CN103087747B - Process for preparing needle coke raw material by using coal-tar pitch and through heavy-phase circulation - Google Patents
Process for preparing needle coke raw material by using coal-tar pitch and through heavy-phase circulation Download PDFInfo
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- CN103087747B CN103087747B CN201110339694.8A CN201110339694A CN103087747B CN 103087747 B CN103087747 B CN 103087747B CN 201110339694 A CN201110339694 A CN 201110339694A CN 103087747 B CN103087747 B CN 103087747B
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- 239000002994 raw material Substances 0.000 title claims abstract description 84
- 239000011294 coal tar pitch Substances 0.000 title claims abstract description 74
- 239000011331 needle coke Substances 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 222
- 238000000034 method Methods 0.000 claims abstract description 90
- 239000000203 mixture Substances 0.000 claims abstract description 54
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 37
- 239000011295 pitch Substances 0.000 claims abstract description 14
- 239000000571 coke Substances 0.000 claims description 44
- 239000003245 coal Substances 0.000 claims description 41
- 239000010426 asphalt Substances 0.000 claims description 33
- 239000003208 petroleum Substances 0.000 claims description 31
- 238000007670 refining Methods 0.000 claims description 30
- 239000004615 ingredient Substances 0.000 claims description 27
- 238000002360 preparation method Methods 0.000 claims description 21
- 238000005119 centrifugation Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 13
- 239000011269 tar Substances 0.000 claims description 11
- 230000001133 acceleration Effects 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 8
- 239000011280 coal tar Substances 0.000 claims description 7
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical group [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims description 5
- WHRZCXAVMTUTDD-UHFFFAOYSA-N 1h-furo[2,3-d]pyrimidin-2-one Chemical compound N1C(=O)N=C2OC=CC2=C1 WHRZCXAVMTUTDD-UHFFFAOYSA-N 0.000 claims description 4
- 235000006173 Larrea tridentata Nutrition 0.000 claims description 4
- 244000073231 Larrea tridentata Species 0.000 claims description 4
- 229960002126 creosote Drugs 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 abstract description 14
- 239000007788 liquid Substances 0.000 abstract 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 238000001914 filtration Methods 0.000 description 9
- 125000003118 aryl group Chemical group 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 5
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000011311 coal-based needle coke Substances 0.000 description 3
- 239000002283 diesel fuel Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 239000011305 binder pitch Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000010512 thermal transition Effects 0.000 description 1
Landscapes
- Coke Industry (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention relates to a process for preparing a needle coke raw material by using coal-tar pitch and through heavy-phase circulation. The process comprises the steps that: (1) coal-tar pitch is sufficiently mixed with a first solvent; first solvent insoluble matters are removed from the mixture with a physical separation method, such that a first clarified liquid is obtained; (2) the first solvent is removed by separation; the obtained residual component is subjected to hydrogenation, such that refined pitch is obtained; (3) the first solvent insoluble matters and a second solvent are sufficiently mixed; second solvent insoluble matters are removed from the mixture with a physical separation method, such that a second clarified liquid is obtained; (4) the second solvent in the second clarified liquid is removed by separation, such that a refined heavy component is obtained; and (5) the refined pitch and the refined heavy component are mixed, such that the raw material used for preparing needle coke is obtained. With the process provided by the invention, the obtained needle coke raw material has high polyaromatic condensed polycyclic aromatic content, such that needle coke product yield is effectively improved.
Description
Technical field
The present invention relates to needle coke preparation field, be specifically related to a kind of coal-tar pitch that utilizes and prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle.
Background technology
Needle coke is the quality matetrial manufacturing superpower and ultra-high power graphite electrode, has the advantages such as thermal shock resistance is strong, physical strength is high, oxidation susceptibility is good, consumption of electrode is low and allow current density is large with the Graphite Electrodes that needle coke is made.The needle coke of current production can be divided into petroleum needle coke and the large class of coal-based needle coke two according to using the difference of raw material; big lake carbon element company of the U.S. 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; the raw material of petroleum needle coke is caused to reduce gradually; in addition the seventies twice oil crisis; people are more made to feel the instability 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 that raw material is prepared from coal-tar pitch, the main component of coal-tar pitch is polycyclc aromatic compound, also containing a certain amount of quinoline insolubles (QI), quinoline insolubles is when pitch thermal transition generates mesophasespherule, spherular growth can be hindered, make it form carbonization structure, and then affect the quality of needle coke.Therefore, when preparing high-quality needle-shape coke raw material with coal-tar pitch, must remove the purifying treatment of quinoline insolubles to coal-tar pitch, in the method for many purifying treatment, solvent method is widely used because of simple to operate, low cost.Solvent method is mixed with pitch by suitable solvent, in stirring tank after stirring, leave standstill, precipitating, pitch is made to be dissolved in solvent, thus the mixture of pitch and solvent is formed on upper strata, this mixture is extracted out feeding solvent recovery tower again by pump, recycling design also produces refined asphaltic bitumen, finally obtains the raw material being applicable to preparing needle coke.In prior art, conventional solvent is the mixed solution that aliphatic hydrocarbon and aromatic hydrocarbon are made by a certain percentage.
As Chinese patent literature CN101531909A discloses a kind of continuous sedimentation process for the production of needle coke, this technique take coal tar soft asphalt as raw material, take organic solvent as extraction agent, through the settlement separate quinoline insolubles removed in raw material, the light of acquisition obtains needle coke produced by refined asphaltic bitumen raw material as cracking units after distillation, and the heavy phase settled down then is made outside binder pitch and sold after distillation.The organic solvent used in this technique is exactly the mixture of aliphatic hydrocarbon and aromatic hydrocarbon, and wherein, the mass ratio of described aliphatic hydrocarbon and aromatic hydrocarbon is 1:0.6-1.4; Described organic solvent initial boiling point >=150 DEG C at ambient pressure, the quantity of distillate >=95%(w/w before 310 DEG C).The qualified refined asphaltic bitumen of quinoline insolubles content can be obtained by above-mentioned technique, and there is equipment advantage few, simple to operate.
In fact, the applicant is found by research, in the heavy phase settled down in above-mentioned technique except the quinoline insolubles of obstruction microsphere growth and impurity, also containing a large amount of how fragrant fused-ring aromatic compositions, and this part composition is the basic substance that greying generates needle coke, but but the heavy phase settled down is removed completely in above-mentioned technique, cause the how fragrant fused-ring aromatic component content in the needle-shape coke raw material obtained lower, if so utilize above-mentioned raw materials to prepare needle coke, and then cause the productive rate of described needle coke product lower; And the conventional techniques means of the prior art exactly that this technique embodies, that is, the technology prejudice that technical development those skilled in the art for many years exist all the time is exactly the heavy phase containing substantial quinoline-insoluble content and impurity will be removed, and so just can make in needle-shape coke raw material containing the least possible quinoline insolubles affecting greying process.So, up to the present, in prior art, not yet there is the technology carrying out processing Posterior circle utilization to described heavy phase.
Summary of the invention
Heavy phase composition is isolated owing to completely removes in solvent method in order to solve to use in prior art to prepare in the technique of needle-shape coke raw material, and cause the how fragrant fused-ring aromatic component content in the needle-shape coke raw material obtained lower, and cause thus utilize above-mentioned raw materials to prepare needle coke time, the problem that the productive rate of described needle coke product is lower.The invention provides a kind of coal-tar pitch that utilizes and prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, the needle-shape coke raw material that this technique prepares has more much higher fragrant fused-ring aromatic content, effectively improves the productive rate of described needle coke product.
The technical scheme utilizing coal-tar pitch to prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle of the present invention is:
Utilize coal-tar pitch to prepare a technique for needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing physical sepn removes the first solvent insolubles in described mixture, obtains the first clear liquor;
Described first solvent is lightweight oil, and the mass ratio of described first solvent and described coal-tar pitch is 0.1-15;
(2) be separated the first solvent in described first clear liquor of removing, hydrogenation carried out to the remaining component after described first solvent of removing, obtains refined asphaltic bitumen;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor;
Described second solvent is the mixture of matter oil in lightweight oil and coal measures, and in the coal measures in described second solvent, matter oil is 1:0.1-1:2 with the mass ratio of described lightweight oil; The mass ratio of described second solvent and described first solvent insolubles is 0.5-50;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
The mass ratio of described first solvent and described coal-tar pitch is 0.4-10.
The mass ratio of described first solvent and described coal-tar pitch is 0.5-2.
In described coal measures, matter oil is 1:0.1-1:1 with the mass ratio of described lightweight oil.
The mass ratio of described second solvent and described first solvent insolubles is 1-10.
Lightweight oil in described first solvent and the second solvent is coal measures lightweight oil.
Described coal measures lightweight oil is one or more in vapour light oil, BTX, tar light oil, petroleum naphtha.
In described coal measures, matter oil is one or more in washing oil, absorption oil, creosote, carbolineum.
The temperature of described hydrogenation reaction is 300-400 DEG C, and pressure is 5-20MPa.
Hydrogenation catalyst is nickel molybdenum series catalyst.
The temperature of described hydrogenation reaction is 300-350 DEG C, and pressure is 10-15MPa.
Physical sepn in described step (1) and step (3) is centrifugation, and the centrifugal acceleration of described centrifugation is 2000-4000G.
The centrifugal acceleration of described centrifugation is 2200-3500G.
The coal-tar pitch that utilizes of the present invention prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, coal-tar pitch fully mixes with the first solvent by step (1), the method of employing physical sepn removes the first solvent insolubles in described mixture, obtains the first clear liquor; Wherein, described first solvent is chosen as lightweight oil, and the mass ratio of described first solvent and described coal-tar pitch is 0.1-15, is preferably 0.4-10, more preferably 0.5-2; This step is to provide to hydrogenation reaction the raw material that quinoline insolubles content, free carbon and foreign matter content are low, because in hydrogenation reaction, the impurity such as the quinoline insolubles in raw material and free carbon can cause hydrogenation catalyst deterioration, reduce speed of reaction, the productive rate of described hydrogenation reaction is reduced, and economy also declines thereupon, therefore, for making hydrotreatment carry out for a long time, stably, need in advance by the quinoline insolubles removing in asphalt stock.
Step (2) is separated the first solvent in described first clear liquor of removing, carries out hydrogenation, obtain refined asphaltic bitumen to the remaining component after described first solvent of removing; The object of removing lightweight oil solvent is the processing efficiency improving described hydrogenator.Hydrotreatment is carried out to described heavy ends, object is the carbohydrate content in order to improve in described pitch, and in the process of hydrotreatment, the impurity in described pitch can be removed, thus substantially increase carbohydrate content, effectively prevent the swelling of needle coke product.
The the first solvent insolubles obtained in step (1) fully mixes with the second solvent by step (3), and the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor; Described second solvent is matter oil in coal measures, and in the coal measures in described second solvent, matter oil is 1:0.1-1:2 with the mass ratio of described lightweight oil, is preferably set to 1:0.1-1:1; The mass ratio of described second solvent and described first solvent insolubles is 0.5-50, and be preferably set to 1-10, the object of this step is to refine heavy ends isolated in solvent method further, extract how fragrant fused-ring aromatic composition wherein, thus abandon the technology prejudice that heavy phase that existing technical staff thinks containing substantial quinoline-insoluble content and impurity ought to remove.In coal measures in the present invention, matter oil refers to the oil product of boiling temperature within the scope of 220-350 DEG C.
Step (4) is separated the second solvent in described second clear liquor of removing with (5), obtain refining heavy ingredient; Again by described refined asphaltic bitumen and described refining heavy ingredient mixing, thus obtain the higher needle-shape coke raw material of how fragrant fused-ring aromatic component content, effectively improve the productive rate of needle coke product.
The technological advantage utilizing coal-tar pitch to prepare needle-shape coke raw material in conjunction with heavy phase recycle 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 in conjunction with heavy phase recycle, first coal-tar pitch is fully mixed with the first solvent, the method of employing physical sepn removes the first solvent insolubles in described mixture, obtain the first clear liquor, after hydrogenation is carried out to described first clear liquor, obtain refined asphaltic bitumen; Again described first solvent insolubles is fully mixed with matter oil in coal measures, the method of employing physical sepn removes the insolubles in described mixture, obtain the second clear liquor, remove in the coal measures in described second clear liquor and obtain refining heavy ends after matter oil, finally described refined asphaltic bitumen is mixed with described refining heavy ends, namely obtain the raw material for the preparation of needle coke.The present invention has abandoned the technology prejudice that heavy phase that existing technical staff thinks containing substantial quinoline-insoluble content and impurity ought to remove, by using matter oil in coal measures, described first solvent insolubles is extracted, effectively can extract how fragrant fused-ring aromatic composition wherein, refining heavy ends containing a large amount of how fragrant fused-ring aromatic composition is back to and prepares needle coke, effectively can improve the productive rate of described needle coke product.
(2) coal-tar pitch that utilizes described in the present invention prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, arranging described lightweight oil is coal measures lightweight oil, and the described coal measures lightweight oil of restriction is one or more in vapour light oil, BTX, tar light oil, petroleum naphtha further.Reason is to use this several oil to be suitable for the uncombined carbon in coal-tar pitch, solid impurity containing uncombined carbon and heavy ingredient effectively to separate.
(3) coal-tar pitch that utilizes described in the present invention prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, the method of the physical sepn that selection is arranged in described step (1) and (3) is centrifugation, and the centrifugal acceleration of described centrifugation is 2000-4000G.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 tar pitch raw material.In order to improve centrifugal effect further, it is 2200-3500G that the present invention also limits described centrifugal acceleration further.
Accompanying drawing explanation
More being convenient to make content of the present invention understand, below in conjunction with accompanying drawing embodiment, technical solutions according to the invention being described further;
That the coal-tar pitch that utilizes of the present invention prepares the schematic diagram of needle-shape coke raw material technique in conjunction with heavy phase recycle as shown in Figure 1.
Embodiment
embodiment 1
the coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing filtering separation removes the first solvent insolubles in described mixture, obtains the first clear liquor;
First solvent described in the present embodiment is petroleum petroleum naphtha, and the mass ratio of described first solvent and described coal-tar pitch is 0.1;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 410 DEG C, and reaction pressure is 22MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing filtering separation removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is used as the petroleum petroleum naphtha of the first solvent and the mixture of washing oil, and the mass ratio of described washing oil and described petroleum petroleum naphtha is 1:2; The mass ratio of described second solvent and described first solvent insolubles is 0.5;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 2
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) coal-tar pitch is fully mixed with the first solvent, adopt settlement separate method to remove the first solvent insolubles in described mixture, obtain the first clear liquor;
First solvent described in the present embodiment is petroleum petroleum naphtha, and the mass ratio of described first solvent and described coal-tar pitch is 15;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 410 DEG C, and reaction pressure is 22MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing filtering separation removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is used as the petroleum petroleum naphtha of the first solvent and the mixture absorbing oil, and absorbing oil with the mass ratio of described petroleum petroleum naphtha is 1:2; The mass ratio of described second solvent and described first solvent insolubles is 50;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 3
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) coal-tar pitch is fully mixed with the first solvent, adopt settlement separate method to remove the first solvent insolubles in described mixture, obtain the first clear liquor;
First solvent described in the present embodiment is petroleum petroleum naphtha, and the mass ratio of described first solvent and described coal-tar pitch is 0.4;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 400 DEG C, and reaction pressure is 5MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing filtering separation removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is used as the petroleum petroleum naphtha of the first solvent and the mixture absorbing oil, and absorbing oil with the mass ratio of described petroleum petroleum naphtha is 1:2; The mass ratio of described second solvent and described first solvent insolubles is 10;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 4
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) coal-tar pitch is fully mixed with the first solvent, adopt settlement separate method to remove the first solvent insolubles in described mixture, obtain the first clear liquor;
First solvent described in the present embodiment is petroleum petroleum naphtha, and the mass ratio of described first solvent and described coal-tar pitch is 10;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 400 DEG C, and reaction pressure is 20MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing filtering separation removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is used as the petroleum petroleum naphtha of the first solvent and the mixture absorbing oil, and described absorption oil is 1:2 with the mass ratio of described petroleum petroleum naphtha; The mass ratio of described second solvent and described first solvent insolubles is 1;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 5
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) coal-tar pitch is fully mixed with the first solvent, adopt settlement separate method to remove the first solvent insolubles in described mixture, obtain the first clear liquor;
First solvent described in the present embodiment is coal measures lightweight oil, and described coal measures lightweight oil is vapour light oil, and the mass ratio of described first solvent and described coal-tar pitch is 1;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 350 DEG C, and reaction pressure is 10MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing filtering separation removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is used as the vapour light oil of the first solvent and the mixture absorbing oil, and described absorption oil is 1:1.5 with the mass ratio of described vapour light oil; The mass ratio of described second solvent and described first solvent insolubles is 1;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient; The mass ratio of described second solvent and described first solvent insolubles is 5;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 6
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) coal-tar pitch is fully mixed with the first solvent, adopt settlement separate method to remove the first solvent insolubles in described mixture, obtain the first clear liquor;
First solvent described in the present embodiment is coal measures lightweight oil, and described coal measures lightweight oil is BTX, and the mass ratio of described first solvent and described coal-tar pitch is 0.3;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 320 DEG C, and reaction pressure is 12MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is coal measures vapour light oil and the mixture absorbing oil, and described absorption oil is 1:1.5 with the mass ratio of described vapour light oil; The mass ratio of described second solvent and described first solvent insolubles is 1;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 7
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing centrifugation removes the first solvent insolubles in described mixture, and obtain the first clear liquor, the centrifugal acceleration of described centrifugation is 2000G;
First solvent described in the present embodiment is coal measures lightweight oil, and described coal measures lightweight oil is the diesel oil distillate after the hydrotreatment of coal measures oil, and the mass ratio of described first solvent and described coal-tar pitch is 2;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 300 DEG C, and reaction pressure is 15MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing filtering separation removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is the mixture of coal measures tar light oil and carbolineum, and the mass ratio of described carbolineum and described tar light oil is 1:0.1; The mass ratio of described second solvent and described first solvent insolubles is 10;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 8
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing centrifugation removes the first solvent insolubles in described mixture, and obtain the first clear liquor, the centrifugal acceleration of described centrifugation is 4000G;
First solvent described in the present embodiment is coal measures lightweight oil, and described coal measures lightweight oil is the diesel oil distillate after the hydrotreatment of coal measures oil, and the mass ratio of described first solvent and described coal-tar pitch is 2;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 350 DEG C, and reaction pressure is 15MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor;
The second solvent selected in the present embodiment is the mixture of coal measures tar light oil and carbolineum, and the mass ratio of described carbolineum and described tar light oil is 1:1; The mass ratio of described second solvent and described first solvent insolubles is 1;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 9
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing centrifugation removes the first solvent insolubles in described mixture, and obtain the first clear liquor, the centrifugal acceleration of described centrifugation is 2200G;
First solvent described in the present embodiment is coal measures lightweight oil, and described coal measures lightweight oil is the diesel oil distillate after the hydrotreatment of coal measures oil, and the mass ratio of described first solvent and described coal-tar pitch is 0.5;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 330 DEG C, and reaction pressure is 15MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor;
Described second solvent is the mixture of coal measures tar light oil and creosote, and the mass ratio of described creosote and described tar light oil is 1:1; The mass ratio of described second solvent and described first solvent insolubles is 1;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
embodiment 10
The coal-tar pitch that utilizes described in the present embodiment prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing centrifugation removes the first solvent insolubles in described mixture, and obtain the first clear liquor, the centrifugal acceleration of described centrifugation is 3500G;
First solvent described in the present embodiment is coal measures lightweight oil, and described coal measures lightweight oil is vapour light oil, and the mass ratio of described first solvent and described coal-tar pitch is 0.5;
(2) be separated the first solvent in described first clear liquor of removing, carry out hydrogenation to the remaining component after described first solvent of removing, obtain refined asphaltic bitumen, the temperature of described hydrogenation reaction is 350 DEG C, and reaction pressure is 10MPa;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor;
Described second solvent is the mixture of coal measures tar light oil and carbolineum, and the mass ratio of described carbolineum and described tar light oil is 1:1; The mass ratio of described second solvent and described first solvent insolubles is 1;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
In the above-described embodiments, as preferred embodiment, described hydrogenation reaction is carried out under nickel molybdenum series hydrocatalyst existent condition, and described nickel molybdenum series hydrocatalyst is prepared from a catalyst support described active ingredient Ni and Mo load, and described carrier is Al
2o
3carrier, the selection of catalyzer described in the present invention is the conventional prior art in this area, therefore repeats no more in the present invention.In addition, the Ni-Mo series catalysts described in the present invention is commercially available product.Certainly, as selectable embodiment, also such as FeS can be selected
2deng the hydrogenation catalyst of other kind.
experimental example
In order to prove that technical solutions according to the invention have substantial technique effect compared to prior art, below in conjunction with specific experiment example, the technique effect of technical scheme of the present invention is described further.
The mensuration of experiment 1:QI content and hydrocarbon concentration
The QI content of the first clear liquor obtained after removal the first solvent insolubles in above-described embodiment step (1) is measured, result shows that the first clear liquor QI content in embodiment 1-10 is all lower than 0.01wt%, and the initial Q I concentration of the coal tar pitch raw material used in above-described embodiment is 5.2wt%.
Concentration for the preparation of the QI content in the raw material of needle coke and carbon and hydrogen described in obtaining in above-described embodiment measures, result show in embodiment 1-10 obtained for the preparation of the QI content in the raw material of needle coke all lower than 0.01wt%.The described concentration for the preparation of the carbon in the raw material of needle coke and hydrogen is as shown in the table:
Experiment 2: the mensuration of needle coke thermal expansivity and productive rate
When testing, described in obtaining in above-described embodiment, putting into for the preparation of the raw material of needle coke the coker preparing needle coke, 550 DEG C of condition Using Coke-ovens 5 hours, obtaining needle coke.
Described needle coke product is carried out graphitization processing under 1300 DEG C of conditions, and the thermal expansivity of the needle coke after greying is as shown in the table:
Needle coke productive rate when preparing needle coke to described raw material obtained above further measures, and obtains result as shown in the table:
comparative example
Have Substantial technical effect in order to further illustrate technical scheme described in the present invention compared to prior art, the present invention is provided with following comparative example:
(1) adopt the coal tar pitch raw material identical with embodiment, fully mixed by described coal-tar pitch with solvent, the method for employing filtering separation removes the solvent insolubles in described mixture, obtains clear liquor;
Solvent described in this comparative example is the mixture of aliphatic hydrocarbon and aromatic hydrocarbon, and the mass ratio of described aliphatic hydrocarbon and aromatic hydrocarbon is 1:1; Described solvent initial boiling point at ambient pressure about 160 DEG C, the quantity of distillate of described mixture before 310 DEG C is 97%(w/w)
(2) be separated the solvent in the described clear liquor of removing, namely obtain the raw material for the preparation of needle coke.
Described in obtaining in this comparative example, put into for the preparation of the raw material of needle coke the coker preparing needle coke, 550 DEG C of condition Using Coke-ovens 5 hours, obtain needle coke.
Described needle coke product is carried out graphitization processing under 1300 DEG C of conditions, and the thermal expansivity of the needle coke after greying is 1.5 × 10
-6/ DEG C.
Needle coke productive rate when needle coke prepared by the described raw material obtained this comparative example further measures, and the productive rate obtaining needle coke is 35%.
By above-mentioned more known, in comparative example, the thermal expansivity of needle coke adds 0.4-0.8 × 10 compared to embodiment
-6/ DEG C, when reality uses, this quality being enough to Graphite Electrodes prepared by needle coke is a greater impact; In addition, in comparative example, the productive rate of needle coke reduces 12-18% compared to embodiment, and the technical scheme in visible the present invention can significantly improve the productive rate of needle coke product, therefore, technical scheme in the present invention, compared to prior art, has obvious Substantial technical effect.
Although the present invention is elaborated it by embodiment; but; those skilled in the art should be understood that and made on this basis not exceed any form of claims and the change of details, all belong to invention which is intended to be protected.
Claims (16)
1. utilize coal-tar pitch to prepare a technique for needle-shape coke raw material in conjunction with heavy phase recycle, comprising:
(1) fully mixed with the first solvent by coal-tar pitch, the method for employing physical sepn removes the first solvent insolubles in described mixture, obtains the first clear liquor;
Described first solvent is lightweight oil, and the mass ratio of described first solvent and described coal-tar pitch is 0.1-15;
(2) be separated the first solvent in described first clear liquor of removing, hydrogenation carried out to the remaining component after described first solvent of removing, obtains refined asphaltic bitumen;
(3) fully mixed with the second solvent by the first solvent insolubles obtained in step (1), the method for employing physical sepn removes the second solvent insolubles in described mixture, obtains the second clear liquor;
Described second solvent is the mixture of matter oil in lightweight oil and coal measures, and in the coal measures in described second solvent, matter oil is 1:0.1-1:2 with the mass ratio of described lightweight oil; The mass ratio of described second solvent and described first solvent insolubles is 0.5-50;
(4) be separated the second solvent in described second clear liquor of removing, obtain refining heavy ingredient;
(5) by described refined asphaltic bitumen and described refining heavy ingredient mixing, the raw material for the preparation of needle coke is namely obtained.
2. the coal-tar pitch that utilizes according to claim 1 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the mass ratio of described first solvent and described coal-tar pitch is 0.4-10.
3. the coal-tar pitch that utilizes according to claim 1 and 2 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the mass ratio of described first solvent and described coal-tar pitch is 0.5-2.
4. the coal-tar pitch that utilizes according to claim 1 and 2 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, in described coal measures, matter oil is 1:0.1-1:1 with the mass ratio of described lightweight oil.
5. the coal-tar pitch that utilizes according to claim 3 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, in described coal measures, matter oil is 1:0.1-1:1 with the mass ratio of described lightweight oil.
6. the coal-tar pitch that utilizes according to claim 1 or 2 or 5 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the mass ratio of described second solvent and described first solvent insolubles is 1-10.
7. the coal-tar pitch that utilizes according to claim 3 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the mass ratio of described second solvent and described first solvent insolubles is 1-10.
8. the coal-tar pitch that utilizes according to claim 4 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the mass ratio of described second solvent and described first solvent insolubles is 1-10.
9. the coal-tar pitch that utilizes according to claim 1 or 2 or 5 or 7 or 8 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the lightweight oil in described first solvent and the second solvent is coal measures lightweight oil.
10. the coal-tar pitch that utilizes according to claim 9 prepares the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, described coal measures lightweight oil is one or more in vapour light oil, BTX, tar light oil, petroleum naphtha.
11. coal-tar pitches that utilize according to claim 1 or 2 or 5 or 7 or 8 or 10 prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, in described coal measures matter oil be washing oil, absorb in oil, creosote, carbolineum one or more.
12. coal-tar pitches that utilize according to claim 1 or 2 or 5 or 7 or 8 or 10 prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, and it is characterized in that, the temperature of described hydrogenation reaction is 300-400 DEG C, and pressure is 5-20MPa.
13. coal-tar pitches that utilize according to claim 1 or 2 or 5 or 7 or 8 or 10 prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, and it is characterized in that, hydrogenation catalyst is nickel molybdenum series catalyst.
14. coal-tar pitches that utilize according to claim 13 prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the temperature of described hydrogenation reaction is 300-350 DEG C, and pressure is 10-15MPa.
15. coal-tar pitches that utilize according to claim 1 or 2 or 5 or 7 or 8 or 10 or 14 prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, physical sepn in described step (1) and step (3) is centrifugation, and the centrifugal acceleration of described centrifugation is 2000-4000G.
16. coal-tar pitches that utilize according to claim 15 prepare the technique of needle-shape coke raw material in conjunction with heavy phase recycle, it is characterized in that, the centrifugal acceleration of described centrifugation is 2200-3500G.
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