CN103013566A - Technology for preparing needle coke raw material from coal-tar pitch - Google Patents
Technology for preparing needle coke raw material from coal-tar pitch Download PDFInfo
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- CN103013566A CN103013566A CN2011102844858A CN201110284485A CN103013566A CN 103013566 A CN103013566 A CN 103013566A CN 2011102844858 A CN2011102844858 A CN 2011102844858A CN 201110284485 A CN201110284485 A CN 201110284485A CN 103013566 A CN103013566 A CN 103013566A
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- 239000002994 raw material Substances 0.000 title claims abstract description 53
- 239000011294 coal tar pitch Substances 0.000 title claims abstract description 48
- 239000011331 needle coke Substances 0.000 title abstract description 53
- 238000005516 engineering process Methods 0.000 title abstract description 12
- 239000003921 oil Substances 0.000 claims abstract description 87
- 239000002904 solvent Substances 0.000 claims abstract description 70
- 239000003054 catalyst Substances 0.000 claims abstract description 42
- 239000003245 coal Substances 0.000 claims abstract description 41
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 239000010692 aromatic oil Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 68
- 239000011295 pitch Substances 0.000 claims description 47
- 239000000571 coke Substances 0.000 claims description 32
- 238000005119 centrifugation Methods 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 21
- 239000003208 petroleum Substances 0.000 claims description 11
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical class [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims description 7
- 239000011269 tar Substances 0.000 claims description 6
- 150000001896 cresols Chemical class 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000010426 asphalt Substances 0.000 abstract description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 12
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 39
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 38
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 28
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 238000002360 preparation method Methods 0.000 description 11
- 239000005864 Sulphur Substances 0.000 description 9
- 238000012545 processing Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000011311 coal-based needle coke Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 2
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- AYOOGWWGECJQPI-NSHDSACASA-N n-[(1s)-1-(5-fluoropyrimidin-2-yl)ethyl]-3-(3-propan-2-yloxy-1h-pyrazol-5-yl)imidazo[4,5-b]pyridin-5-amine Chemical compound N1C(OC(C)C)=CC(N2C3=NC(N[C@@H](C)C=4N=CC(F)=CN=4)=CC=C3N=C2)=N1 AYOOGWWGECJQPI-NSHDSACASA-N 0.000 description 1
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Abstract
The invention provides a technology for preparing a needle coke raw material from coal-tar pitch. The technology comprises the following steps of 1, fully mixing asphalt and a solvent, and removing insoluble substances in the mixture by a physical separation method, wherein the solvent is a mixture of coal light oil and coal aromatic oil or is a mixture of BTX and coal aromatic oil; a mass ratio of the coal light oil or the BTX to the coal aromatic oil is in a range of (20: 80) to (95: 5); and a mass ratio of the solvent to the asphalt is in a range of 0.5 to 10, 2, feeding a clear liquor without the insoluble substances into a separator, and separating the light solvent from the clear liquor to obtain a heavy fraction having low QI, and 3, carrying out hydrotreatment on the heavy fraction in the presence of a hydrogenation catalyst at a temperature of 300 to 450 DEG C under the pressure of 5 to 20MPa. The needle coke raw material obtained by the technology has low sulfur content and a small expansion coefficient.
Description
Technical field
The invention belongs to coal chemical technology, be specifically related to a kind of technique of utilizing coal-tar pitch to prepare the coal-based needle coke raw material.
Background technology
Needle coke is the quality matetrial of making superpower and ultra-high power graphite electrode, and the Graphite Electrodes made from needle coke has the advantages such as thermal shock resistance is strong, physical strength is high, oxidation susceptibility is good, consumption of electrode low and allow current density is large.The needle coke of producing at present can be divided into petroleum needle coke and coal-based needle coke two large classes according to the difference of using raw material; U.S. big lake carbon element company has at first developed the production technique of petroleum needle coke in the fifties; but 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; in addition the seventies twice oil crisis; more make people feel the unstable of raw material supply; so from the later stage seventies, the preparation technology of coal-based needle coke is developed.
Coal-based needle coke is prepared from take coal-tar pitch as raw material, the main component of coal-tar pitch is polycyclc aromatic compound, also contain a certain amount of quinoline insolubles (QI), when quinoline insolubles generates mesophasespherule in the pitch thermal transition, can hinder spherular growth, can not form carbonization structure, and then affect the quality of needle coke.Therefore, when preparing the high-quality needle-shape coke raw material with coal-tar pitch, must remove to coal-tar pitch the purifying treatment of quinoline insolubles, treatment process commonly used in the prior art mainly contains following three kinds:
(1) flash distillation-condensation methods.This method is that mixing raw material oil is delivered in the specific flashing tower, flashes off flash oil under certain temperature and vacuum, flash oil is imported polycondensation vessel again and carries out polymerization and obtain polycondensation asphalt.For example, Hongte Coal Chemical Co., Ltd., Shanxi is in the application documents of CN1944578A in the patent No., a kind of industrialized producing technology of coal-based needle coke is disclosed, by with coal-tar pitch, the full cut of flash oil after vacuum flashing adopts the fractional condensation method to carry out the segmentation condensation, obtains three sections cuts of heavy, medium and light; Adopt improved pitch circulation method that the stage casing flash oil is carried out polycondensation and obtain polycondensation asphalt; Described polycondensation asphalt and heavy flash oil are carried out delayed coking process under the conditions that nitrogen exists, the coking later stage with N
2Injecting noncoking oils carries out the final heating of needle coke coking and draws Jiao; Carry out again high-temperature calcination and obtain coal-based needle coke.
(2) solvent method.Solvent method is to make by a certain percentage mixed solvent with aliphatic hydrocarbon and aromatic hydrocarbon, mixed solvent is mixed with pitch, after process stirs, leaves standstill, precipitates in stirring tank, form the mixture of pitch and solvent on the upper strata, extracted out by pump again and send into solvent recovery tower, reclaim solvent and produce refined asphaltic bitumen, obtain being fit to the raw material of tar needle-shape coke.
(3) centrifuging.Coal-tar pitch enters whizzer under suitable temperature and viscosity, the residue that is rich in QI that obtains after the centrifugation is removed, and remaining centrifugate is as the raw material of preparation needle coke.
Above-mentioned three kinds of methods all can be removed the QI in the raw material, wherein, solvent method is because simple to operate, expense is lower and be widely used, a kind of preparation method of needle coke is disclosed such as Chinese patent literature CN1724611A, adopted solvent method raw material to be removed the purifying treatment of quinoline insolubles in the method, be specially: with the feed coal tar-bitumen, the light constituent oil of viscid bitumen or coal tar fraction and the condensation of vacuum flashing cat head is according to 1:(0.5-4) ratio enter the first settlement separate tower after mixing and separate, temperature is controlled to be 100-250 ℃, the residence time of material in tower is 0.5-20 hour, discharge at the bottom of the tower contain quinoline insolubles and easily the residual oil of polymeric component mixture account for the 5-30% of inlet amount, flow out from cat head and contain quinoline insolubles less than 5% refined asphaltic bitumen oil.
Be the composition synoptic diagram of coal-tar pitch as shown in Figure 1, wherein γ is the toluene solvend, β
2Be toluene insoluble pyridine solvend (TI-PS), β
1Be the insoluble quinoline solvend of pyridine (PI-QS), α is quinoline insolubles.In the prior art, those skilled in the art are when processing the needle-shape coke raw material coal-tar pitch, because α quinoline insolubles component is to be unprofitable to needle coke fully produce, so all this material will be removed up hill and dale as much as possible; In addition, β
1The insoluble quinoline solvend of component pyridine also should be removed as far as possible, for β
2Component, the at present technology cognition in this field are because β
2Component can have influence on spherular growth, and then has influence on the quality of needle coke, so also all be as much as possible this component to be removed.
In the above-mentioned technique, because adopt light constituent oil as solvent, this solvent has also removed the insoluble quinoline solvend with pyridine of the toluene insoluble pyridine solvend in the coal-tar pitch in large quantities when quinoline insolubles (QI) is removed, the inventor finds by research, β
2The existence of component is not to be absolute harmful, selects the β of sufficient quantity
2Component can be when not affecting the needle coke quality, obviously play the productive rate that improves needle coke and the effect that reduces the needle coke thermal expansivity, and being prior art those skilled in the art, this point do not recognize, also just because of in above-mentioned technology, with β
2Component is removed as much as possible, so use the coal-tar pitch after the above-mentioned processing to prepare needle coke as raw material, its productive rate is very low, and the thermal expansivity of the needle coke for preparing is large, has had a strong impact on like this use properties of needle coke as electrode.
In addition, in the pitch of above-mentioned explained hereafter, still also has a small amount of sulphur content, these sulphur content can remain in the needle coke that described pitch prepares, under hot conditions, can generate gas at the graphitization processing Sulfur During Process of making electrode to described needle coke, cause electrode to expand, and then affect the quality of Graphite Electrodes.Although time of described graphitization processing prolonged can suppress to a certain extent electrode and expand, the lengthening in treatment time can cause electric quantity consumption to increase, thereby reduces the economic benefit of described technology for preparing electrode as far as possible.
Summary of the invention
In order to solve the needle-shape coke raw material that uses treatment process preparation of the prior art, owing to adopt light constituent oil as solvent, when quinoline insolubles is removed, also removed in large quantities the toluene insoluble pyridine solvend in the coal-tar pitch, thereby when causing using this asphalt stock to prepare needle coke, the problem that the productive rate of needle coke is very low, thermal expansivity is larger; Simultaneously also in order to solve owing to containing sulphur in asphalt stock inside, under hot conditions, can generate gas at the graphitization processing Sulfur During Process of making electrode, cause electrode to expand, and then affect the problem of Graphite Electrodes quality, the invention provides a kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material, output when the raw material that uses technique of the present invention to be prepared from prepares needle coke is higher, and the content of sulphur is very low, and the needle coke for preparing has the little advantage of thermal expansivity.
The technical scheme of the technique that pitch prepares needle-shape coke raw material of utilizing of the present invention is:
A kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) with pitch with after solvent fully mixes, adopt the method for physical sepn to remove insolubles in the described mixed solution;
Described solvent is the mixture of coal measures lightweight oil and coal measures aromatic oil, or the mixture of BTX and coal measures aromatic oil, and the mass ratio of described coal measures lightweight oil or BTX and coal measures aromatic oil is 20:80-95:5; The mass ratio of described solvent and described pitch is 0.5-10;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300～450 ℃, and pressure is 5～20Mpa.
Described coal measures lightweight oil is one or more in gas light oil, tar light oil, the petroleum naphtha light oil, and described coal measures aromatic oil is washing oil, absorb oil, cresols is oily, in the carbolineum one or more.
Described physical sepn is centrifugation.
In the described step (1), the viscosity of carrying out the described mixed solution of centrifugation is 40～90mpas.
In the described step (1), under 50-55 ℃ of condition with pitch and solvent.
The mass ratio of described solvent and described pitch is 0.7～2.
In the described step (1), the mass ratio of described coal measures lightweight oil and coal measures aromatic oil is 30:70-90:10.
In the described step (1), the mass ratio of described coal measures lightweight oil and coal measures aromatic oil is 80:20-40:60.
Hydrogenation catalyst in the described step (3) is any one in Ni-Mo series catalysts or the Ni-W series catalysts.
In the described step (3), the temperature condition of hydrotreatment is 300～350 ℃, and pressure is 8～12MPa scope.
The technique of utilizing coal-tar pitch to prepare needle-shape coke raw material of the present invention, step (1) is fully mixed pitch with solvent, then adopt the method for physical sepn to remove insolubles in the described mixed solution, in order to provide quinoline insolubles content low asphalt stock to hydrogenation reaction, because in hydrogenation reaction, quinoline insolubles in the pitch can cause hydrogenation catalyst deteriorated, reduce speed of reaction, so that the productive rate of described hydrogenation reaction reduces, economy also descends thereupon, therefore, for making hydrotreatment long-term, stably carry out, need in advance the quinoline insolubles in the asphalt stock to be removed.
The clear liquor that step (2) will be removed behind the insolubles is sent into separator, isolates the lightweight solvent in the clear liquor, obtains the heavy ends of low QI; The purpose of this step is to remove the lightweight oil content, only remaining pitch is carried out hydrotreatment, improves the processing efficiency of hydrogenator.
Step (3) is carried out hydrotreatment to described heavy ends under the condition that hydrogenation catalyst exists, purpose is in order to remove the sulphur in the described asphalt stock, in the process of hydrotreatment, sulphur in the described pitch can change corresponding hydrogen sulfide into and remove, thereby greatly reduce the content of sulphur, effectively prevented the swelling of needle coke product.
Solvent described in the present invention is the mixture of coal measures lightweight oil and coal measures aromatic oil, or the mixture of BTX(benzene,toluene,xylene) with the mixture of coal measures aromatic oil, the mass ratio of described coal measures lightweight oil or BTX and coal measures aromatic oil is 20:80-95:5; The mass ratio of described solvent and described pitch is 0.5-10.The present inventor finds by a large amount of research, although also can have influence on spherular growth when the content of described toluene insoluble pyridine solvend is excessive, and then have influence on the quality of needle coke, but the toluene insoluble pyridine solvend can obviously play the productive rate that improves needle coke and the effect that reduces the needle coke thermal expansivity, if coal-tar pitch contains the toluene insoluble pyridine solvend of suitable proportion, the productive rate of needle coke can obviously improve in the quality that does not affect needle coke, thermal expansivity also can reduce, but those skilled in the art not yet recognize this point.The mixture that described solvent is coal measures lightweight oil and coal measures hydrocarbon oil is set among the present invention, and the mass ratio of described coal measures hydrocarbon oil and coal measures lightweight oil is 20:80-95:5; The blending ratio of these two kinds of oil, described two kinds of oil is set and states solvent and the ratio of described pitch by selection, removing as far as possible up hill and dale α quinoline insolubles and β
1In the time of the insoluble quinoline solvend of component pyridine, the described solvent of capable of regulating is to described β
2The extraction quantity of toluene insoluble pyridine soluble components, thus a certain proportion of β suitably kept
2Component when not affecting the needle coke quality, obviously plays the productive rate that improves needle coke and the effect that reduces the needle coke thermal expansivity, finds β by contriver's research
2Component is advisable to remain on 3.5%-9.5%.
The technological advantage that utilizes coal-tar pitch to prepare needle-shape coke raw material described in the present invention is:
(1) coal-tar pitch that utilizes described in the present invention prepares the technique of needle-shape coke raw material, described coal measures lightweight oil be set be in gas light oil, tar light oil, the petroleum naphtha light oil one or more, described coal measures aromatic oil is washing oil, absorb oil, cresols is oily, in the carbolineum one or more, and reason is to use these several oil more to be suitable for adjusting described solvent to described β
2The extraction quantity of toluene insoluble pyridine soluble components.
(2) coal-tar pitch that utilizes described in the present invention prepares the technique of needle-shape coke raw material, the method that selection arranges the physical sepn in the described step (1) is centrifugation, reason with, the method of described centrifugation is than other physical separation method, such as filtration method, settling process etc., higher separation efficiency is arranged, by described centrifugal method, can effectively remove the quinoline insolubles in the described coal tar raw material.The viscosity that the present invention also further defines the described mixed solution that carries out centrifugation is 40～90mpas, reason is, those skilled in the art think in the prior art, when adopting the QI in the centrifuging separate bitumen, the viscosity of described pitch should be more low better, and the QI particle under lower viscosity in the pitch has higher subsidence rate.But, fact proved that this to fall low viscous method only effective to oarse-grained QI, and for the QI particle of diameter less than 1um, because undersized, in settling process, can be subject to the collision impact of asphaltene molecule, therefore be difficult to sedimentation, this just so that centrifuging the removal efficient of QI is difficult to be improved.The present inventor is by long-term research, abandoned those skilled in the art's technology prejudice always, find suitably to improve the viscosity of described pitch, when not reducing QI macrobead removal effect, also can improve the content of large particulate matter in the described coal tar, the QI particulate of described large particulate matter in can the described pitch of active adsorption, and drive the together sedimentation of described QI particulate, therefore the present invention is 40～90mpas by the viscosity that described mixed solution is set, Effective Raise the removal efficient of QI particle in the described pitch.
(3) coal-tar pitch that utilizes described in the present invention prepares the technique of needle-shape coke raw material, hydrogenation catalyst in the described step (3) is that hydrogen catalyst is any one in Ni-Mo series catalysts or the Ni-W series catalysts, reason is, described Ni-Mo series catalysts or Ni-W series catalysts taking off S efficient and will be higher than iron series hydrocatalyst of the prior art during as hydrogenation catalyst, divide by hydrogenation and to free S, can be with H behind the S hydrogenation in the described heavy ends
2The S form removes, thereby obtains the heavy ends of low S.The content of described S can satisfy the needs of actual use fully.
Description of drawings
In order to make content of the present invention more be convenient to understand, below in conjunction with the accompanying drawing embodiment technical solutions according to the invention are described further;
Shown in Figure 1 is the composition synoptic diagram of coal-tar pitch.
Embodiment
Embodiment 1
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material, comprising:
(1) with coal-tar pitch with after solvent fully mixes, adopt the method for filtering separation to remove insolubles in the described mixed solution;
Described solvent is the mixture of petroleum naphtha light oil and washing oil, and the mass ratio of described petroleum naphtha light oil and washing oil is 20:80; The mass ratio of described solvent and described pitch is 0.5;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300 ℃, and pressure is 5Mpa, and the hydrogenation catalyst described in the present embodiment is FeS
2
Embodiment 2
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material, comprising:
(1) with pitch with after solvent fully mixes, adopt settlement separate method to remove insolubles in the described mixed solution, the described settling time is 6h;
Described solvent is the mixture of tar light oil and cresols oil, and the mass ratio of described tar light oil and cresols oil is 95:5; The mass ratio of described solvent and described pitch is 10;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 450 ℃, and pressure is 20Mpa, and the hydrogenation catalyst described in the present embodiment is FeS
2
Embodiment 3
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material, may further comprise the steps:
(1) with pitch with after solvent fully mixes, adopt the method for centrifugation to remove insolubles in the described mixed solution, the relative centrifugal force of described centrifugation is 2500G;
Described solvent is the mixture of petroleum naphtha light oil and carbolineum, and the mass ratio of described petroleum naphtha light oil and carbolineum is 90:5; The mass ratio of described solvent and described pitch is 5, and the viscosity of carrying out the described mixed solution of centrifugation is 40mpas;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 400 ℃, and pressure is 15Mpa, and the hydrogenation catalyst described in the present embodiment is FeS
2
Embodiment 4
A kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) with pitch with after solvent fully mixes, adopt the method for centrifugation to remove insolubles in the described mixed solution, the relative centrifugal force of described centrifugation is 2500G;
Described solvent is gas light oil and the mixture that absorbs oil, and described gas light oil is 20:80 with the mass ratio that absorbs oil; The mass ratio of described solvent and described pitch is 5; The viscosity of carrying out the described mixed solution of centrifugation is 90mpas;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300 ℃, and pressure is 5Mpa, and the hydrogenation catalyst described in the present embodiment is FeS
2
Embodiment 5
A kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) with pitch with after solvent fully mixes, adopt the method for centrifugation to remove insolubles in the described mixed solution, the relative centrifugal force of described centrifugation is 2500G;
Described solvent is BTX and the mixture that absorbs oil, and described BTX is 30:70 with the mass ratio that absorbs oil; The mass ratio of described solvent and described pitch is 0.7; The viscosity of carrying out the described mixed solution of centrifugation is 90mpas;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300 ℃, and pressure is 5Mpa, and the hydrogenation catalyst described in the present embodiment is FeS
2
BTX described in the present embodiment is the mixture of benzene,toluene,xylene.
Embodiment 6
A kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) under 50 ℃ of conditions with pitch with after solvent fully mixes, adopt the method for centrifugation to remove insolubles in the described mixed solution, the relative centrifugal force of described centrifugation is 2500G;
Described solvent is gas light oil and the mixture that absorbs oil, and described gas light oil is 90:10 with the mass ratio that absorbs oil; The mass ratio of described solvent and described pitch is 2; The viscosity of carrying out the described mixed solution of centrifugation is 90mpas;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300 ℃, and pressure is 5Mpa, and the hydrogenation catalyst described in the present embodiment is FeS
2
Embodiment 7
A kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) under 55 ℃ of conditions with pitch with after solvent fully mixes, adopt the method for centrifugation to remove insolubles in the described mixed solution, the relative centrifugal force of described centrifugation is 2500G;
Described solvent is gas light oil and the mixture that absorbs oil, and described gas light oil is 80:20 with the mass ratio that absorbs oil; The mass ratio of described solvent and described pitch is 2, and the viscosity of carrying out the described mixed solution of centrifugation is 90mpas;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300 ℃, and pressure is 12Mpa, and the hydrogenation catalyst described in the present embodiment is the Ni-Mo series catalysts.
Embodiment 8
A kind of technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) under 55 ℃ of conditions with pitch with after solvent fully mixes, adopt the method for centrifugation to remove insolubles in the described mixed solution, the relative centrifugal force of described centrifugation is 2500G;
Described solvent is gas light oil and the mixture that absorbs oil, and described gas light oil is 40:60 with the mass ratio that absorbs oil; The mass ratio of described solvent and described pitch is 1, and the viscosity of carrying out the described mixed solution of centrifugation is 90mpas;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 350 ℃, and pressure is 8Mpa, and the hydrogenation catalyst described in the present embodiment is the Ni-W series catalysts.
Need to prove, carry out in the device of the carried out hydrogenation reaction of the arbitrary form that the hydrogenation reaction among above-mentioned all embodiment can be used in the prior art, such as flow type bubbling reactor etc., as preferred embodiment, described hydrogenator can be fixed bed hydrogenation reactor, thereby has avoided existing in the raw material of the preparation needle coke that obtains the phenomenon of catalyst precipitation.
The principle of work of the separator in above-described embodiment is: the product that described heat from hydrogenation is decomposed carries out flash separation, is separated into high score oil and low minute oil.Described separator is being heated to 350 ℃, and material enters in the separator, and the composition of boiling point below 350 ℃ becomes vaporised gas on separator top, and the composition of boiling point more than 350 ℃ forms liquid or the slurry attitude places the separator bottom." low minute oil " described in the present invention is the term that those skilled in the art commonly use with " high score oil ", the line of delimitation that described low minute oily and high score oil is unfixing, just the technician asks convenient to define according to practical situation, oil referred to the cut below 350 ℃ in low minute in the present invention, and high score oil refers to the cut more than 350 ℃.
In addition, in above-described embodiment, described Ni-Mo series catalysts and described Ni-W series catalysts can be the metal particles of Ni and Mo or Ni and W, also can be described active ingredient Ni and Mo or Ni and W to be loaded on the support of the catalyst be prepared from, and described carrier can be Al
2O
3Carrier, the selection of catalyzer described in the present invention are this area prior art commonly used, therefore repeat no more in the present invention.In addition, the Ni-Mo series catalysts described in the present invention and described Ni-W series catalysts are commercially available any products.
Experimental example
In order to illustrate that technical scheme described in the present invention has substantive technique effect than prior art, the present invention is provided with following experimental example:
When experiment, the Initial Composition of the coal-tar pitch that uses in above-described embodiment is:
QI:4.3%,?PI?:5.8%、TI:?10.6%，S:0.24?wt%。
To describedly measuring for the preparation of the sulphur in the raw material of needle coke that above-described embodiment obtains, the result is as shown in the table:
Described raw material for the preparation of needle coke obtained above is put into the coker of preparation needle coke, 550 ℃ of condition Using Coke-ovens 5 hours, obtain needle coke.
Described needle coke product is carried out graphitization processing under 2800 ℃ of conditions, the thermal expansivity of the needle coke after greying is as shown in the table:
β to described raw material for the preparation of needle coke obtained above
2Component is measured, and it is as shown in the table to obtain the result:
Needle coke productive rate when further described raw material obtained above being prepared needle coke is measured, and it is as shown in the table to obtain the result:
Comparative example
Have substantive technique effect in order to further specify technical scheme described in the present invention than prior art, the present invention is provided with following comparative example:
The pitch that utilizes in this comparative example prepares the technique of needle-shape coke raw material, comprise: the coal-tar pitch that uses in the experimental example is raw material, at abundant Agitation and mixing, pitch is fully dissolved described asphalt stock and solvent, the mass ratio of solvent and pitch is 0.25:1, carry out centrifugation after the pitch dissolving, tail is abandoned residue, and the gained stillness of night distills, behind removal and the recovery solvent, can be purified pitch, wherein, described solvent is coker light oil;
Sulphur content in the purifying pitch that this comparative example obtains is 0.20wt%, greater than the 0.12-0.14wt% in the experimental example;
Purifying pitch obtained above is put into the coker of preparation needle coke, and 550 ℃ of condition Using Coke-ovens 5 hours, the productive rate that obtains needle coke was 30%;
Described needle coke product is carried out graphitization processing under 2800 ℃ of conditions, the thermal expansivity of the needle coke after greying is 1.4 * 10
-6/ ℃, the content of its toluene insoluble pyridine solvend is 1.9%.
By as can be known above-mentioned, the thermal expansivity of needle coke has increased 0.1-0.5 * 10 than embodiment in the comparative example
-6/ ℃, when reality was used, this was enough to make the quality of the Graphite Electrodes of needle coke preparation to be a greater impact; In addition, the productive rate of needle coke has reduced 18-20% than embodiment in the comparative example, as seen the coal-tar pitch that the coal-tar pitch productive rate that contains suitable proportion toluene insoluble pyridine solvend among the present invention uses in the prior art, therefore, coal-tar pitch among the present invention has obvious substantive technique effect than prior art.
Although the present invention elaborates it by embodiment; but; those skilled in the art should be understood that any form that does not exceed the claim protection domain made on this basis and the variation of details, all belong to invention which is intended to be protected.
Claims (10)
1. technique of utilizing coal-tar pitch to prepare needle-shape coke raw material may further comprise the steps:
(1) with pitch with after solvent fully mixes, adopt the method for physical sepn to remove insolubles in the described mixed solution;
Described solvent is the mixture of coal measures lightweight oil and coal measures aromatic oil, or the mixture of BTX and coal measures aromatic oil, and the mass ratio of described coal measures lightweight oil or BTX and coal measures aromatic oil is 20:80-95:5; The mass ratio of described solvent and described pitch is 0.5-10;
(2) will remove the clear liquor that obtains behind the insolubles and send into separator, isolate the lightweight solvent in the clear liquor, obtain the heavy ends of low QI;
(3) under the condition that hydrogenation catalyst exists described heavy ends is carried out hydrotreatment, the temperature condition of hydrotreatment is 300～450 ℃, and pressure is 5～20Mpa.
2. the technique of utilizing coal-tar pitch to prepare needle-shape coke raw material according to claim 1, it is characterized in that, described coal measures lightweight oil is one or more in gas light oil, tar light oil, the petroleum naphtha light oil, and described coal measures aromatic oil is washing oil, absorb oil, cresols is oily, in the carbolineum one or more.
3. the technique of utilizing coal-tar pitch to prepare needle-shape coke raw material according to claim 1 is characterized in that, described physical sepn is centrifugation.
4. the technique of utilizing coal-tar pitch to prepare needle-shape coke raw material according to claim 3 is characterized in that, in the described step (1), the viscosity of carrying out the described mixed solution of centrifugation is 40～90mpas.
5. according to claim 1 and 2 or the 3 or 4 described techniques of utilizing coal-tar pitch to prepare needle-shape coke raw material, it is characterized in that, in the described step (1), under 50-55 ℃ of condition with pitch and solvent.
6. according to claim 1 and 2 or 3 or the 4 or 5 described techniques of utilizing coal-tar pitch to prepare needle-shape coke raw material, it is characterized in that the mass ratio of described solvent and described pitch is 0.7～2.
7. arbitrary described technique of utilizing coal-tar pitch to prepare needle-shape coke raw material is characterized in that according to claim 1-6, and in the described step (1), the mass ratio of described coal measures lightweight oil and coal measures aromatic oil is 30:70-90:10.
8. arbitrary described technique of utilizing coal-tar pitch to prepare needle-shape coke raw material is characterized in that according to claim 1-7, and in the described step (1), the mass ratio of described coal measures lightweight oil and coal measures aromatic oil is 80:20-40:60.
9. arbitrary described technique of utilizing coal-tar pitch to prepare needle-shape coke raw material is characterized in that according to claim 1-8, and the hydrogenation catalyst in the described step (3) is any one in Ni-Mo series catalysts or the Ni-W series catalysts.
10. arbitrary described technique of utilizing coal-tar pitch to prepare needle-shape coke raw material is characterized in that according to claim 1-8, and in the described step (3), the temperature condition of hydrotreatment is 300～350 ℃, and pressure is 8～12MPa scope.
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