CN101942314A - Technology for producing needle coke by kettle-type coking - Google Patents
Technology for producing needle coke by kettle-type coking Download PDFInfo
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- CN101942314A CN101942314A CN2009100125063A CN200910012506A CN101942314A CN 101942314 A CN101942314 A CN 101942314A CN 2009100125063 A CN2009100125063 A CN 2009100125063A CN 200910012506 A CN200910012506 A CN 200910012506A CN 101942314 A CN101942314 A CN 101942314A
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Abstract
The invention discloses a technology for producing needle coke by kettle-type coking, comprising the following steps: filling raw oils into a coke still; heating slowly a system to 480-500 DEG C under system pressure of 1.0-2.0MPa; controlling appropriate gas emissions rate, keeping constant temperature for 2-6h when system temperature reaches 480-500 DEG C, and blowing in inert gas from the bottom of the coke still; and heating the system to 520-550 DEG C and continuously baking for 1-4h to generate the needle coke through reaction, wherein the obtained needle coke is deposited at the bottom of a coke tower. The technology of the invention has simple flow and small investment and can obtain the high-quality needle coke.
Description
Technical field
The present invention relates to a kind of processing method for preparing needle coke, specifically, is the method that adopts still formula coking process to produce needle coke, obtains byproduct light ends oil simultaneously.
Background technology
Needle coke is a main raw material of producing superpower, ultra-high power graphite electrode, and its economic worth is very high.At present, needle coke mainly adopts delay coking process production, selects suitable raw material, obtains needle coke under suitable delayed coking condition.When producing needle coke raw material generally had higher requirement, mainly concentrate on obtaining of raw material or system aspect about the needle coke production technology in the prior art, as CN00125962.8, CN200510073095.0 etc., few to needle coke preparation technology's improvement project itself.
CN01140582.1 discloses a kind of method for preparing needle coke, puts into raw material in tubular react furnace, charges into the rare gas element of 0.1-2MPa, and 2-30 internal heating second is to 480-550 ℃ coking temperature after sealing.After treating that system pressure surpasses the 0.2-1MPa of original pressure, promptly 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 the Reaktionsofen internal pressure is constant, continue coking 4-8 hour.Prepared needle coke has the streamlined optical texture of high-orientation.There is following deficiency in foregoing invention: (1) invention requires material to realize in industrial being difficult in 2～30s internal heating to 480～550 ℃; (2) invention proposes to adopt filling with inert gas in filling the reactor of raw material in advance, in reaction, discharge the method for preparing needle coke then, because rare gas element is merely able to be filled to the reactor upper space, can not be dissolved in the material, therefore discharge gas in the reaction process, flowing of rare gas element can not exert an influence to the order of intermediate phase; (3) react the later stage based on polyreaction, the reacted gas generating rate slows down, and is not enough to form enough wall pressure and shearing force, makes whole anisotropic zone force to align when air-flow is discharged.Therefore, this method obtains the further raising of product performance of needle coke.
Summary of the invention
At the deficiency of above-mentioned technology, the invention provides the processing method of the still formula coking production high quality needle-type coke that a kind of flow process is simple, investment is little.
The processing method of still formula coking production needle coke of the present invention comprises the steps:
(1) charging feedstock oil in the coking still, reacting system pressure is controlled to be 1.0～2.0MPa;
(2) reactive system is warming up to 480～500 ℃, and constant temperature 2～6 hours, when the reactive system gas production rate is not enough, goes into rare gas element from the coking still bottom blowing, and the free air delivery that makes reactive system by volume pitot meter reaches 0.02～1.0h
-1, free air delivery unit is volume and the stock oil volume ratio under the free air delivery standard state;
(3) after constant temperature finishes, stop to be blown into rare gas element, system is warming up to 520～550 ℃, burned 1～4h, and the needle coke that reaction generates is deposited at the bottom of the coking tower.
Reaction process discharging gas bag is drawn together through separating and can be obtained gas, benzoline, last running wet goods.
Stock oil can be coal tar or the coal-tar pitch of coal measures raw material as removing the objectionable constituent quinoline insolubles, also oil is raw material such as black petroleum products, ethylene bottom oil, catalytic cracking residual oil or thermal cracking residue, also can be that coal measures raw material and oil are the multipolymer of raw material.
Any gas of required rare gas element for not reacting in reactive system is as nitrogen, hydrogen, C
1-4Alkane etc. also can be mixed gass.
The principle of the inventive method 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.In the initial reaction stage process, system is based on 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, the effusion of gas makes mobile anisotropic 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; In reaction later stage process, system is based on polyreaction, have only a small amount of reacted gas to produce, slowly charge into the rare gas element compensation this moment at the bottom of coking still, make the anisotropic zone produce enough wall pressure and shearing force along air flow line, thereby form the intensive airflow scouring, thereby make whole anisotropic zone when air-flow is discharged, force to align, and then guaranteed quality product.
Embodiment
Embodiment 1
With catalytic cracking residual oil is raw material, and the coking still of packing into cuts out constant pressure valve, and system slowly heats up, and when treating that system pressure reaches 1.5MPa, regulates constant pressure valve, make system pressure constant in 1.5MPa, and pilot-gas is with 0.04h
-1Speed is discharged, when the slow temperature of system reaches 480 ℃, and constant temperature 3 hours, and go into inert nitrogen gas from the coking still bottom blowing, keeping discharging gas velocity is 0.05h
-1Constant temperature stops to be blown into rare gas element after finishing, and system is warming up to 520 ℃, burned 3h, and producing out oil as a trial is the needle coke product, its performance index are:
Volatile matter V, (wt%) 0.50
Ash content A, (wt%) 0.10
Sulphur content S, (wt%) 0.26
True specific gravity, (g/ml) 2.12
Long-width ratio K 2.04
Thermal expansivity CTE, (* 10
-6/ ℃) 0.94 (100-600 ℃)
Comparative example 1
According to embodiment 1 described method and operational condition, topping up not just, product property is as follows:
Volatile matter V, (wt%) 0.51
Ash content A, (wt%) 0.12
Sulphur content S, (wt%) 0.27
True specific gravity, (g/ml) 2.08
Long-width ratio K 1.54
Thermal expansivity CTE, (* 10
-6/ ℃) 1.18 (100-600 ℃)
Embodiment 2
With the coal tar of removing the objectionable constituent quinoline insolubles is raw material, and the coking still of packing into cuts out constant pressure valve, and system slowly heats up, and when treating that system pressure reaches 2.0MPa, regulates constant pressure valve, make system pressure constant in 2.0MPa, and pilot-gas is with 0.06h
-1Speed is discharged, when the slow temperature of system reaches 480 ℃, and constant temperature 4 hours, and go into rare gas element hydrogen from the coking still bottom blowing, keeping discharging gas velocity is 0.05h
-1Constant temperature stops to be blown into rare gas element after finishing, and system is warming up to 530 ℃, and burned 2h produces out the coal-based needle coke product as a trial, and its performance index are:
Volatile matter V, (wt%) 0.59
Ash content A, (wt%) 0.09
Sulphur content S, (wt%) 0.17
True specific gravity, (g/ml) 2.21
Long-width ratio K 2.06
Thermal expansivity CTE, (* 10
-6/ ℃) 0.93 (100-600 ℃)
Comparative example 2
According to embodiment 2 described method and operational conditions, topping up not just, product property is as follows:
Volatile matter V, (wt%) 0.56
Ash content A, (wt%) 0.11
Sulphur content S, (wt%) 0.20
True specific gravity, (g/ml) 2.15
Long-width ratio K 1.57
Thermal expansivity CTE, (* 10
-6/ ℃) 1.16 (100-600 ℃).
Claims (5)
1. the processing method of a still formula coking production needle coke comprises following content:
(1) charging feedstock oil in the coking still, reacting system pressure is controlled to be 1.0～2.0MPa;
(2) reactive system is warming up to 480～500 ℃, and constant temperature 2～6 hours, when the reactive system gas production rate is not enough, goes into rare gas element from the coking still bottom blowing, and the free air delivery that makes reactive system by volume pitot meter reaches 0.02～1.0h
-1
(3) after constant temperature finishes, stop to be blown into rare gas element, system is warming up to 520～550 ℃, burned 1～4h, and the needle coke that reaction generates is deposited at the bottom of the coking tower.
2. in accordance with the method for claim 1, it is characterized in that: stock oil is the coal measures raw material, or oil is raw material, or coal measures raw material and oil are the multipolymer of raw material.
3. in accordance with the method for claim 2, it is characterized in that: described coal measures raw material is coal tar or a coal-tar pitch of removing the objectionable constituent quinoline insolubles, and described oil is that raw material is black petroleum products, ethylene bottom oil, catalytic cracking residual oil or cracking-residuum.
4. it is characterized in that in accordance with the method for claim 1: any gas of described rare gas element in reactive system, not reacting.
5. according to claim 1 or 4 described methods, it is characterized in that: described rare gas element is nitrogen, hydrogen, C
1-4Alkane, or any mixed gas of above-mentioned gas.
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| CN 200910012506 CN101942314B (en) | 2009-07-09 | 2009-07-09 | Technology for producing needle coke by kettle-type coking |
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| CN 200910012506 CN101942314B (en) | 2009-07-09 | 2009-07-09 | Technology for producing needle coke by kettle-type coking |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045278A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Kettle-type method for preparing needle coke |
| CN103102890A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Process method for preparing needle coke through kettle type charring |
| CN103788977A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | Kettle-type method for preparing needle coke |
| 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 |
| CN106198133A (en) * | 2016-06-23 | 2016-12-07 | 中国石油大学(华东) | The device and method that quickly preparation simulation pipe is burnt |
| CN106403579A (en) * | 2016-10-21 | 2017-02-15 | 中国石油大学(华东) | Method for preparing high-quality needle cook electrode material from mesophase pitch |
| CN106635101A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Delay coking tower and method for preparing needle coke |
| CN108795462A (en) * | 2018-06-11 | 2018-11-13 | 中国石油大学(华东) | A kind of preparation method of high degree of order acicular petroleum coke |
| CN110018194A (en) * | 2019-04-12 | 2019-07-16 | 山东益大新材料有限公司 | A kind of reactive apparatus system of evaluation coking raw material and evaluation method |
| CN114381295A (en) * | 2022-01-17 | 2022-04-22 | 中国石油大学(华东) | Method for preparing high-quality carbon material by using tar |
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| 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 |
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| 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 |
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| 李太平等: "针状焦技术的研究进展", 《炭素》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045278A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Kettle-type method for preparing needle coke |
| CN103102890A (en) * | 2011-11-10 | 2013-05-15 | 中国石油化工股份有限公司 | Process method for preparing needle coke through kettle type charring |
| 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 |
| CN103788977A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | Kettle-type method for preparing 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 |
| CN106635101A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Delay coking tower and method for preparing needle coke |
| 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 |
| CN106198133A (en) * | 2016-06-23 | 2016-12-07 | 中国石油大学(华东) | The device and method that quickly preparation simulation pipe is burnt |
| CN106198133B (en) * | 2016-06-23 | 2018-11-20 | 中石油华东设计院有限公司 | The quickly device and method of preparation simulation pipe coke |
| CN106403579A (en) * | 2016-10-21 | 2017-02-15 | 中国石油大学(华东) | Method for preparing high-quality needle cook electrode material from mesophase pitch |
| CN108795462A (en) * | 2018-06-11 | 2018-11-13 | 中国石油大学(华东) | A kind of preparation method of high degree of order acicular petroleum coke |
| CN108795462B (en) * | 2018-06-11 | 2021-09-21 | 中国石油大学(华东) | Preparation method of high-order needle petroleum coke |
| CN110018194A (en) * | 2019-04-12 | 2019-07-16 | 山东益大新材料有限公司 | A kind of reactive apparatus system of evaluation coking raw material and evaluation method |
| CN114381295A (en) * | 2022-01-17 | 2022-04-22 | 中国石油大学(华东) | Method for preparing high-quality carbon material by using tar |
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