CN1169911C - Method for preparing needle coke - Google Patents
Method for preparing needle coke Download PDFInfo
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- CN1169911C CN1169911C CNB011405821A CN01140582A CN1169911C CN 1169911 C CN1169911 C CN 1169911C CN B011405821 A CNB011405821 A CN B011405821A CN 01140582 A CN01140582 A CN 01140582A CN 1169911 C CN1169911 C CN 1169911C
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Abstract
The present invention relates to a method for preparing needle-shaped coke. A raw material is put in a tube type reaction furnace, and inert gas of 0.1 to 2MPa is filled; the tube type reaction furnace is sealed and heated until the coking temperature of 480 to 550 DEG C is obtained in 2 to 30 seconds; after the pressure of a system is 0.2MPa to 1MPa higher than the original pressure, the gas is released, and the original pressure of 0.2 to 2MPa is obtained; the tube type reaction furnace is sealed again until the pressure in the reaction furnace is not higher than the original pressure of 0.2 to 1MPa; when the pressure in the reaction furnace is unchanged, the coking operation is continuously carried out for 4 to 8 hours. Needle-shaped coke prepared according to the method has a streamline optical structure with high degree of orientation. The method has the advantages of simple experimental facilities, convenient preparation, simple technology, time saving, labor saving, adjustable discharge pressure, etc.
Description
Technical field:
The invention belongs to a kind of method for preparing needle coke, relate in particular to and a kind ofly draw Jiao to prepare the method for needle coke by venting.
Background technology:
Needle coke is a main raw of producing ultra-high power graphite electrode.At present, the method for preparing needle coke is that raw material is directly carried out coking, as at document carbon[1989,27 (3): 375-380] in, the pitch that is rich in the pitch of naphthalene ring or has elevated oxygen level and enrich alkyl group side chain directly carries out coking under 500 ℃ and 0.8MPa, the former can make the needle coke with certain orientation in the coking scope of broad, the latter then needs just can make needle coke under suitable condition; Another method is to carrying out coking through the raw material after the thermal polycondensation modification, as at document Chemistry andphysics of carbon (1994,24:111) and carbon[1989,27 (3): 359-365] in, be with fluid catalytic cracking residual oil and low-sulfur oil vacuum resid with 5: 5 mixed after 460 ℃ of following coking, or under 480 ℃, carry out coking with 7: 3 ratio, make needle coke with certain streamlined structure.
Although aforesaid method can make needle coke, be difficult for making the needle coke of the streamlining optical texture with high-orientation of excellent performance.Because aforesaid method only is directly to carry out coking to raw material or through the raw material of modification, the effect that makes the gas that produced in the process of preparation needle coke produce to the growth of intermediate phase spherocrystal with to the pressure orientation in anisotropy zone when overflowing is limited.
Goal of the invention:
The purpose of this invention is to provide a kind of method for preparing needle coke.
Principle of the present invention is as follows: raw material produces mesophase ball after being heated to a certain degree.These mesophase balls form, increase, melt and process in, in the different steps reaction system, produce the gases of different amounts, the motion of gas has promoted the abundant growth of spherocrystal.These gases leave system with bubble form in reaction process, and the effusion of gas makes mobile anisotropy zone force to be orientated in order along air flow line, and these regional ordered arrangement are necessary to obtaining high quality needle-type coke.For this reason, the present invention designs after the reactor pressure predetermined fixed, is raised to temperature of reaction fast.Along with the rising pressure increase of temperature of reaction, also put aside a certain amount of gas in the system simultaneously.Venting decompression then makes the anisotropy zone produce wall pressure and shearing force along air flow line, thereby forms intensive airflow scouring power, thereby makes whole anisotropy zone force to align when air-flow is discharged.
Preparation method of the present invention comprises the steps:
(1) in tubular react furnace, puts into raw material, charge into rare gas element and the sealing of 0.2-2MPa in advance;
(2) at the coking temperature of 2-30 internal heating second to 480-550 ℃; After treating that system pressure surpasses the 0.2-1MPa of original pressure, disengage gas to original 0.2-2MPa, and then sealing, the pressure in Reaktionsofen no longer surpasses till the 0.2-1MPa of original pressure.
When (3) the Reaktionsofen internal pressure is constant, continue coking 4-8 hour.
Aforesaid raw material can be coal tar and the coal-tar pitch of coal measures raw material as removing the objectionable constituent quinoline insolubles; Also can be that oil is raw material such as black petroleum products, ethylene bottom oil, catalytic cracking residual oil and thermal cracking residue etc.; Can also be that coal measures raw material and oil are the multipolymer of raw material.
The present invention has following advantage:
1. prepared needle coke has the streamlining optical texture of high-orientation;
2. used experimental installation is simple, easy to make;
3. technology is simple, saves time, laborsaving;
4. blow off pressure is adjustable;
Embodiment:
Embodiment 1:
With coal measures flash oil and oil are housed is after the tubular react furnace of the multipolymer of slurry oil is inflated to 2MPa in advance, sealing.At utmost point short period of time internal heating to 530 ℃, boost certainly when pressure is raised to 3MPa then, begin to be deflated to original pressure 2MPa.When system pressure surpasses the 0.2MPa of original pressure, exit afterwards, till the pressure of system no longer rises, continue coking 5h subsequently and get final product.The optical texture of gained coke button is seen Fig. 1.Can find out that whole coke button is the streamlining optical texture based on the high-orientation of fiber.
Comparative Examples 1:
After will the system identical with embodiment 1 being inflated to 2MPa, be always under the 2MPa at the pressure that keeps system, carry out coking in 530 ℃ in the scorch time identical with embodiment 1, the optical texture of gained coke button is seen Fig. 1.Can find out that whole coke button is the not high wide area optical texture of orientation degree.
Embodiment 2:
With oil is housed is that the tubular react furnace of supercritical extraction slurry oil is inflated in advance and is inflated to 0.2MPa, then sealing and at utmost point short period of time internal heating to 480 ℃.Treat that the 0.5MPa that pressure surpasses virgin pressure promptly exits, all the other processes are with embodiment 1.Gained (see figure 3) as a result shows, draws burnt method can obtain the coke button of optical texture based on the high-orientation of fiber by venting.
Comparative Examples 2:
After will the system identical with embodiment 2 being inflated to 0.2MPa, at utmost point short period of time internal heating to 480 ℃, remain this pressure up to the scorch time identical with embodiment 2, the optical texture of gained coke button is seen Fig. 4.Can find out that whole coke button is the wide area optical texture.
Embodiment 3:
After the tubular react furnace that the polycondensate of coal measures flash oil is housed is inflated to 0.8MPa, sealing.At utmost point short period of time internal heating to 490 ℃, boost certainly when pressure is raised to 1.6MPa then, begin to be deflated to 0.8MPa, when system pressure surpasses 0.3MPa, exit afterwards, till the pressure of system no longer rises, continue coking 8h subsequently and get final product.The optical texture of gained coke button is seen Fig. 5.Can find out that whole coke button is the higher streamlining optical texture of orientation degree that contains fiber.
Comparative Examples 3:
After will the system identical being inflated to 0.8MPa, make the pressure of system remain 0.8MPa with embodiment 3.Carry out coking in the scorch time identical with embodiment 1, the optical texture of gained coke button is seen Fig. 6.Can find out that whole coke button is the wide area optical texture.
Embodiment 4:
After the tubular react furnace that thermal cracking residue is housed is inflated to 1.0MPa in advance, after boosting to 2.0MPa, begin to be deflated to original pressure, when surpassing 0.7MPa, system pressure exits afterwards, till the pressure of system no longer rises, continue coking 4h subsequently and get final product.The optical texture of gained coke button mainly is streamlined based on fine-fibered, sees Fig. 7.
Comparative Examples 4:
After will the system identical with embodiment 4 being inflated to 1.0MPa, carry out coking in the scorch time identical with embodiment 4, the optical texture of gained coke button is seen Fig. 8.Can find out that whole coke button is the not high wide area optical texture of orientation degree.
Claims (3)
1. method for preparing needle coke, its characteristics are that the preparation method comprises the steps:
(1) in tubular react furnace, puts into raw material, charge into rare gas element and the sealing of 0.2-2MPa;
(2) at the coking temperature of 2-30 internal heating second to 480-550 ℃; After treating that system pressure surpasses the 0.2-1MPa of original pressure, disengage gas to original 0.2-2MPa, and then sealing, the pressure in Reaktionsofen no longer surpasses till the 0.2-1MPa of original pressure;
When (3) the Reaktionsofen internal pressure is constant, continue coking 4-8 hour;
Described raw material is that coal measures raw material, oil are that raw material or coal measures raw material and oil are the multipolymer of raw material.
2. a kind of method for preparing needle coke as claimed in claim 1 is characterized in that described coal measures raw material is coal tar and a coal-tar pitch of removing the objectionable constituent quinoline insolubles.
3. a kind of method for preparing needle coke as claimed in claim 1 is characterized in that described oil is that raw material is black petroleum products, ethylene bottom oil, catalytic cracking residual oil and thermal cracking residue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011405821A CN1169911C (en) | 2001-11-14 | 2001-11-14 | Method for preparing needle coke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011405821A CN1169911C (en) | 2001-11-14 | 2001-11-14 | Method for preparing needle coke |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1418931A CN1418931A (en) | 2003-05-21 |
| CN1169911C true CN1169911C (en) | 2004-10-06 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB011405821A Expired - Fee Related CN1169911C (en) | 2001-11-14 | 2001-11-14 | Method for preparing needle coke |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4809675B2 (en) * | 2005-12-27 | 2011-11-09 | Ｊｘ日鉱日石エネルギー株式会社 | Petroleum coke and method for producing the same |
| CN101302434B (en) * | 2008-06-20 | 2012-09-26 | 中国石油大学(华东) | Process for preparing needle coke |
| CN101580242B (en) * | 2009-06-15 | 2011-03-16 | 太原理工大学 | Method for preparing needle coke by coal-tar asphalt |
| US20110044881A1 (en) * | 2009-08-21 | 2011-02-24 | Stansberry Peter G | Method For The Catalytic Extraction Of Coal |
| CN101776547B (en) * | 2010-01-20 | 2011-06-08 | 中国科学院山西煤炭化学研究所 | Method for easily and quickly evaluating needle coke |
| CN102634361B (en) * | 2011-02-10 | 2013-11-06 | 中国石油天然气股份有限公司 | Preparation method of acicular petroleum coke |
| CN103102890B (en) * | 2011-11-10 | 2014-04-16 | 中国石油化工股份有限公司 | Process method for preparing needle coke through kettle type charring |
| CN103509574B (en) * | 2012-06-19 | 2015-04-15 | 北京宝塔三聚能源科技有限公司 | Process for preparing high-quality coal-series needle-coke |
| CN103788977B (en) * | 2012-11-01 | 2015-04-01 | 中国石油化工股份有限公司 | Kettle-type method for preparing needle coke |
| CN103760053B (en) * | 2014-01-15 | 2016-04-27 | 中钢集团鞍山热能研究院有限公司 | A kind of raw material evaluation method instructing needle coke coking production |
| CN109181730B (en) * | 2018-09-30 | 2021-05-04 | 中国科学院山西煤炭化学研究所 | Method for preparing needle coke from kerosene co-refining residues |
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2001
- 2001-11-14 CN CNB011405821A patent/CN1169911C/en not_active Expired - Fee Related
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| CN1418931A (en) | 2003-05-21 |
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