A (en) | Coal tar pitch-based high-softening point spinning pitch and preparation method thereof | |
| CN102776014B (en) | Preparation method of petroleum-based high softening point spinning pitch | |
| CN103184062A (en) | Preparation method of high softening point spinning pitch | |
| CN105567275B (en) | A kind of production method for preparing high-purity high softening point bitumen | |
| CN103361096B (en) | Preparation method of high-softening-point asphalt for producing general-grade carbon fibers | |
| CN102732280A (en) | High-softening-point coal-tar pitch production method | |
| CN102690672A (en) | Preparing method for coal tar refined pitch | |
| Yoo et al. | Modification of isotropic coal-tar pitch by acid treatments for carbon fiber melt-spinning | |
| CN103740400A (en) | Method for preparing high-quality needle coke raw material by removing QI (Quinoline Insolubles) in coal tar | |
| CN107163971A (en) | A kind of continuous production method of pitch base carbon material feedstock | |
| CN106398736A (en) | Preparation method of mesophase pitch | |
| CN106190211A (en) | A kind of method preparing high-purity dipping agent bitumen | |
| CN103014918A (en) | Method for preparing coal-series general asphalt carbon fiber | |
| CN102674265A (en) | Method for producing insoluble sulfur by one-step water method | |
| CN103923681A (en) | Intermediate-phase asphalt and method for preparing intermediate-phase asphalt from coal liquefaction refined asphalt | |
| CN109423318A (en) | After Atmospheric vacuum plus alkali directly produces the coal tar deep processing technique of crude naphthalene | |
| CN108221089A (en) | A kind of preparation method of asphalt base carbon fiber | |
| CN102704042A (en) | Method for preparing pitch-based carbon fiber | |
| CN102703104B (en) | Production method for low-QI (Quality Index) coal pitch | |
| CN110408418B (en) | Preparation method of high-regular-carbon microcrystalline pitch coke | |
| CN103965932A (en) | Treatment method for mixed asphalt as raw material for preparing needle coke | |
| CN102504853A (en) | Method for preparing high softening point asphalt for producing carbon fibers | |
| CN113604241B (en) | Method for preparing needle coke by medium-low temperature coal tar pitch composite extraction modification | |
| CN103952168A (en) | Method for preparing high-softening-point asphalt for general grade asphalt carbon fiber from coal tar pitch | |
| BR112015004326A2 (en) | improved carbon electrode fabrication |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130703 |