CN101302434A - Process for preparing needle coke - Google Patents
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- CN101302434A CN101302434A CNA2008100171103A CN200810017110A CN101302434A CN 101302434 A CN101302434 A CN 101302434A CN A2008100171103 A CNA2008100171103 A CN A2008100171103A CN 200810017110 A CN200810017110 A CN 200810017110A CN 101302434 A CN101302434 A CN 101302434A
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Abstract
The invention provides a method for preparing needle coke. The method is as follows: after delayed coking treatment of fraction or residual oil which are rich in arene through a certain temperature rise formula, green coke obtained is calcined, and the needle coke with high intermediate phase content and developed needle structure are prepared. The petroleum raw materials used comprise mixture of one type or a plurality of types among virgin wax oil, coked wax oil, catalytic cracking clarified oil, ethylene tar, coal tar, dense oil, residual oil and other hydrocarbon-enriched substances. The delayed coking temperature rise formula is characterized in that: intermediate phases generated can be driven to grow fully and are flushed by air flow with enough flow rate before solidification, thereby the granularity of the needle coke prepared is large (the content of coke breeze is not more than 25 weight percent) and the needle coke can be used for large-scale steel-making electric furnaces. When the method is used for an industrial device, people only need to adjust the prior temperature rise formula according to the characteristics of the raw materials and the technological flow.
Description
Technical field
The invention belongs to a kind of preparation method of needle coke, more specifically, the present invention carries out delayed coking with one or more aromatic enriched fractions that derive from oil and coal tar and composition thereof, improve feeding temperature producing more gaseous products that can wash away intermediate phase voluntarily in the charging later stage, thereby obtain the advanced preparation technology of superpower and ultra high power needle coke.
Background technology
The preparation of needle coke is not only relevant with feedstock property, and closely related with the processing parameter of preparation, by adjusting these processing parameters, can improve this key index of thermal expansivity of needle coke greatly.United States Patent (USP) (USP4547284) is pointed out after delayed coking stops charging, injects high temperature inert gas and significantly promotes the interior temperature (improving 10 ℃) of coke drum, thereby reduce burnt thermal expansivity.Chinese patent CN1169911C then claims, when pyrogenic reaction, coke drum is sealed, the tower internal pressure constantly raises, pressure release and return to original pressure when treating that lift-off value reaches 0.2～1MPa, so repeatedly, wall pressure that the intermediate phase zone produces along air flow line when relying on pressure release and shearing force and take place to force to align, thus the needle coke of high-orientation obtained.
Aforesaid method is not all paid attention to abundant growth and these two key factors of tensile deformation subsequently of intermediate phase simultaneously, therefore is difficult for making the needle coke of excellent performance, the prosperity of needle-like Streamline Texture.
Summary of the invention
Purpose of the present invention is exactly the method that the needle coke of a kind of processability excellence, the prosperity of needle-like Streamline Texture is provided for the deficiency that overcomes the prior art existence.
The technical scheme that the present invention is taked for its purpose of realization comprises the steps:
(1) with the rich fragrant oil pumping of filtering solid impurity bottom to delayed coker fractionator, mix by weight 1: 0.05～1: 1 with online circulating stock, the gained compound is extracted out after the coking heater formula is warming up to 430～550 ℃ of heater outlet temperatures, enters coke drum then and finishes pyrogenic reaction;
(2) setting the delay coking process parameter is: 420～540 ℃ of coke drum temperature ins, input speed 10
-1～10
5Kghr
-1, recycle ratio 0.3～0.8, coke tower top pressure 0.1～2.0MPa (G), burnt 16～48 hours time is filled in charging, by 2 ℃ of hr
-1～5 ℃ of hr
-1Formula heats up, and treats to use instead when temperature rises to 460 ℃～500 ℃ 10 ℃ of hr
-1～15 ℃ of hr
-1Formula is warming up to 500 ℃～540 ℃ and stops to heat up and constant temperature 1～10 hour, and the needle-like green coke of generation is enriched in the coke drum;
(3) will send into the coking fractional distillation column separation from the oil gas product that the coke cat head is overflowed and obtain gas, gasoline and part of fraction of fuel-oil, remaining diesel oil distillate, gas oil and heavy ends are as online circulating stock.
(4) the needle-like green coke is placed in the calcining furnace, promptly obtains needle coke (ripe Jiao) through 1350～1460 ℃ of calcinings.
The rich fragrant oil product of aforesaid coking raw material is one or more the mixture in the rich fragrant logistics such as straight-run gas oil, wax tailings, fluid catalytic cracking decant oil, ethylene bottom oil, coal tar, viscous crude, residual oil.Filled burnt last 3～8 hours in charging in coke drum, the coke drum temperature in is increased to 500～540 ℃.In the coking boiler tube, can inject the high-temperature steam that accounts for fresh feed weight 0.1%～10.0%, also can inject the noncoking high temperature lighter hydrocarbons that account for fresh feed weight 10%～50%,, avoid heating up and the furnace tubing coking that may cause to increase mobile linear speed.
Because the rich fragrant oil product of coking raw material is that a class is formed complicated mixture, the green coke speed of each component differs bigger, same component green coke speed strengthens with the rising of coking temperature, therefore the alternating temperature charing by suitable formula can make the generating rate of coke be controlled at slower level, make the green coke speed under the low temperature mainly then contribute, thereby the abundant growth of piling up with intermediate phase needle-like green coke for the physics of liquid crystal original molecule create favorable conditions by green coke component at a slow speed by quick green coke component contribution high temperature green coke speed down.On the other hand, coking raw material is along with the carrying out of pyrogenic reaction, the ability of evolving gas product more and more a little less than, the gas flow that is produced in the coking later stage may be not enough so that obvious tensile deformation takes place in the intermediate phase zone that has become to grow up in early days, at this moment appropriate regulation coke drum temperature in improves coking temperature, can increase the gas yield of coking system, and bigger gas flow rate has the effect of washing away with tensile deformation to still uncured intermediate phase zone, just can obtain the needle-like green coke of streamline structure prosperity.The aciculiform structural development is good, can make that needle coke intensity is big, is difficult for being broken into finely powdered Jiao.
Embodiment
The present invention describes with following embodiment and Comparative Examples.
Embodiment 1: with coking raw material A (FCC clarified oil, asphalt content 0.5wt%, density 0.98gcm
-3, ash content 0.03wt%, aromatic hydrocarbon 75wt%, sulphur content 0.45wt%) be pumped into and carry out delayed coking, input speed 1kghr in the delayed coking coke drum
-1, coke drum tower top pressure 0.8MPa fills the burnt 36 hours time, recycle ratio 0.6, and coke drum inlet initial temperature is 430 ℃, then by 3 ℃ of hr
-1Carry out formula and heat up, treat to adopt when temperature is increased to 500 ℃ 15 ℃ of hr
-1Carrying out formula is warming up to 530 ℃ and stops to heat up and this temperature continuity 3hr is finished to coking test, obtain the needle-like green coke, green coke through 1400 ℃ of calcinings (in calcining furnace by the needle-like green coke be heated the volatile matter that discharges burning and finish calcining, calcination time is 0.1～1hr) to obtain needle coke, find that needle coke is flourishing fibre stream wire structure, thermal expansivity CTE is 2.08 * 10 after measured
-6℃
-1
Comparative Examples 1: coking raw material A is pumped into carries out delayed coking, input speed 1kghr in the delayed coking coke drum
-1, coke drum tower top pressure 0.8MPa fills the burnt 36 hours time, recycle ratio 0.6, and coke drum inlet initial temperature is 430 ℃, then by 3 ℃ of hr
-1Carrying out formula heats up, rise to 500 ℃ of constant temperature and this temperature continuity 3hr is arrived the coking test end, obtain the needle-like green coke, green coke through 1400 ℃ of calcinings (in calcining furnace by the needle-like green coke be heated the volatile matter that discharges burning and finish calcining, calcination time is 0.1～1hr) to obtain needle coke, find that needle coke part intermediate phase is spherical in shape, fibre stream wire structure is less-developed, and thermal expansivity CTE is 2.53 * 10 after measured
-6℃
-1
Embodiment 2: with coking raw material B (thermal cracking residue, asphalt content 0.5wt%, density 0.92gcm
-3, ash content＜0.01wt%, aromatic hydrocarbon 40wt%, sulphur content 0.20wt%) be pumped into and carry out delayed coking, input speed 1kghr in the delayed coking coke drum
-1, coke drum tower top pressure 1.2MPa fills the burnt 40 hours time, recycle ratio 0.5, and coke drum inlet initial temperature is 420 ℃, then by 2.5 ℃ of hr
-1Carry out formula and heat up, treat to adopt when temperature is increased to 490 ℃ 10 ℃ of hr
-1Carrying out formula is warming up to 520 ℃ of constant temperature and this temperature continuity 2hr is arrived the coking test end, obtain the needle-like green coke, green coke through 1400 ℃ of calcinings (in calcining furnace by the needle-like green coke be heated the volatile matter that discharges burning and finish calcining, calcination time is 0.1～1hr) to obtain needle coke, find that needle coke is relatively advanced fibre stream wire structure, thermal expansivity CTE is 2.17 * 10 after measured
-6℃
-1
Comparative Examples 2: coking raw material B is pumped into carries out delayed coking, input speed 1kghr in the delayed coking coke drum
-1, coke drum tower top pressure 1.2MPa fills the burnt 40 hours time, recycle ratio 0.5, and coke drum inlet initial temperature is 420 ℃, then by 2.5 ℃ of hr
-1Carrying out formula heats up, temperature is increased to 490 ℃ of constant temperature and this temperature continuity 2hr is arrived the coking test end, obtain the needle-like green coke, green coke through 1400 ℃ of calcinings (in calcining furnace by the needle-like green coke be heated the volatile matter that discharges burning and finish calcining, calcination time is 0.1～1hr) to obtain needle coke, find that needle coke part intermediate phase is spherical in shape, fibre stream wire structure is less-developed, and thermal expansivity CTE is 2.71 * 10 after measured
-6℃
-1
In the coking boiler tube, can inject the high-temperature steam that is no more than fresh feed weight 5wt%, also can inject the noncoking high temperature lighter hydrocarbons that are no more than fresh feed weight 30wt%,, avoid heating up and the furnace tubing coking that may cause to increase mobile linear speed.
The prosperity of the prepared needle coke fibre flow of the present invention structure, intensity is big, non-friable, fine powder is burnt few, and this method can directly apply to full scale plant, need not to change device hardware.
Claims (4)
1. the preparation method of a needle coke is characterized in that comprising the steps:
(1) with the rich fragrant oil pumping of filtering solid impurity bottom to delayed coker fractionator, mix by weight 1: 0.05～1: 1 with online circulating stock, the gained compound is extracted out after the coking heater formula is warming up to heater outlet temperature is 430～550 ℃, enters coke drum then and finishes pyrogenic reaction;
(2) setting the delay coking process parameter is: 420～540 ℃ of coke drum temperature ins, input speed 10
-1～10
5Kghr
-1, recycle ratio 0.3～0.8, coke tower top pressure 0.1～2.0MPa (G), burnt 16～48 hours time is filled in charging, by 2 ℃ of hr
-1～5 ℃ of hr
-1Formula heats up, and treats to use instead when temperature rises to 460 ℃～500 ℃ 10 ℃ of hr
-1～15 ℃ of hr
-1Formula is warming up to 500 ℃～540 ℃ and stops to heat up and constant temperature 1～10 hour, and the needle-like green coke of generation is enriched in the coke drum;
(3) will send into the coking fractional distillation column separation from the oil gas product that the coke cat head is overflowed and obtain gas, gasoline and part of fraction of fuel-oil, remaining diesel oil distillate, gas oil and heavy ends are as online circulating stock;
(4) the needle-like green coke is placed in the calcining furnace, promptly obtain needle coke through 1350～1460 ℃ of calcinings;
The rich fragrant oil product of aforesaid coking raw material is one or more the mixture in straight-run gas oil, wax tailings, fluid catalytic cracking decant oil, ethylene bottom oil, coal tar, viscous crude or the residual oil.
2. in accordance with the method for claim 1, it is characterized in that filling burnt last 3～8 hours, the coke drum temperature in is increased to 500～540 ℃ in charging in coke drum.
3. in accordance with the method for claim 1, it is characterized in that in the coking boiler tube, can injecting the high-temperature steam that accounts for fresh feed weight 0.1%～10.0%,, avoid heating up and the furnace tubing coking that may cause to increase mobile linear speed.
4. in accordance with the method for claim 1, it is characterized in that in the coking boiler tube, can injecting the noncoking high temperature lighter hydrocarbons that account for fresh feed weight 10%～50%,, avoid heating up and the furnace tubing coking that may cause to increase mobile linear speed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810017110A CN101302434B (en) | 2008-06-20 | 2008-06-20 | Process for preparing needle coke |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810017110A CN101302434B (en) | 2008-06-20 | 2008-06-20 | Process for preparing needle coke |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101302434A true CN101302434A (en) | 2008-11-12 |
| CN101302434B CN101302434B (en) | 2012-09-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810017110A Expired - Fee Related CN101302434B (en) | 2008-06-20 | 2008-06-20 | Process for preparing needle coke |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760221A (en) * | 2010-01-20 | 2010-06-30 | 中国科学院山西煤炭化学研究所 | Method for producing needle coke by non-delayed coking |
| CN102041011A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for preparing needle coke through still coking |
| CN102311800A (en) * | 2011-08-29 | 2012-01-11 | 云南昆钢煤焦化有限公司 | Modification method of coal tar pitch needle coke oily by product |
| CN102329637A (en) * | 2011-08-29 | 2012-01-25 | 云南昆钢煤焦化有限公司 | Intensive production method of coal tar pitch needle coke |
| CN102373080A (en) * | 2010-08-19 | 2012-03-14 | 中国石油化工股份有限公司 | Coking delaying method |
| CN102502581A (en) * | 2011-10-31 | 2012-06-20 | 中钢集团鞍山热能研究院有限公司 | Method for calcining low-volatile needle coke in rotary kiln |
| 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 |
| CN103045301A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Method for producing needle coke by catalytic cracking-delayed coking combination process |
| CN102021005B (en) * | 2009-08-20 | 2013-05-29 | 山东金诚重油化工有限公司 | Method for producing needle coke |
| CN103760053A (en) * | 2014-01-15 | 2014-04-30 | 中钢集团鞍山热能研究院有限公司 | Raw material evaluation method for guiding coking production of needle coke |
| CN104099124A (en) * | 2013-04-15 | 2014-10-15 | 中石化洛阳工程有限公司 | Test method for on-line circulation of delayed coking cycle oil |
| CN104560083A (en) * | 2014-12-30 | 2015-04-29 | 山东益大新材料有限公司 | Needle coke refined aromatic hydrocarbon oil |
| CN106635150A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Method for preparing needle-like coke through catalytic cracking-delayed coking combination process |
| CN106635143A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Needle-like coke preparation method |
| CN108219839A (en) * | 2018-01-02 | 2018-06-29 | 中和亚通能源科技有限公司 | A kind of needle coke production method and device |
| CN109777458A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of preparation method of high-quality needle coke |
| CN110066676A (en) * | 2019-04-24 | 2019-07-30 | 中国石油大学(华东) | A kind of continuous processing producing high-quality needle coke |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4547284A (en) * | 1982-02-16 | 1985-10-15 | Lummus Crest, Inc. | Coke production |
| CN1169911C (en) * | 2001-11-14 | 2004-10-06 | 中国科学院山西煤炭化学研究所 | Method for preparing needle coke |
| CN1323131C (en) * | 2004-03-31 | 2007-06-27 | 中国石油化工股份有限公司 | Delayed coking method for increasing coke strength |
-
2008
- 2008-06-20 CN CN200810017110A patent/CN101302434B/en not_active Expired - Fee Related
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021005B (en) * | 2009-08-20 | 2013-05-29 | 山东金诚重油化工有限公司 | Method for producing needle coke |
| CN102041011A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for preparing needle coke through still coking |
| CN102041011B (en) * | 2009-10-16 | 2014-08-20 | 中国石油化工股份有限公司 | Method for preparing needle coke through still coking |
| CN101760221A (en) * | 2010-01-20 | 2010-06-30 | 中国科学院山西煤炭化学研究所 | Method for producing needle coke by non-delayed coking |
| CN102373080A (en) * | 2010-08-19 | 2012-03-14 | 中国石油化工股份有限公司 | Coking delaying method |
| CN102311800B (en) * | 2011-08-29 | 2013-04-24 | 云南昆钢煤焦化有限公司 | Modification method of coal tar pitch needle coke oil by-product |
| CN102311800A (en) * | 2011-08-29 | 2012-01-11 | 云南昆钢煤焦化有限公司 | Modification method of coal tar pitch needle coke oily by product |
| CN102329637A (en) * | 2011-08-29 | 2012-01-25 | 云南昆钢煤焦化有限公司 | Intensive production method of coal tar pitch needle coke |
| CN102329637B (en) * | 2011-08-29 | 2013-04-24 | 云南昆钢煤焦化有限公司 | Intensive production method of coal tar pitch needle coke |
| 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 |
| CN103045301B (en) * | 2011-10-17 | 2014-10-22 | 中国石油化工股份有限公司 | Method for producing needle coke by catalytic cracking-delayed coking combination process |
| CN103045301A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Method for producing needle coke by catalytic cracking-delayed coking combination process |
| CN102502581A (en) * | 2011-10-31 | 2012-06-20 | 中钢集团鞍山热能研究院有限公司 | Method for calcining low-volatile needle coke in rotary kiln |
| CN104099124A (en) * | 2013-04-15 | 2014-10-15 | 中石化洛阳工程有限公司 | Test method for on-line circulation of delayed coking cycle oil |
| 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 |
| CN103760053A (en) * | 2014-01-15 | 2014-04-30 | 中钢集团鞍山热能研究院有限公司 | Raw material evaluation method for guiding coking production of needle coke |
| CN104560083A (en) * | 2014-12-30 | 2015-04-29 | 山东益大新材料有限公司 | Needle coke refined aromatic hydrocarbon oil |
| CN106635150A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Method for preparing needle-like coke through catalytic cracking-delayed coking combination process |
| CN106635143A (en) * | 2015-11-02 | 2017-05-10 | 中国石油化工股份有限公司 | Needle-like coke preparation method |
| CN106635150B (en) * | 2015-11-02 | 2018-02-09 | 中国石油化工股份有限公司 | Catalytic cracking delayed coking group technology prepares needle coke method |
| CN106635143B (en) * | 2015-11-02 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of method for preparing needle coke |
| CN109777458A (en) * | 2017-11-14 | 2019-05-21 | 中国石油化工股份有限公司 | A kind of preparation method of high-quality needle coke |
| CN108219839A (en) * | 2018-01-02 | 2018-06-29 | 中和亚通能源科技有限公司 | A kind of needle coke production method and device |
| CN108219839B (en) * | 2018-01-02 | 2024-04-09 | 亚通石化集团有限公司 | Needle coke production method and device |
| CN110066676A (en) * | 2019-04-24 | 2019-07-30 | 中国石油大学(华东) | A kind of continuous processing producing high-quality needle coke |
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