CN102965132A - Method for preparing needle coke by magnetization reaction kettle - Google Patents
Method for preparing needle coke by magnetization reaction kettle Download PDFInfo
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- CN102965132A CN102965132A CN2012103028207A CN201210302820A CN102965132A CN 102965132 A CN102965132 A CN 102965132A CN 2012103028207 A CN2012103028207 A CN 2012103028207A CN 201210302820 A CN201210302820 A CN 201210302820A CN 102965132 A CN102965132 A CN 102965132A
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Abstract
The invention relates to a device and a method for preparation of needle coke. A magnetization reaction kettle comprises a reaction kettle body, which is equipped with a pressure release valve, a pressure gauge, and an inert gas inlet. The reaction kettle is mainly characterized in that magnetization device are symmetrically arranged on two sides of the reaction kettle body. The device and the method provided in the invention have the advantages that: (1) the system has a small pressure, easy controllability, and high security; (2) the prepared needle coke has a good needle structure, a low thermal expansion coefficient, and high strength; and (3) the prepared needle coke has significantly improved appearance and coking rate, and the graphitization property at the later period can be improved.
Description
Technical field
The present invention relates to a kind of device for preparing needle coke and preparation method thereof.
Background technology
Needle coke is mainly for the production of the blast furnace steel-making Graphite Electrodes, and the intensity of Graphite Electrodes, thermal shock resistance etc. largely depend on the needle coke performance.Because be subjected to the restriction of external STUDY OF NEEDLE COKE TECHNOLOGY fort, the U.S., Japan, Britain have monopolized the needle coke market of global 80-90%, and annual sales volume is limited.Domestic needle coke manufacturing enterprise does not also break through gordian technique at present, and the needle coke outward appearance of production, thermal expansivity, acicular structure, product strength, granularity aspect etc. are far away from overseas enterprise.
The processing method of tradition autoclave coking production needle coke, the stock oil of in coking still, packing into, reacting kettle inner pressure is controlled at 1.0-2.0MPa, and reactor temperature rises to 480-500 ℃, and constant temperature 2-6 hour, be blown into rare gas element from Polycondensation Reactor and Esterification Reactor, constant temperature stops to be blown into rare gas element after finishing, and is warming up to 520-550 ℃ again, constant temperature 1-4 hour, the needle coke that reaction is produced was deposited at the bottom of the coking tower.Have following deficiency: (1) in addition, considers higher this point of the higher requirement to reaction vessel of pressure although the needle coke intensity of producing under the 1.0-2.0MPa pressure is large, and acicular structure is bad, should reduce production pressure.(2) find that through test carbonization temperature is at 460 ℃ and 550 ℃, the coke of testing out there is no too large difference in appearance, and because the reduction of temperature also reduces for power consumption, and production cost also reduces accordingly thereupon, therefore, carbonization temperature need not be too high.
Summary of the invention
The object of the invention is to avoid the deficiencies in the prior art that a kind of magnetization reactor is provided.
Another purpose of the present invention provides a kind ofly uses described magnetization reactor to prepare the method for needle coke.
For achieving the above object, the technical scheme that the present invention takes is: a kind of magnetization reactor, include reaction kettle body, and be provided with pressure release valve at reaction kettle body, tensimeter, inert gas entrance, its principal feature is to be arranged with magnetizing assembly on the side of reaction kettle body.
Described magnetization reactor, described magnetizing assembly are electro-magnet, and magnetic induction density is 4-25mT.
Use described magnetization reactor to prepare the method for needle coke, it is characterized in that step is:
(1) magnetize pack in the reactor Catalytic Cracking Residual Oil or coal tar, reacting kettle inner pressure is controlled at 0.3-1.0MPa;
(2) the magnetization reactor was warming up to 400-420 ℃ in 1-2 hour, and constant temperature 2-3 hour, emission gases, when temperature in the kettle reaches 420-450 ℃, constant temperature 10-12 hour, when the still internal pressure is lower than 0.3-1.0MPa, enter rare gas element from the still bottom blowing, speed is 20-40ml/min;
(3) after constant temperature finishes, stop to be blown into rare gas element, continue to be heated to 450-470 ℃, constant temperature coking 2-3 hour.
The inventive method has promoted the coking power of needle coke, effectively improves its aciculiform structure, has reduced the average crystallite size of needle coke, has improved the graphitization characteristic in later stage.
Principle of the present invention is as follows: stock oil 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.In the initial reaction stage process, system is as main take cracking reaction, the motion of reacted gas has promoted the abundant growth of spherocrystal, reacted gas leaves system with the form of bubble, under certain pressure fitted, by the reactor external magnetic field middle phase condensed ring fragrance plane macromole is aligned, along with the mesophase pitch molecule constantly solidifies in ordered arrangement, thereby progressively form raphioid fiber, simultaneously in reaction later stage process, at the bottom of coking still, slowly pour the rare gas element compensation, make every irregular shaped region produce enough wall pressure and shearing force along air flow line, form strong airflow scouring, make whole anisotropy zone when air-flow is discharged, force to align, and then guaranteed quality product.
Beneficial effect of the present invention is:
(1) system pressure is little, and control is safe easily;
(2) the needle coke acicular structure of preparation is good, and thermal expansivity is low, and intensity is high.
(3) needle coke of preparation is significantly improved from exterior appearance and coking power, has improved the graphitization characteristic in later stage.
Description of drawings
Fig. 1 is structural representation of the present invention.
Embodiment
Below in conjunction with accompanying drawing principle of the present invention and feature are described, institute gives an actual example and only is used for explaining the present invention, is not be used to limiting scope of the present invention.
Embodiment 1: a kind of magnetization reactor, include reaction kettle body 1, and be provided with pressure release valve 2 at reaction kettle body 1, tensimeter 3, inert gas entrance 4 is arranged with magnetizing assembly 5 on the side of reaction kettle body 1.Described magnetizing assembly is electro-magnet, and magnetic induction density is 4mT.
Embodiment 2: a kind of magnetization reactor, described magnetizing assembly are electro-magnet, and magnetic induction density is 15mT.All the other structures are identical with embodiment 1.
Embodiment 3: a kind of magnetization reactor, described magnetizing assembly are electro-magnet, and magnetic induction density is 25mT.All the other structures are identical with embodiment 1.
Embodiment 4: use embodiment 1 described magnetization reactor to prepare the method for needle coke, it is characterized in that step is:
(1) magnetize the Catalytic Cracking Residual Oil of packing in the reactor, reacting kettle inner pressure is controlled at 0.4MPa;
(2) the magnetization reactor was warming up to 400 ℃ in 1 hour, constant temperature 2 hours, and emission gases, when temperature in the kettle reached 430 ℃, constant temperature 11 hours when the still internal pressure is lower than 0.4MPa, entered rare gas element from the still bottom blowing, and speed is 20ml/min;
(3) after constant temperature finishes, stop to be blown into rare gas element, continue to be heated to 460 ℃, constant temperature coking 2.5 hours.
The needle coke performance of producing is as follows:
Embodiment 5: use embodiment 2 described magnetization reactors to prepare the method for needle coke, it is characterized in that step is:
(1) magnetize the Catalytic Cracking Residual Oil of packing in the reactor, reacting kettle inner pressure is controlled at 0.8MPa;
(2) the magnetization reactor was warming up to 420 ℃ in 2 hours, constant temperature 2.5 hours, and emission gases, when temperature in the kettle reached 420 ℃, constant temperature 12 hours when the still internal pressure is lower than 0.8MPa, entered rare gas element from the still bottom blowing, and speed is 30ml/min;
(3) after constant temperature finishes, stop to be blown into rare gas element, continue to be heated to 450 ℃, constant temperature coking 3 hours.
The needle coke performance of producing is as follows:
Embodiment 6: use embodiment 3 described magnetization reactors to prepare the method for needle coke, it is characterized in that step is:
(1) the magnetization quinoline insolubles of packing in the reactor is 0 coal tar, and reacting kettle inner pressure is controlled at 0.95MPa;
(2) the magnetization reactor was warming up to 420 ℃ in 2 hours, constant temperature 3 hours, and emission gases, when temperature in the kettle reached 450 ℃, constant temperature 10 hours when the still internal pressure is lower than 0.95MPa, entered rare gas element from the still bottom blowing, and speed is 40ml/min;
(3) after constant temperature finishes, stop to be blown into rare gas element, continue to be heated to 470 ℃, constant temperature coking 2 hours.
The needle coke performance of producing is as follows:
Comparative Examples: number of patent application is 200910012506
Take the coal tar of removing the objectionable constituent quinoline insolubles as raw material, the reactor of packing into cuts out constant pressure valve, slowly heats up, and when reactor pressure reaches 2.0MPa, regulates constant pressure valve, makes constant pressure at 2.0MPa, and control gas is with 0.06h
-1Speed get rid of, when reactor temperature reaches 480 ℃, constant temperature 4 hours, and be blown into rare gas element hydrogen from Polycondensation Reactor and Esterification Reactor, keeping Exhaust Gas speed is 0.05h
-1Constant temperature stops to be blown into rare gas element after finishing, and is warming up to 530 ℃, and the coal-based needle coke product is produced out in coking 2 hours as a trial, and its performance index are:
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. a magnetization reactor includes reaction kettle body, is provided with pressure release valve at reaction kettle body, tensimeter, and inert gas entrance is characterized in that being arranged with magnetizing assembly on the side of reaction kettle body.
2. magnetization reactor as claimed in claim 1 is characterized in that described magnetizing assembly is electro-magnet, and magnetic induction density is 4-25mT.
3. use magnetization reactor as claimed in claim 1 to prepare the method for needle coke, it is characterized in that step is:
(1) magnetize pack in the reactor Catalytic Cracking Residual Oil or coal tar, the still internal pressure is controlled at 0.3-1.0MPa;
(2) the magnetization reactor was warming up to 400-420 ℃ in 1-2 hour, and constant temperature 2-3 hour, emission gases, when temperature in the kettle reaches 420-450 ℃, constant temperature 10-12 hour, when the still internal pressure is lower than 0.3-1.0MPa, enter rare gas element from the still bottom blowing, speed is 20-40ml/min;
(3) after constant temperature finishes, stop to be blown into rare gas element, continue to be heated to 450-470 ℃, constant temperature coking 2-3 hour.
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| CN2012103028207A CN102965132A (en) | 2012-08-23 | 2012-08-23 | Method for preparing needle coke by magnetization reaction kettle |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195072A (en) * | 2015-08-10 | 2015-12-30 | 刘焰琼 | Reaction kettle |
| CN105950206A (en) * | 2016-06-13 | 2016-09-21 | 中国石油大学(华东) | Device and method for simulating carbon-base macromolecule delayed coking process to achieve quick coking and coke forming |
| CN108067173A (en) * | 2016-11-14 | 2018-05-25 | 深圳市红莓生物科技有限公司 | A kind of inductive reaction equipment |
| CN112614984A (en) * | 2020-12-25 | 2021-04-06 | 湖州凯金新能源科技有限公司 | Graphite negative electrode material of low-magnetism substance for lithium battery and preparation method thereof |
| CN112635739A (en) * | 2020-12-25 | 2021-04-09 | 湖州凯金新能源科技有限公司 | Graphite material with long-cycle characteristic for lithium battery and preparation method thereof |
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| CN2300790Y (en) * | 1997-01-06 | 1998-12-16 | 茂名市水东开发区燃气技术发展中心 | Storage equipment for gas-making by exciting petroleum liquid hydrocarbon molecule |
| CN1418930A (en) * | 2001-11-14 | 2003-05-21 | 中国科学院山西煤炭化学研究所 | Method for preparing needle coke using petrolium and coal series raw material |
| CN201832651U (en) * | 2010-10-25 | 2011-05-18 | 山东科技大学 | Hydrothermal reaction kettle with additional magnetic field |
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2012
- 2012-08-23 CN CN2012103028207A patent/CN102965132A/en active Pending
Patent Citations (3)
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| CN2300790Y (en) * | 1997-01-06 | 1998-12-16 | 茂名市水东开发区燃气技术发展中心 | Storage equipment for gas-making by exciting petroleum liquid hydrocarbon molecule |
| CN1418930A (en) * | 2001-11-14 | 2003-05-21 | 中国科学院山西煤炭化学研究所 | Method for preparing needle coke using petrolium and coal series raw material |
| CN201832651U (en) * | 2010-10-25 | 2011-05-18 | 山东科技大学 | Hydrothermal reaction kettle with additional magnetic field |
Non-Patent Citations (1)
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| 赵世贵 等: "磁场作用下有序针状焦的制备", 《炭素技术》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195072A (en) * | 2015-08-10 | 2015-12-30 | 刘焰琼 | Reaction kettle |
| CN105195072B (en) * | 2015-08-10 | 2018-06-19 | 乳源瑶族自治县永恒实业有限公司 | A kind of reaction kettle |
| CN105950206A (en) * | 2016-06-13 | 2016-09-21 | 中国石油大学(华东) | Device and method for simulating carbon-base macromolecule delayed coking process to achieve quick coking and coke forming |
| CN108067173A (en) * | 2016-11-14 | 2018-05-25 | 深圳市红莓生物科技有限公司 | A kind of inductive reaction equipment |
| CN112614984A (en) * | 2020-12-25 | 2021-04-06 | 湖州凯金新能源科技有限公司 | Graphite negative electrode material of low-magnetism substance for lithium battery and preparation method thereof |
| CN112635739A (en) * | 2020-12-25 | 2021-04-09 | 湖州凯金新能源科技有限公司 | Graphite material with long-cycle characteristic for lithium battery and preparation method thereof |
| CN112614984B (en) * | 2020-12-25 | 2022-11-11 | 湖州凯金新能源科技有限公司 | Graphite negative electrode material of low-magnetism substance for lithium battery and preparation method thereof |
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Application publication date: 20130313 |