CN103509572B - A kind of technique utilizing solvent method to prepare high-quality coal-based needle coke - Google Patents
A kind of technique utilizing solvent method to prepare high-quality coal-based needle coke Download PDFInfo
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- CN103509572B CN103509572B CN201210208103.8A CN201210208103A CN103509572B CN 103509572 B CN103509572 B CN 103509572B CN 201210208103 A CN201210208103 A CN 201210208103A CN 103509572 B CN103509572 B CN 103509572B
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Abstract
The invention discloses a kind of technique utilizing solvent method to prepare high-quality coal-based needle coke.This technique makes raw material and solvent, removes quinoline insolubles by physical sepn, distills after separation to clear liquor, and the light ends after distillation is used as solvent.Carry out hydrotreatment to the heavy ends after distillation, then coking obtains coal-based needle coke, and distills the oil gas that coking produces, and fractionates out heavy ends and is used as solvent.The present invention, recycle is raw-material while, can prepare quinoline insolubles content and be less than 0.1% and the lower high-quality coal-based needle coke raw material of toluene insoluble-quinoline solubles content.
Description
Technical field
The invention belongs to coal chemical technology, be specifically related to a kind of technique utilizing solvent method to prepare high-quality coal-based needle coke.
Background technology
Needle coke is the main raw material producing ultra-high power graphite electrode and high power graphite electrode, the advantages such as the current density having that thermal shock resistance is strong, physical strength is high, oxidation susceptibility is good, electrical consumption is low with the Graphite Electrodes that needle coke is made and allow is large, therefore the market requirement is huge.The needle coke of current production uses the difference of raw material can be divided into petroleum needle coke and the large class of coal-based needle coke two according to it.Wherein, petroleum needle coke is that raw material production obtains with petroleum residual oil, and prepares needle coke using coal tar or coal-tar pitch etc. as raw material and be called coal-based needle coke.Because refining of petroleum trend is towards the future development of catalytic cracking lighting deep processing, cause the raw material of petroleum needle coke to reduce gradually, so from the later stage seventies in last century, coal-based needle coke prepared broad development.
The raw material of coal-based needle coke is made up of three parts, is respectively xylene solubles (TS), toluene insoluble-quinoline solvend (QS-TI) and quinoline insolubles (QI).Those skilled in the art when carrying out purifying treatment to needle-shape coke raw material, due to QI component be unprofitable to completely needle coke produce, so this material will be removed up hill and dale as much as possible; In addition, QS-TI component can have influence on spherular growth, and then has influence on the quality of needle coke, and the content of this component is more, and the quality obtaining needle coke is poorer, therefore in order to obtain the needle coke of high-quality, also should this component be removed as far as possible.In the method for many purifying treatment, solvent method is widely used because of simple to operate, low cost.Solvent method is fully mixed with coal tar or coal tar pitch raw material by suitable solvent, removes solvent insolubles wherein by modes such as centrifugation, filtering separation or gravity settlings again.
In prior art, Chinese patent CN1940017A discloses a kind of preparation method of needle coke.Its key step comprises catalytic cracking Residual oil (FCC slurry oil), send into settlement separate tower after one or more and light constituent solvent in coal tar fraction or asphalt stock and carry out standing separation, isolated refined asphaltic bitumen mixing oil enters vacuum flasher again and carries out rapid flash after the tower top outflow of settlement separate tower, temperature in vacuum flasher is 250-400 DEG C, the light constituent oil deviate from after flash distillation is back to settlement separate tower again as circulating solvent and mixes with raw material or to send into the oily medial launder of light constituent for subsequent use, the exquisite asphalt oil obtained after removing light constituent oil enters tubular reactor and carries out heated polymerizable generation mesophase spherule after vacuum flasher discharge.This technique adopts light constituent oil to carry out purifying treatment as solvent to needle-shape coke raw material, and the content of the quinoline insolubles from the exquisite asphalt oil that vacuum flasher is discharged is less than 2%.
Above-mentioned technique processes needle-shape coke raw material by adopting light constituent oil, although eliminate the quinoline insolubles in refined asphaltic bitumen oil to a certain extent, but because the diameter of quinoline insolubles is less than 0.1um usually, be difficult to be removed, therefore the content of its quinoline insolubles only can reach less than 2%, cannot meet preparation high-quality needle coke time raw material in quinoline insolubles content should lower than the requirement of 0.1%.In addition, the solubleness of light constituent Oil solvent in above-mentioned technique to the toluene insoluble in asphalt oil-quinoline solvend component is larger, the content of toluene insoluble in the needle-shape coke raw material after above-mentioned art breading-quinoline solvend component is also higher, cannot meet the requirement of preparation high-quality needle coke equally.
Summary of the invention
Light constituent oil is adopted to process needle-shape coke raw material in order to solve in prior art the technique preparing needle coke, cannot meet preparation high-quality needle coke time raw material in quinoline insolubles content should lower than the requirement of 0.1%, and the solubleness of light constituent Oil solvent to the toluene insoluble in asphalt oil-quinoline solvend component is larger, the content of toluene insoluble in the needle-shape coke raw material after process-quinoline solvend component is also higher, the problem of the requirement of preparation high-quality needle coke cannot be met equally, the invention provides a kind of solvent method that utilizes effectively can removing quinoline insolubles and toluene insoluble-quinoline solvend component in needle-shape coke raw material and prepare the technique of high-quality coal-based needle coke.
The technical scheme utilizing solvent method to prepare the technique of high-quality coal-based needle coke of the present invention is:
Utilize solvent method to prepare a technique for high-quality coal-based needle coke, comprise following steps:
(1), by coal measures raw material and solvent, after stirring, adopt physical sepn to remove desolventizing insolubles and obtain clear liquor, described coal measures raw material is coal tar or coal-tar pitch;
Described solvent at least comprises one or more products obtained through hydrogenation or coking process in the distillate of 200 ~ 350 DEG C that coal tar, coal-tar pitch or Doak Tar Oil obtain again through the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation obtains;
The mass ratio of described solvent and described coal measures raw material is 0.5-10;
(2) hydrotreatment is carried out to described clear liquor;
(3) product after hydrotreatment is distilled, coking is carried out to the heavy ingredient of >300 DEG C that fractionates out, obtains needle coke product;
(4) distill the oil gas that coking produces, the coal measures heavy ends fractionated out between 200 DEG C-300 DEG C is used as the solvent in step (1).
The mass ratio of described solvent and described coal measures raw material is 2-8.
Described solvent at least comprises a kind of in the distillate of 200 ~ 350 DEG C that coal-tar pitch or Doak Tar Oil obtain or two kinds of products obtained through hydrogenation or coking process again through the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation obtains.
Described solvent also comprises the petroleum heavy ends of 200 DEG C-300 DEG C obtained through fractionation.
The described coal measures heavy ends comprised in described solvent and the mass ratio of described petroleum heavy ends are 5:95-99:1.
The described coal measures heavy ends comprised in described solvent and the mass ratio of described petroleum heavy ends are 10:90-75:25.Described solvent also comprises coal measures light ends.
Before hydrotreatment is carried out to described clear liquor, described clear liquor is distilled, fractionate out≤cut of 200 DEG C is used as in described solvent coal measures light ends, carries out hydrotreatment to the cut of residue >200 DEG C.
The mass ratio of described coal measures heavy ends and described coal measures light ends is 5:95-75:25.
The mass ratio of described coal measures heavy ends and described coal measures light ends is 20:80-60:40.
The temperature of described hydrotreatment is 330 DEG C-390 DEG C, and pressure is less than or equal to 19Mpa.
The temperature of described hydrotreatment is 350 DEG C-380 DEG C, and pressure is 8-15Mpa.
Described physical sepn is centrifugation.
The relative centrifugal force of described centrifugation is 1200-4000G.
The relative centrifugal force of described centrifugation is 2000-3500G.
The temperature of described coking is 480-510 DEG C, and the pressure of coking is 0.2-0.3MPa.
The technique utilizing solvent method to prepare high-quality coal-based needle coke of the present invention, step (1) is by coal tar or coal-tar pitch and coal tar, one or more products obtained through hydrotreatment in the distillate of 200 ~ 350 DEG C that coal-tar pitch or Doak Tar Oil obtain are again through the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation obtains, reason is that the solubleness of described coal measures heavy ends to above-mentioned coal measures raw material is lower, use the above-mentioned coal measures heavy ends gone out through hydrotreatment aftercut as solvent, after described solvent is mixed with coal tar or coal-tar pitch, clear liquor can be formed by described dissolution with solvents to preparing the useful xylene solubles of needle coke in raw material, quinoline insolubles and a large amount of QS-TI then form insolubles precipitation, wherein undissolved QS-TI can be coated on around quinoline insolubles particulate, because the solubleness of described solvent to raw material in the present invention is lower, therefore undissolved QS-TI precipitation capacity is larger, and then make the coating thickness around described quinoline insolubles larger, more easily be removed in the process of physical sepn.Therefore, technique of the present invention, while the content effectively reducing quinoline insolubles in raw material, also effectively eliminates the QS-TI in raw material.
The mass ratio arranging described solvent and described coal tar or described coal-tar pitch in step of the present invention (1) is 0.5-10, reason is the too little dissolving that can limit xylene solubles of this mass ratio, thus reduce the output of needle coke, then can cause too greatly the waste of solvent.The present invention is 0.5-10 by limiting the mass ratio of described solvent and described coal measures raw material, effectively prevent above-mentioned two situations.The mass ratio of the present invention also further preferred described solvent and described coal measures raw material is 2-8, is because both fully can dissolve xylene solubles further in this proportional range, does not waste solvent again.
In the present invention, step (2) carries out hydrotreatment to described clear liquor; The present invention is by carrying out hydrotreatment to described clear liquor, object is the sulphur in order to remove needle-shape coke raw material, and in the process of hydrotreatment, the sulphur in raw material can change corresponding hydrogen sulfide into and remove, thus greatly reduce the content of sulphur, effectively prevent the swelling of needle coke product.In order to improve hydrogenation efficiency, the temperature that the present invention also limits described hydrotreatment is 330 DEG C-390 DEG C, and pressure is less than 19Mpa, and the temperature condition of further preferred described hydrotreatment is 350 DEG C-380 DEG C, pressure 8-15Mpa.
Step of the present invention (3) carries out coking to the heavy ingredient after hydrotreatment, obtains needle coke product;
Step of the present invention (4) is distilled the oil gas that coking produces, and the coal measures heavy ends fractionated out between 200 DEG C-300 DEG C is used as the solvent in step (1).Heavy ends after hydrogenation is used as solvent, reduces quinoline insolubles and QS-TI solubleness in a solvent to a great extent, thus obtains the needle-shape coke raw material of high-quality.
The advantage utilizing solvent method to prepare the technique of high-quality coal-based needle coke of the present invention is:
(1) technique utilizing solvent method to prepare high-quality coal-based needle coke of the present invention, arranging described physical sepn is centrifugation, and further preferred described relative centrifugal force is 2000-3500G.Reason is, the method for described centrifugation, compared to other physical separation method, such as filtration method, settling process etc., has higher separation efficiency, by described centrifugal method, effectively can remove the quinoline insolubles in described coal measures raw material.
(2) technique utilizing solvent method to prepare high-quality coal-based needle coke of the present invention, described solvent is also set and comprises coal measures light ends, be because quinoline insolubles and QS-TI solubleness in a solvent can be reduced further adding of coal measures light ends, thus improve the quality of needle-shape coke raw material.Simultaneously, the mass ratio that the present invention also limits described coal measures heavy ends and described coal measures light ends is 5:95-75:25, select this proportional range to be make TS quantitative change few because quinoline insolubles and QS-TI solubleness in a solvent too much can be made extremely low for light ends, thus cause needle coke output few; And light ends crosses the effect not having at least and reduce quinoline insolubles and QS-TI solubleness in a solvent further, the quality of needle-shape coke raw material can not be improved.The mass ratio of the present invention also preferred described coal measures heavy ends and described coal measures light ends is 20:80-60:40.
(3) technique utilizing solvent method to prepare high-quality coal-based needle coke of the present invention, before hydrotreatment is carried out to described clear liquor, first described clear liquor is distilled under 200 DEG C of conditions, the coal measures light ends fractionated out is used as the solvent in step (1), thus achieve the recycle of light ends, because the coal measures heavy ends in solvent described in the present invention is distill the hydrogenation products in step (3), cut between 200 DEG C-300 DEG C that fractionate out, therefore solvent of the present invention can be obtained by the circulation in technique, reduce the cost of technique.
In addition, before the present invention is arranged on and carries out hydrotreatment to described clear liquor, described clear liquor is distilled, fractionate out≤cut of 200 DEG C is used as in solvent coal measures light ends, only hydrotreatment is carried out to the cut of remaining >200 DEG C, also serve the effect improving hydrogenation efficiency.
Accompanying drawing explanation
More being convenient to make content of the present invention understand, below in conjunction with the drawings and specific embodiments, technical solutions according to the invention being further elaborated.
Fig. 1 is the process flow sheet utilizing solvent method to prepare high-quality coal-based needle coke raw material of the present invention.
Embodiment
Embodiment 1
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, comprises following steps:
(1) preparation of solvent: coal tar is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add SAS-10 type dearsenification desulfurization catalyst, hydrotreatment is carried out to described coal tar, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent.
(2), by coal tar and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal tar is 0.5;
(3) described clear liquor is pumped into the second hydrogenator, set temperature is 330 DEG C, and pressure is 19Mpa, adds SAS-10 type dearsenification desulfurization catalyst, carries out hydrotreatment to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 460 DEG C, and the pressure of coking is 0.15MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, be used as the solvent in step (2).
Embodiment 2
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first coking tower, set temperature is 400 DEG C, pressure is 0.1Mpa, coking is carried out to described coal-tar pitch, the oil gas that coking produces is sent into the first distillation tower distill, the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 10;
(3) described clear liquor is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, and pressure is 19Mpa, adds FHRS-2 type hydrogenation and mends Si catalyst, carry out hydrotreatment to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of the >300 fractionated out DEG C is sent into the second coking tower, the temperature arranging coking is 460 DEG C, and the pressure of coking is 0.15MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, be used as the solvent in step (2).
Embodiment 3
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, comprises following steps:
(1) preparation of solvent: the distillate of 200 ~ 350 DEG C that are obtained by Doak Tar Oil pumps into, set temperature is 300 DEG C, pressure is 20Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent, in addition the petroleum heavy ends of 200 DEG C-300 DEG C that petroleum raw material obtains through fractionation is also contained in solvent, the mass ratio of described coal measures heavy ends and described petroleum heavy ends is 5:95.(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 10;
(3) described clear liquor is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, and pressure is 19Mpa, adds FV-20 type Hydrobon catalyst, carries out hydrotreatment to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of the >300 fractionated out DEG C is sent into the second coking tower, the temperature arranging coking is 460 DEG C, and the pressure of coking is 0.15MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, be used as the solvent in step (2).
Embodiment 4
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first coking tower, set temperature is 400 DEG C, pressure is 0.1Mpa, coking is carried out to described coal-tar pitch, the oil gas that coking produces is sent into the first distillation tower distill, the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent, in addition also contain the petroleum heavy ends of 200 DEG C-300 DEG C that petroleum raw material obtains through fractionation in solvent, the mass ratio of described coal measures heavy ends and described petroleum heavy ends is 99:1;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 10;
(3) described clear liquor is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, and pressure is 19Mpa, adds FH-40A type Hydrobon catalyst, carries out hydrotreatment to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of the >300 fractionated out DEG C is sent into the second coking tower, the temperature arranging coking is 460 DEG C, and the pressure of coking is 0.15MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, be used as the solvent in step (2).
Embodiment 5
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first coking tower, set temperature is 400 DEG C, pressure is 0.1Mpa, coking is carried out to described coal-tar pitch, the oil gas that coking produces is sent into the first distillation tower distill, the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent, in addition also contain the petroleum heavy ends of 200 DEG C-300 DEG C that petroleum raw material obtains through fractionation in solvent, the mass ratio of described coal measures heavy ends and described petroleum heavy ends is 10:90;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 10;
(3) described clear liquor is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, and pressure is 19Mpa, adds SAS-10 type dearsenification desulfurization catalyst, carries out hydrotreatment to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of the >300 fractionated out DEG C is sent into the second coking tower, the temperature arranging coking is 460 DEG C, and the pressure of coking is 0.15MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, be used as the solvent in step (2).
Embodiment 6
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first coking tower, set temperature is 400 DEG C, pressure is 0.1Mpa, coking is carried out to described coal-tar pitch, the oil gas that coking produces is sent into the first distillation tower distill, the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent, in addition also contain the petroleum heavy ends of 200 DEG C-300 DEG C that petroleum raw material obtains through fractionation in solvent, the mass ratio of described coal measures heavy ends and described petroleum heavy ends is 75:25;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, pressure is 19Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures lightweight oil content is 5:95.
Embodiment 7
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first coking tower, set temperature is 400 DEG C, pressure is 0.1Mpa, coking is carried out to described coal-tar pitch, the oil gas that coking produces is sent into the first distillation tower distill, the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent, in addition also contain the petroleum heavy ends of 200 DEG C-300 DEG C that petroleum raw material obtains through fractionation in solvent, the mass ratio of described coal measures heavy ends and described petroleum heavy ends is 55:45;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, pressure is 19Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 75:25.
Embodiment 8
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, pressure is 19Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 20:80.
Embodiment 9
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add SAS-10 type dearsenification desulfurization catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, pressure is 19Mpa, carries out hydrotreatment to described clear liquor;
(4) product after hydrotreatment is distilled, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, add SAS-10 type dearsenification desulfurization catalyst, after coking, obtain needle coke product;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 40:60.
Embodiment 10
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, pressure is 19Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 11
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 330 DEG C, pressure is 19Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, be used as the solvent in step (2);
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 12
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 13
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add SAS-10 type dearsenification desulfurization catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 2;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add SAS-10 type dearsenification desulfurization catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 14
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 15
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: coal-tar pitch is pumped into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to described coal-tar pitch, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt the settlement separate desolventizing insolubles that removes to obtain clear liquor, the time settlement separate in the present embodiment is 24 hours, and the mass ratio of described solvent and described coal-tar pitch is 8;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 16
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: the distillate of 200 ~ 350 DEG C that are obtained by Doak Tar Oil pumps into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to the distillate of 200 ~ 350 DEG C that described Doak Tar Oil obtains, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal tar and solvent, after stirring, adopt centrifugation to remove desolventizing insolubles and obtain clear liquor, the centrifugal force of centrifugation is 2900G, and the mass ratio of described solvent and described coal tar is 0.5;
(3) described clear liquor is distilled, fractionate out≤cut of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of the heavy ends of coal measures described in solvent and described coal measures light ends is 60:40.
Embodiment 17
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: the distillate of 200 ~ 350 DEG C that are obtained by Doak Tar Oil pumps into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add SAS-10 type dearsenification desulfurization catalyst, hydrotreatment is carried out to the distillate of 200 ~ 350 DEG C that described Doak Tar Oil obtains, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt centrifugation to remove desolventizing insolubles and obtain clear liquor, the centrifugal force of centrifugation is 3100G, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add SAS-10 type dearsenification desulfurization catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 450 DEG C, and the pressure of coking is 0.1MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of described coal measures heavy ends and described coal measures light ends is 60:40.
Embodiment 18
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: the distillate of 200 ~ 350 DEG C that are obtained by Doak Tar Oil pumps into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to the distillate of 200 ~ 350 DEG C that described Doak Tar Oil obtains, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal tar and solvent, after stirring, adopt centrifugation to remove desolventizing insolubles and obtain clear liquor, the centrifugal force of centrifugation is 3100G, and the mass ratio of described solvent and described coal tar is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FHRS-2 type hydrogenation and mend Si catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 480 DEG C, and the pressure of coking is 0.2MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of described coal measures heavy ends and described coal measures light ends is 60:40.
Embodiment 19
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: the distillate of 200 ~ 350 DEG C that are obtained by Doak Tar Oil pumps into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to the distillate of 200 ~ 350 DEG C that described Doak Tar Oil obtains, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal-tar pitch and solvent, after stirring, adopt centrifugation to remove desolventizing insolubles and obtain clear liquor, the centrifugal force of centrifugation is 3100G, and the mass ratio of described solvent and described coal-tar pitch is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FV-20 type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 510 DEG C, and the pressure of coking is 0.3MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of described coal measures heavy ends and described coal measures light ends is 60:40.
Embodiment 20
The solvent method that utilizes described in the present embodiment prepares the technique of high-quality coal-based needle coke, as shown in Figure 1, comprises following steps:
(1) preparation of solvent: the distillate of 200 ~ 350 DEG C that are obtained by Doak Tar Oil pumps into the first hydrogenator, set temperature is 300 DEG C, pressure is 20Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to the distillate of 200 ~ 350 DEG C that described Doak Tar Oil obtains, product hydrotreatment obtained is sent into the first distillation tower and is distilled, and the heavy ends of 200 DEG C-300 DEG C that fractionation are obtained is used as solvent;
(2), by coal tar and solvent, after stirring, adopt centrifugation to remove desolventizing insolubles and obtain clear liquor, the centrifugal force of centrifugation is 3100G, and the mass ratio of described solvent and described coal tar is 0.5;
(3) described clear liquor is distilled, fractionate out≤the coal measures light ends of 200 DEG C backflow is used as in step (2) solvent, the cut of remaining >200 DEG C is pumped into fixed bed hydrogenation reactor, set temperature is 380 DEG C, pressure is 15Mpa, add FH-40A type Hydrobon catalyst, hydrotreatment is carried out to described clear liquor;
(4) distill the product after hydrotreatment, the heavy ingredient of >300 DEG C fractionated out is sent into coking tower, and the temperature arranging coking is 500 DEG C, and the pressure of coking is 0.26MPa, obtains needle coke product after coking;
(5) oil gas that coking produces is sent into second column to distill, after fractionating out the coal measures heavy ends backflow between 200 DEG C-300 DEG C, is used as the solvent in step (2),
The mass ratio of described coal measures heavy ends and described coal measures light ends is 60:40.
In the above-described embodiments, the air speed of described fixed bed hydrogenation reactor is set to 0.5h
-1, the service temperature of described distillation tower is greater than 200 DEG C.Described first hydrogenator and the second hydrogenator are fixed bed hydrogenation reactor.
Experimental example
In order to confirm technique effect of the present invention, the present invention is provided with experimental example, the mass percentage of QI and the QS-TI component in the raw material before and after above-described embodiment step (1) process is measured, test sample wherein in embodiment 6-20 is the raw material after the solvent in the coal measures heavy ends and the complete step of replacing of coal measures light ends (1) refluxed, and result is as follows:
Comparative example
In order to confirm technique effect of the present invention further, the present invention is also provided with comparative example, and this comparative example adopts the coal tar raw material described in embodiment 1, the preparation technology of the needle coke adopting Chinese patent CN1940017A to announce:
1), by described coal tar and solvent, after stirring, adopt settlement separate method to remove desolventizing insolubles and obtain clear liquor, the mass ratio of described solvent and described coal tar is 0.5; Described solvent is the light ends coming from vacuum flasher;
2) described clear liquor is sent into vacuum flasher, distill under 300 DEG C of conditions, after the coal measures light ends backflow distilled out, be used as the solvent in step 1).
QI and QS-TI component in the clear liquor obtained in described step 1) is measured, its content is respectively 1.5% and 5.9%, compared to the clear liquor in embodiment 1, in comparative example, QI and QS-TI component concentration has exceeded 1.41% and 3.3% respectively, therefore, technique in the present invention, compared to comparative example, can prepare the needle-shape coke raw material that QI and QS-TI component concentration is lower, and then prepares the needle coke product of high-quality.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (18)
1. utilize solvent method to prepare a technique for high-quality coal-based needle coke, it is characterized in that, comprise following steps:
(1), by coal measures raw material and solvent, after stirring, adopt physical sepn to remove desolventizing insolubles and obtain clear liquor, described coal measures raw material is coal tar or coal-tar pitch;
Described solvent at least comprises one or more products obtained through hydrogenation or coking process in the distillate of 200 ~ 350 DEG C that coal tar, coal-tar pitch or Doak Tar Oil obtain again through the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation obtains;
The mass ratio of described solvent and described coal measures raw material is 0.5-10;
(2) hydrotreatment is carried out to described clear liquor;
(3) product after hydrotreatment is distilled, coking is carried out to the heavy ingredient of >300 DEG C that fractionates out, obtains needle coke product;
(4) distill the oil gas that coking produces, the coal measures heavy ends fractionated out between 200 DEG C-300 DEG C is used as the solvent in step (1).
2. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 1, is characterized in that, the mass ratio of described solvent and described coal measures raw material is 2-8.
3. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 1 and 2, it is characterized in that, described solvent at least comprises a kind of in the distillate of 200 ~ 350 DEG C that coal-tar pitch or Doak Tar Oil obtain or two kinds of products obtained through hydrogenation or coking process again through the coal measures heavy ends of 200 DEG C-300 DEG C that fractionation obtains.
4. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 3, is characterized in that, described solvent also comprises the petroleum heavy ends of 200 DEG C-300 DEG C obtained through fractionation.
5. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 4, is characterized in that, the described coal measures heavy ends comprised in described solvent and the mass ratio of described petroleum heavy ends are 5:95-99:1.
6. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 5, is characterized in that, the described coal measures heavy ends comprised in described solvent and the mass ratio of described petroleum heavy ends are 10:90-75:25.
7. the solvent method that utilizes according to claim 1,2,4,5 or 6 prepares the technique of high-quality coal-based needle coke, and it is characterized in that, described solvent also comprises coal measures light ends.
8. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 3, it is characterized in that, described solvent also comprises coal measures light ends.
9. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 7, it is characterized in that, before hydrotreatment is carried out to described clear liquor, described clear liquor is distilled, fractionate out≤cut of 200 DEG C is used as in described solvent coal measures light ends, carries out hydrotreatment to the cut of residue >200 DEG C.
10. the technique utilizing solvent method to prepare high-quality coal-based needle coke according to claim 8, it is characterized in that, before hydrotreatment is carried out to described clear liquor, described clear liquor is distilled, fractionate out≤cut of 200 DEG C is used as in described solvent coal measures light ends, carries out hydrotreatment to the cut of residue >200 DEG C.
11. solvent methods that utilize according to claim 9 or 10 prepare the technique of high-quality coal-based needle coke, and it is characterized in that, the mass ratio of described coal measures heavy ends and described coal measures light ends is 5:95-75:25.
12. techniques utilizing solvent method to prepare high-quality coal-based needle coke according to claim 11, is characterized in that, the mass ratio of described coal measures heavy ends and described coal measures light ends is 20:80-60:40.
13. solvent methods that utilize according to claim 1,2,4,5,6,8,9,10 or 12 prepare the technique of high-quality coal-based needle coke, it is characterized in that, in step (2), the temperature of described hydrotreatment is 330 DEG C-390 DEG C, and pressure is less than or equal to 19Mpa.
14. techniques utilizing solvent method to prepare high-quality coal-based needle coke according to claim 13, is characterized in that, the temperature of described hydrotreatment is 350 DEG C-380 DEG C, and pressure is 8-15Mpa.
15. techniques utilizing solvent method to prepare high-quality coal-based needle coke according to claim 14, it is characterized in that, described physical sepn is centrifugation.
16. techniques utilizing solvent method to prepare high-quality coal-based needle coke according to claim 15, is characterized in that, the relative centrifugal force of described centrifugation is 1200-4000G.
17. techniques utilizing solvent method to prepare high-quality coal-based needle coke according to claim 16, is characterized in that, the relative centrifugal force of described centrifugation is 2000-3500G.
18. techniques utilizing solvent method to prepare high-quality coal-based needle coke according to claim 17, it is characterized in that, the temperature of described coking is 480-510 DEG C, the pressure of coking is 0.2-0.3MPa.
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| CN106520164B (en) * | 2016-10-28 | 2019-08-23 | 中国矿业大学(北京) | A kind of method that overcritical combination extraction mode separates needle-shape coke raw material from high temperature coal-tar |
| CN109370629B (en) * | 2018-10-16 | 2019-11-29 | 陕西煤业化工集团神木天元化工有限公司 | A kind of production method of coal-based needle coke |
| CN109370628B (en) * | 2018-10-16 | 2020-09-08 | 陕西煤业化工集团神木天元化工有限公司 | Production process of coal-based needle coke |
| CN109370631B (en) * | 2018-10-16 | 2020-09-08 | 陕西煤业化工集团神木天元化工有限公司 | Production method for producing coal-based needle coke by utilizing coal tar to the maximum extent |
| CN109233886B (en) * | 2018-10-26 | 2021-10-15 | 重庆润科新材料技术有限公司 | Production method for preparing coal-based needle coke by using medium-low temperature coal tar |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105609A (en) * | 1984-06-22 | 1987-01-28 | 千代田化工建设株式会社 | The method of hydrogenation of coal tar pitch |
| CN101787299A (en) * | 2010-03-01 | 2010-07-28 | 上海尚元化工工程技术有限公司 | Method for extracting, producing and purifying pitch with mixed solvent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105609A (en) * | 1984-06-22 | 1987-01-28 | 千代田化工建设株式会社 | The method of hydrogenation of coal tar pitch |
| CN101787299A (en) * | 2010-03-01 | 2010-07-28 | 上海尚元化工工程技术有限公司 | Method for extracting, producing and purifying pitch with mixed solvent |
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