CN101724421B - Production method of needle coke - Google Patents

Production method of needle coke Download PDF

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Publication number
CN101724421B
CN101724421B CN 200810228427 CN200810228427A CN101724421B CN 101724421 B CN101724421 B CN 101724421B CN 200810228427 CN200810228427 CN 200810228427 CN 200810228427 A CN200810228427 A CN 200810228427A CN 101724421 B CN101724421 B CN 101724421B
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coking
raw
oil
needle
coke
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CN 200810228427
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Chinese (zh)
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CN101724421A (en
Inventor
张学萍
任翠霞
初人庆
勾连忠
郑庆华
石岩
高翔
朱文权
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中国石油化工股份有限公司
中国石油化工股份有限公司抚顺石油化工研究院
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Abstract

The invention discloses a method for producing needle coke by adopting the technique combining delay coking and kettle-type coking. The method comprises: when treating the conventional coking raw material by using the delay coking technique, introducing FCC slurry oil into a delay coking tower from the upper part inside the tower at the low temperature, and obtaining needle coke raw material by fractionating high temperature oil gas obtained by the reaction; and then, treating the needle coke raw material by using the kettle-type coking technique, and obtaining high quality needle coke. In the method, as the FCC slurry oil is injected into the coking tower at the lower temperature, the decomposition temperature of the conventional coking raw material is lowered, the high temperature decomposition time of the raw material is shortened, the occurrence of secondary reaction is reduced, green coke rate is reduced, the stable operation cycle of a signal tower is prolonged, and light components which have high reaction activity and are not beneficial to producing the needle coke, heavy components with high polymerization activity, and a great deal of impurities such as catalyst powder, heavy metal and the like can be removed. The obtained needle coke has high yield and good quality.

Description

A kind of production method of needle coke
Technical field
The invention belongs to a kind of processing method of producing needle coke.Specifically, be to adopt the coking process integration to produce needle coke, produce simultaneously a kind of method of light ends oil and coke.
Background technology
Needle coke is the main raw material of producing superpower, ultra-high power graphite electrode.The most critical issue of producing needle coke is selection and the pre-treatment of raw material.According to the mechanism of coke formation of needle coke, the raw material of producing needle coke must satisfy the aromaticity content height, and three rings, Fourth Ring short-side chain aromaticity content that its neutral line connects are in the majority, and the general requirement aromaticity content reaches 30-50%; Resin and asphalt content is low, resin and asphalt itself is exactly macromole condensed ring or the hydrocarbon compound of being with again longer side chain, molecular structure is complicated, carburizing reagent speed is fast, be cured into very soon the original state solid, mosaic structure in needle coke, occurs, thereby reduced the quality of needle coke, more be conducive to guarantee the needle coke quality so the resin and asphalt content of raw material is more low, general control heptane insolubles content is less than 2.0%; Ash content comprises that catalyst fines, uncombined carbon metal equal size are low, high grey branch hinders growing up of mesophasespherule and melts also, mutually undeveloped in the middle of showing in the needle coke structure, the primary quinoline insolubles content of general requirement is zero, catalyst fines content is less than 100ppm, and heavy metal content is less than 100ppm; Sulphur content is low, and great majority concentrate in the coke after the sulphur carbonization, affects the needle coke use properties, and the general requirement feed sulphur content is not more than 0.5%.
Catalytic cracking (FCC) slurry oil is the mink cell focus catalytic cracking production, although wherein be rich in a large amount of three rings, Fourth Ring aromatic hydrocarbons, contains also that the higher light constituent of cracking activity and the high restructuring of polymerization activity divide and the impurity such as a large amount of catalyst fines, heavy metal.If these are fallen producing the disadvantageous composition pre-treatment of needle coke, it is exactly good needle-shape coke raw material.At present, delayed coking is carried out in have the FCC slurry oil is mixed in the vacuum residuum, be used for improving productive rate and the character of needle-shape coke raw material, but FCC slurry oil add-on can not be too many, otherwise react the obviously running period of shortening delayed coking drums list tower, and FCC slurry oil under higher temperature, and long reaction time, make the suitable a large amount of cracking of cut meeting of making needle-shape coke raw material, reduce the productive rate of needle coke.
Raw materials pretreatment refers to remove in the raw material to generating the process of the disadvantageous composition of needle coke and impurity.CN1382761A discloses a kind of method of utilizing preparing acicular coke by catalytic cracking of classified oil.The method mainly is to utilize extraction process to remove catalyst fines in the fluid catalytic cracking decant oil, then utilizes delay coking process to produce needle coke.USP4686048 is with after being lower than 100 ℃ light oil dilution fluid catalytic cracking decant oil, after filtration, washing, removes catalyst fines wherein.USP5593572 adds the heteroatoms aliphatic polymer in fluid catalytic cracking decant oil, carry out flocculating settling, removes catalyst fines.Above-mentioned patented method mainly is be used to removing catalyst fines, be not suitable for the pre-treatment of catalytically cracked oil raw material, and all needs special device to process raw material, and flow process is numerous and diverse, uses duration, has also increased production cost.
CN1872963A discloses a kind of preprocessing method of raw materials of producing needle coke, stock oil removes wherein undesirable components through underpressure distillation first, remaining ideal composition contacts with hydrogen, hydrogenation catalyst, and the hydrogenation reaction logistics is isolated to the raw material of producing needle coke.Wherein stock oil can be catalytically cracked oil or clarified oil.The method can remove light, the heavy undesirable components in the stock oil by the combination of two kinds of techniques, keeps to greatest extent ideal composition, and the stock oil after the processing satisfies the requirement of producing needle-shape coke raw material.The method needs independent vacuum distillation apparatus, and the cut that distillation obtains needs further hydrotreatment, and hydrotreatment generates oil and also needs further to separate, and the cost of hydrogenation own is high, and investment is large.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of production method of needle coke, the method can effectively be removed in the FCC slurry oil producing that the higher light constituent of the disadvantageous cracking activity of needle coke and the high restructuring of polymerization activity divide and the impurity such as a large amount of catalyst fines, heavy metal, kept the ideal composition of producing needle coke, gained needle coke productive rate is high, and character is good.
The production method of needle coke of the present invention is with the delay coking process production needle coke that combines with the autoclave coking process, comprises the steps:
(1) the conventional coking raw material of high temperature through being heated to 450 ℃~550 ℃ enters in the delayed coking drums from the delayed coking tower bottom; Low temperature FCC slurry oil through being heated to 380 ℃~460 ℃ enters in the delayed coking drums from the delayed coking drums middle and upper part, contacts through the high-temperature oil gas that Pintsch process produces with conventional coking raw material, reacts under the delayed coking condition;
(2) the described FCC slurry oil of step (1) is derived to enter the coking fractional distillation column from cat head with the oil gas that conventional coking raw material generates at the delayed coking drums internal reaction and is separated, and obtains light ends and needle-shape coke raw material and tail oil;
(3) needle-shape coke raw material of step (2) gained enters process furnace, be heated to 440 ℃~460 ℃, after best 430 ℃~450 ℃, enter and carry out pyrogenic reaction in the autoclave coking reactor, the needle coke that generates is deposited in the autoclave coking reactor, and the oil gas of generation enters coking fractional distillation column to be separated.
Among the present invention, the initial boiling point of the described needle-shape coke raw material of step (2) is 340~380 ℃, and final boiling point is 440~460 ℃.Described light ends refers to its final boiling point less than the cut of needle-shape coke raw material initial boiling point, and described tail oil refers to that its initial boiling point greater than the cut of needle-shape coke raw material final boiling point, generally loops back delayed coking drums with conventional coking raw material.
Among the present invention, the high-temperature oil gas that the high-temperature-coked oil gas that step (3) autoclave coking reactor produces is best and step (2) delayed coking drums produces shares a coking fractional distillation column, like this can economy system and production cost.Step (3) also can adopt the another one coking fractional distillation column, and the tail oil circulation of fractionation gained together enters delayed coking drums with conventional coking raw material.
The operational condition of the delayed coking unit described in the present invention is as follows: 450 ℃~550 ℃ of conventional coking raw material furnace outlet temperature, best 485 ℃~505 ℃; Reaction pressure 0.05MPa~0.20MPa, preferably 0.15MPa~0.17MPa; Circulation weight ratio 0.05~1.0, best 0.2~0.4; Coking cycle 24h~36h; FCC slurry oil furnace outlet temperature is 380 ℃~460 ℃, best 420 ℃~440 ℃; FCC slurry oil furnace outlet temperature is than low 50 ℃~70 ℃ of conventional coking raw material furnace outlet temperature.Described circulation weight ratio refers to loop back the weight ratio of tail oil and the conventional coking raw material of delayed coking drums.
The operational condition of the described autoclave coking reactor of step of the present invention (3) is as follows: reaction pressure 1.0MPa~2.0MPa, preferably 1.3MPa~1.7MPa; 440 ℃~520 ℃ of still interior reaction temperatures, best 475 ℃~495 ℃; Coking cycle 18h~48h, preferably 24h~36h.
In the inventive method, one or more in vacuum residuum, visbroken resids, ethylene bottom oil, thermal cracking residue and the shale oil that the described conventional coking raw material of step (1) is petroleum.
In the inventive method, stop to enter the FCC slurry oil in each coking cycle operation later stage, improve simultaneously conventional coking raw material furnace outlet temperature and improve the interior temperature of coking tower, reduce the volatile matter of coke.Generally need to improve 3~5 ℃.
In the inventive method, conventional coking raw material adopts conventional delay coking process flow process, namely first be heated to 330~350 ℃ through the process furnace convection zone, then enter the separation column bottom further with the high-temperature-coked oil gas heat exchange that enters separation column, the coke powder that carries in the simultaneously drip washing coking oil gas.The described Fractionator Bottom tail oil of step (2) together goes out separation column with conventional coking raw material, after the radiation section that enters process furnace is heated to 450 ℃~550 ℃, enters in the tower from the delayed coking tower bottom and to react.
In the inventive method, FCC slurry oil, conventional coking raw material and needle-shape coke raw material can in transition section and the radiation section heating of same process furnace, also can heat in different process furnace respectively.Enter in the tower from the delayed coking drums middle and upper part FCC slurry oil is heated to 380 ℃~460 ℃ in process furnace after and react, the position that wherein said FCC slurry oil enters delayed coking drums accounts for 5/10~6/10 place of the whole height of coking tower apart from the distance of coking tower bottom.
Among the present invention, the FCC slurry oil is 10:90~50:50 with the feed weight ratio of conventional coking raw material, is preferably 20:80~40:60.
The inventive method is with the delay coking process production needle coke that combines with the autoclave coking process, when namely utilizing delay coking process to process conventional coking raw material, the FCC slurry oil is introduced in the tower from the delayed coking drums middle and upper part with low temperature, the high-temperature oil gas of reaction gained obtains needle-shape coke raw material through fractionation, then utilize the autoclave coking process to process needle-shape coke raw material, obtain the high-quality needle coke, concrete advantage is as follows:
(1) the component cracking that reactive behavior is higher under relatively mild coking condition of FCC slurry oil is fallen, and then fractionation is gone out in separation column, reaches the purpose that removes the higher light constituent of reactive behavior.
(2) the FCC slurry oil remains the desirable needle-shape coke raw material components such as most of three rings, Fourth Ring, five rings under relatively mild condition, and the identical cut of producing with conventional coking raw material is together as the raw material of producing pin Jiao.
(3) the FCC slurry oil is under the condition of delayed coking, bituminous matter and part colloid are condensed into coke, together be deposited in the coking tower together with heavy metal, catalyst fines etc., be unfavorable for that the restructuring of producing needle coke divides and impurity thereby removed, and in the pyrogenic reaction process, do not remove in coking fractional distillation column afterwards, stay tower after the fractionation at the bottom of further removed in the tail oil.
(4) the method can be processed the FCC slurry oil and be obtained needle-shape coke raw material, has enlarged the source of needle-shape coke raw material.
(5) the method can be with a process furnace and a coking fractional distillation column, and flow process is simple, in the needle coke of production high-quality anisotropic optical structure, can also produce light ends and ordinary coke.
(6) the FCC slurry oil is heated to the highest 440 ℃ and just enters delayed coking drums, and process furnace is difficult for coking, increases the service life.
(7) injection of lesser temps FCC slurry oil has reduced the cracking temperature of conventional coking raw material, has shortened the Pintsch process time of conventional raw material, has reduced the secondary reaction generation, causes coking yield to reduce, and has prolonged single tower stable operation cycle.
(8) the inventive method turndown ratio is large, and cost is low, flexible, be easy to grasp, and can be widely used.
(9) the present invention utilizes the autoclave coking process to produce needle coke, and not only the needle coke productive rate is high, and its Graphite Electrodes intensity is good.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.
Embodiment
Be further explained in detail below in conjunction with Fig. 1 and specific embodiment, but the present invention is not subjected to the restriction of embodiment.
As shown in Figure 1, the FCC slurry oil enters process furnace 1 by pipeline 15, is heated to after 380 ℃-460 ℃ to enter in the delayed coking drums 3 by the middle and upper part of pipeline 16 from delayed coking drums 3; The high-temperature oil gas that generates with the conventional coking raw material reaction that enters from the delayed coking tower bottom contact, and one coexist and react under the delayed coking condition, and the oil gas of generation enters coking fractional distillation column 5 by pipeline 4, through separation, obtains gas products and goes out device by pipeline 6; C5-180 ℃ cut goes out device by pipeline 7; 180 ℃ of-350 ℃ of cuts go out device by pipeline 17; 350 ℃-450 ℃ as needle-shape coke raw material.The needle-shape coke raw material of gained passes through pipeline 8 after process furnace 1 heating, enter autoclave coking reactor 10 by pipeline 12 and carry out cracking and polyreaction, the high-temperature oil gas that generates enters coking fractional distillation column 5 by pipeline 13 and carries out product separation, and the needle coke of production goes out device from pipeline 14; Conventional coking raw material enters the bottom of coking fractional distillation column 5 from pipeline 9, with from the high-temperature oil gas of delayed coking drums 3 and the high-temperature oil gas countercurrent flow of autoclave coking reactor 10, the coke powder that carries in the simultaneously drip washing oil gas, then together turning back to process furnace 1 by pipeline 18 with the coking tail oil enters delayed coking drums 3 by pipeline 2 and carries out pyrogenic reaction through being heated to 450 ℃~550 ℃, it is separated that the oil gas that generates enters separation column 5 by pipeline 4, and coke goes out device by pipeline 11.After coking tower 3 is full of, switches coking tower 3A and carry out same operation, adustion 4 hours is removed volatile matter.
Embodiment 1-5:
All experiments use stock oil identical among the embodiment, are intended to the effect under the comparison different operating condition.The character of testing used conventional coking raw material oil and FCC slurry oil sees Table 1, and experiment condition and test-results see Table 2.
The stock oil character that table 1 embodiment adopts
Raw material The FCC slurry oil Conventional coking raw material oil
Density (20 ℃)/kgm -3 1.0058 0.998
Viscosity (100 ℃)/mm 2·s 1 10.00 700
Condensation point/℃ 34 50
Carbon residue, % (massfraction) 7.10 16.2
Ash content, % (massfraction) 0.372 0.06
S, % (massfraction) 0.53 0.55
N/μg·g -1 4678 8841
C,% 88.44 87.36
H, % (massfraction) 8.90 11.21
Four components, % (massfraction)
Saturated minute 32.1 24.5
Fragrance divides 54.2 28.9
Colloid 13.2 39.7
Bituminous matter 0.5 6.9
Metal composition/μ gg -1
Fe/Ca 114.7/67.25
Ni/V 108.6/5.175 76.65/2.46
Na 91.79
Table 2 technological condition and product distribute and main products character
Annotate: autoclave coking tower inlet amount is the massfraction that needle-shape coke raw material accounts for the delayed coking unit total feed.

Claims (15)

1. the production method of a needle coke is with the delay coking process production needle coke that combines with the autoclave coking process, comprises the steps:
(1) the conventional coking raw material of high temperature through being heated to 450 ℃~550 ℃ enters in the delayed coking drums from the delayed coking tower bottom; Low temperature FCC slurry oil through being heated to 380 ℃~460 ℃ enters in the delayed coking drums from the delayed coking drums middle and upper part, contacts through the high-temperature oil gas that Pintsch process produces with conventional coking raw material, reacts under the delayed coking condition; The position that described FCC slurry oil enters delayed coking drums accounts for 5/10~6/10 place of the whole height of coking tower apart from the distance of coking tower bottom;
(2) the described FCC slurry oil of step (1) is derived to enter the coking fractional distillation column from cat head with the oil gas that conventional coking raw material generates at the delayed coking drums internal reaction and is separated, and obtains light ends and needle-shape coke raw material and tail oil;
(3) needle-shape coke raw material of step (2) gained enters process furnace, after being heated to 440 ℃~460 ℃, enter and carry out pyrogenic reaction in the autoclave coking reactor, the needle coke of generation is deposited in the autoclave coking reactor, and the oil gas of generation enters coking fractional distillation column to be separated.
2. in accordance with the method for claim 1, the initial boiling point that it is characterized in that needle-shape coke raw material described in the step (2) is 340~380 ℃, and final boiling point is 440~460 ℃.
3. in accordance with the method for claim 1, it is characterized in that the high-temperature oil gas that high-temperature-coked oil gas that step (3) autoclave coking reactor produces and step (2) delayed coking drums produce shares a coking fractional distillation column fractionation.
4. according to claim 1 or 2 described methods, it is characterized in that described tail oil be initial boiling point greater than the cut of needle-shape coke raw material final boiling point, loop back delayed coking drums with conventional coking raw material, the circulation weight ratio is 0.05~1.0.
5. according to claim 1 or 2 described methods, it is characterized in that the operational condition of described delayed coking is as follows: 450 ℃~550 ℃ of conventional coking raw material furnace outlet temperature; Reaction pressure 0.05MPa~0.20MPa; Coking cycle 24h~36h; FCC slurry oil furnace outlet temperature is 380 ℃~460 ℃; FCC slurry oil furnace outlet temperature is than low 50 ℃~70 ℃ of conventional coking raw material furnace outlet temperature.
6. in accordance with the method for claim 4, it is characterized in that the operational condition of described delayed coking is as follows: 485 ℃~505 ℃ of conventional coking raw material furnace outlet temperature; Reaction pressure 0.15MPa~0.17MPa; Circulation weight ratio 0.2~0.4; Coking cycle 24h~36h; FCC slurry oil furnace outlet temperature is 420 ℃~440 ℃.
7. in accordance with the method for claim 1, it is characterized in that needle-shape coke raw material enters process furnace described in the step (3), be heated to 430 ℃~450 ℃.
8. in accordance with the method for claim 1, it is characterized in that the operational condition of the described autoclave coking reactor of step (3) is as follows: reaction pressure 1.0MPa~2.0MPa; 440 ℃~520 ℃ of still interior reaction temperatures; Coking cycle 18h~48h.
9. in accordance with the method for claim 1, it is characterized in that the operational condition of the described autoclave coking reactor of step (3) is as follows: reaction pressure 1.3MPa~1.7MPa; 475 ℃~495 ℃ of still interior reaction temperatures; Coking cycle 24h~36h.
10. in accordance with the method for claim 1, it is characterized in that in vacuum residuum, visbroken resids, ethylene bottom oil, thermal cracking residue and the shale oil that the described conventional coking raw material of step (1) is petroleum one or more.
11. in accordance with the method for claim 1, it is characterized in that stopping to enter the FCC slurry oil in each coking cycle operation later stage, improve simultaneously 3~5 ℃ of conventional coking raw material furnace outlet temperature, improve the temperature in the coking tower, reduce the volatile matter of coke.
12. in accordance with the method for claim 1, it is characterized in that the described conventional coking raw material of step (1) is heated to 300~350 ℃ through the process furnace convection zone first, then enter separation column bottom further with the high-temperature-coked oil gas heat exchange that enters separation column, the coke powder that carries in the simultaneously drip washing coking oil gas, and together go out separation column with the described Fractionator Bottom tail oil of step (2), after the radiation section that enters process furnace is heated to 450 ℃~550 ℃, enters in the tower from the delayed coking tower bottom and to react.
13. in accordance with the method for claim 1, it is characterized in that described FCC slurry oil, conventional coking raw material and needle-shape coke raw material in the different sites heating of same process furnace, perhaps heat respectively in different process furnace.
14. in accordance with the method for claim 1, it is characterized in that described FCC slurry oil and the feed weight ratio of conventional coking raw material are 10: 90~50: 50.
15. in accordance with the method for claim 1, it is characterized in that described FCC slurry oil and the feed weight ratio of conventional coking raw material are 20: 80~40: 60.
CN 200810228427 2008-10-29 2008-10-29 Production method of needle coke CN101724421B (en)

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CN105985791A (en) * 2015-02-10 2016-10-05 中国石油化工股份有限公司 Method for preparing needle coke raw material
RU2729191C1 (en) * 2019-05-06 2020-08-05 Общество с ограниченной ответственностью "НефтеХимКонсалт" Method for producing oil needle coke

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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
JP2014527571A (en) * 2012-08-29 2014-10-16 オブシュヘストヴォ エス オグラニチェンノイ オトゥヴェステュヴェンノステュ “プロミンテク”Obshhestvo S Ogranichennoi Otvetstvennost’Yu Promintekh Delayed coking method for petroleum residues
CN104560104B (en) * 2013-10-23 2016-08-17 中国石油化工股份有限公司 A kind of method producing needle coke
CN105623692B (en) * 2014-10-31 2018-07-31 中国石油化工股份有限公司 A method of preparing needle-shape coke raw material
CN105623720B (en) * 2014-10-31 2017-04-26 中国石油化工股份有限公司 Method for preparing raw material for needle-like coke
CN105623691B (en) * 2014-10-31 2018-09-28 中国石油化工股份有限公司 A method of preparing needle-shape coke raw material
CN110066676B (en) * 2019-04-24 2021-05-04 中国石油大学(华东) Continuous process for producing high-quality needle coke

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CN105985791A (en) * 2015-02-10 2016-10-05 中国石油化工股份有限公司 Method for preparing needle coke raw material
CN105985791B (en) * 2015-02-10 2018-11-02 中国石油化工股份有限公司 A method of preparing needle-shape coke raw material
RU2729191C1 (en) * 2019-05-06 2020-08-05 Общество с ограниченной ответственностью "НефтеХимКонсалт" Method for producing oil needle coke

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