CN117264646A - Method for co-producing mesophase pitch and high-quality needle coke - Google Patents
Method for co-producing mesophase pitch and high-quality needle coke Download PDFInfo
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- CN117264646A CN117264646A CN202311460113.5A CN202311460113A CN117264646A CN 117264646 A CN117264646 A CN 117264646A CN 202311460113 A CN202311460113 A CN 202311460113A CN 117264646 A CN117264646 A CN 117264646A
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- 239000011302 mesophase pitch Substances 0.000 title claims abstract description 86
- 239000011331 needle coke Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000004939 coking Methods 0.000 claims abstract description 58
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000012719 thermal polymerization Methods 0.000 claims abstract description 31
- 239000000295 fuel oil Substances 0.000 claims abstract description 18
- 239000000571 coke Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000004062 sedimentation Methods 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000011280 coal tar Substances 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 239000003208 petroleum Substances 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 230000001502 supplementing effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 5
- 239000005977 Ethylene Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 239000011269 tar Substances 0.000 claims description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003350 kerosene Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims description 3
- 239000003502 gasoline Substances 0.000 claims description 3
- 239000011295 pitch Substances 0.000 claims description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 239000001273 butane Substances 0.000 claims description 2
- 238000005336 cracking Methods 0.000 claims description 2
- 238000005235 decoking Methods 0.000 claims description 2
- 239000002283 diesel fuel Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 2
- 239000003345 natural gas Substances 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 150000004950 naphthalene Chemical class 0.000 claims 1
- 239000013589 supplement Substances 0.000 abstract 1
- 239000010426 asphalt Substances 0.000 description 19
- 239000000203 mixture Substances 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000003111 delayed effect Effects 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007614 solvation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B55/00—Coking mineral oils, bitumen, tar, and the like or mixtures thereof with solid carbonaceous material
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Coke Industry (AREA)
Abstract
The invention relates to a method for co-producing mesophase pitch and high-quality needle coke, which uses heavy oil as a raw material, adopts a thermal polymerization-sedimentation-coking three-step method to co-produce the mesophase pitch and the needle coke, utilizes a thermal polymerization and sedimentation separation method to obtain the mesophase pitch with the anisotropic structure content of more than 90%, and enters a coking tower after being heated by a heating furnace, and utilizes a heating medium to pull coke and supplement heat to prepare the high-quality needle coke. The method can obtain low softening point mesophase pitch with anisotropic structure content more than 90% and high-quality needle coke with high relative crystallinity.
Description
Technical Field
The invention relates to a method for co-producing mesophase pitch and high-quality needle coke, which specifically uses heavy oil as a raw material to prepare the mesophase pitch and the high-quality needle coke with anisotropic structure content of more than 90% through a thermal polymerization-sedimentation-coking three-step method. Belongs to the technical field of preparation of novel high-quality carbon materials.
Background
Mesophase pitch is a mixture of multiple polycyclic aromatic hydrocarbons having a relative molecular mass of 370-2000, which has been established as an excellent precursor of carbon materials from which a number of high performance carbon materials, such as carbon fibers, thermally conductive materials, carbon composites, advanced battery electrodes, etc., can be manufactured. These high-grade carbon materials play a great role in many fields such as national defense industry, aerospace, daily life, etc.
Needle coke is coke with special properties generated in the thermal conversion process of coal-based or oil-based raw materials, and is a raw material for producing carbon products such as graphite electrodes, lithium battery cathode materials, carbon composite materials and the like. The carbon product prepared by the method has the characteristics of high purity, low ablation quantity, low thermal expansion coefficient and the like, so the carbon product is widely used in the fields of metallurgy, new energy sources and the like. The existing needle coke production devices all have the problem of unstable quality, including inconsistent quality of needle coke at the upper part, the middle part and the lower part in a single tower and unstable quality control of multi-tower needle coke. The analysis reasons are mainly because in the delayed coking process adopted in the preparation of the needle coke at present, a delayed coking device completes the whole process from heavy oil to needle coke preparation, the coking process is difficult to control due to the non-uniformity of the composition of the heavy oil, the quality of the needle coke is difficult to ensure, and meanwhile, the upper, middle and lower temperature distribution in a coking tower is uneven and the needle Jiao Lajiao process is not sufficiently controlled, so that the needle coke with stable quality and consistent morphological structure cannot be obtained.
The patents CN106635142, CN106544045, CN106147835 and CN104650938 disclose a process for preparing needle coke by a two-step method, and although pre-coking improves the content of anisotropic structure components of heavy asphalt entering a coking tower, the problem of lower content of anisotropic structure in the heavy asphalt exists, so that the quality of the subsequent needle coke is unstable. CN106544045 adopts mesophase pitch with anisotropic content of 25-80% as raw material, and adopts a two-step carbonization method to prepare needle coke, and the process needs solvation reaction, and has the advantages of complex reaction process and high energy consumption.
CN1132895C, CN1172147a adopts a two-stage coking method to prepare needle coke, and adopts light oil with heat to prepare needle coke by two-stage heating in a delayed coking device, and the heated light oil is inevitably polymerized to generate coke at high temperature, which affects the quality of needle coke products.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a co-production process method of mesophase pitch and needle coke, which uses heavy oil as raw materials and adopts a thermal polymerization-sedimentation-coking three-step method to co-produce the mesophase pitch with low softening point and the needle coke with high quality, wherein the anisotropic structure content of the mesophase pitch is more than 90 percent, and the invention adopts the following technical scheme to realize the purposes:
the method comprises the steps of taking heavy oil as a raw material, adopting a thermal polymerization-sedimentation-coking three-step method to co-produce mesophase pitch and needle coke, utilizing a thermal polymerization and sedimentation separation technology to obtain low-softening-point mesophase pitch with anisotropic structure content of more than 90%, heating the mesophase pitch by a heating furnace, then entering a coking tower, and utilizing the actions of pulling coke with a heat medium and supplementing heat to prepare high-quality needle coke.
The specific process comprises the following steps:
s1, heating heavy oil to a certain temperature by a heating furnace, and entering a thermal polymerization reactor to obtain mesophase pitch with an anisotropic structure of 20-50%;
s2: feeding 20-50% of mesophase pitch with an anisotropic structure into a settling tank to obtain low-softening-point mesophase pitch with the anisotropic structure content of more than 90%, and mixing the upper-layer pitch with heavy oil to be used as a feed of a thermal polymerization reactor;
s3: a part of the mesophase pitch is directly extracted from the bottom of the settling tank and is used as a mesophase pitch product; heating a part of mesophase pitch to a certain temperature by a heating furnace and then entering a coking tower; meanwhile, introducing a high-temperature belt heating medium at 500-550 ℃ into the bottom of the coking tower, and carrying out coke pulling and heat supplementing on mesophase pitch, so that high-quality needle coke is obtained, and the needle coke is discharged from a discharge port at the bottom of the coking tower after hydraulic decoking;
s4: oil gas and a coke pulling medium generated in the coking reaction process are discharged from the top of the reactor.
The preparation process of the mesophase pitch and the needle coke adopts a thermal polymerization-sedimentation-coking three-step method.
The preparation of the mesophase pitch adopts thermal polymerization and sedimentation separation technology.
The heavy oil is heated to 350-450 ℃ by a heating furnace.
And heating a part of the mesophase pitch to 490-530 ℃ by a heating furnace, and then entering a coking tower.
The needle coke is prepared by heating low-softening point mesophase pitch with anisotropic structure content of more than 90%, and then feeding the low-softening point mesophase pitch into a coking tower, and carrying out coke pulling and heat supplementing by using a heat medium.
The belt heating medium is water or N 2 At least one of methane, ethane, propane, butane, liquefied gas, natural gas, dry gas, coker gas, gasoline, aviation kerosene, kerosene and diesel oil.
The heavy oil is at least one selected from medium-low temperature coal tar, high temperature coal tar and fractions thereof, ethylene cracking tar and petroleum heavy fractions.
The heavy oil satisfies the requirements of asphaltene content less than 10%, sulfur content less than 0.5%, aromatic hydrocarbon content more than 50% and ash content less than 0.05%.
The thermal polymerization reaction temperature is 350-450 ℃, the reaction pressure is 0.5-5.5MPa, and the reaction time is 10-50h.
The temperature of the materials in the sedimentation tank is 300-400 ℃, the pressure is normal pressure, and the sedimentation time is 2-5h.
The temperature in the coking tower is 490-530 ℃, the pressure is 0-1Mpa, and the coking time is 2-8h.
In the thermal polymerization reactor, heavy oil is quickly reacted at high temperature (350-450 ℃) and high pressure (0.5-5.5 Mpa) to obtain mesophase pellets and fused mesophase pitch, and in order to avoid further polycondensation of the mesophase pitch at high temperature to form a product with a high softening point and carbon powder, when the anisotropic structure of the mesophase pitch is 20-50%, the mesophase pitch is pumped into a low-temperature sedimentation tank for sedimentation.
In the sedimentation tank, the mesophase pitch is settled at low temperature (300-400 ℃) and normal pressure, the low temperature is beneficial to slowing down the polymerization speed and degree of the mesophase pitch, the mesophase pitch with lower softening point is obtained, meanwhile, the phenomenon that carbon powder is formed by excessive carbonization to block a pipeline can be avoided, and the normal pressure can enable light components in the system to escape from a reaction system, so that the distance between mesophase pellets is reduced, and the fusion and growth of the mesophase pellets are facilitated. Through sedimentation, low softening point mesophase pitch with an anisotropic structure content of more than 90% can be obtained, and the mesophase pitch can be sold as a product for downstream mesophase pitch-based carbon fibers, mesophase pitch and foam carbon, mesophase pitch-based electrode materials and other mesophase pitch-based carbon/carbon composites.
In the coking tower, the low softening point mesophase pitch with the anisotropic structure content of more than 90 percent is deeply carbonized at high temperature (490-530 ℃) and low pressure (0-1 Mpa); the intermediate phase pitch with the anisotropic structure content of more than 90% is further carbonized to prepare needle coke, so that the feeding consistency of the coking tower is ensured, the quality stability of the needle coke can be greatly improved, meanwhile, the hot medium is injected to carry out coke pulling and heat supplementing, the problems of uniformity and heat supply uniformity of the needle Jiao Lajiao can be effectively solved by injecting the hot medium, volatile matters are facilitated to be separated out, the needle coke with consistent morphological structure is obtained, the heat supplementing energy of the hot medium enables the upper, middle and lower temperature distribution of the coke tower to be relatively uniform, and the uniformity of the quality of the upper, middle and lower needle coke products of the coke tower is improved.
Compared with the existing preparation method, the invention has the beneficial effects that:
(1) The invention relates to a three-step method for co-producing mesophase pitch and high-quality needle coke, which has larger market fluctuation of the carbon material at present, can adjust products in time according to the market, and improves the capability of the device for resisting risks.
(2) The preparation of the mesophase pitch divides thermal polymerization and sedimentation into two steps, and the thermal polymerization reactor and the sedimentation tank are independently controlled by combining the thermal polymerization and the sedimentation separation, so that the low-softening-point mesophase pitch with the anisotropic structure content of more than 90 percent can be prepared.
(3) And the preparation of the needle coke takes low-softening point mesophase pitch with anisotropic structure content more than 90% as the feeding of the coking tower, so that the feeding consistency can be ensured, the quality of the needle coke is improved, and the stability of the quality of the needle coke is ensured.
(4) At present, the domestic industrial needle coke production device basically does not have injection of a heat medium, the injection of the heat medium can effectively solve the problems of uniformity and heat supply uniformity of needle Jiao Lajiao, and mesophase molecules are orderly arranged and solidified under the action of airflow shearing force to generate needle coke products with higher crystallinity.
Drawings
FIG. 1 is a process flow diagram of the co-production of mesophase pitch and high quality needle coke according to the present invention.
In the figure: 1-thermal polymerization reactor 2-settling tank 3-coking tower P-1, P-2, P-3-pump E-1, E-2, E-3-heat exchanger.
Detailed Description
The method for co-producing mesophase pitch and high-quality needle coke by using heavy oil as a raw material through a three-step method is further described below by combining examples.
Example 1:
heating low-temperature coal tar with 4% of asphaltene, 0.32% of sulfur, 65% of aromatic hydrocarbon and 0.02% of ash content, then feeding the heated low-temperature coal tar into a thermal polymerization reactor, controlling the reaction temperature of the thermal polymerization reactor to 350 ℃, controlling the reaction pressure to 0.5Mpa, feeding the heated low-temperature coal tar into a settling tank after reacting for 50 hours, controlling the temperature of the settling tank to 300 ℃, settling the mixture for 5 hours, mixing isotropic asphalt at the upper part of the settling tank with raw materials, heating the mixture, feeding the mixture into the thermal polymerization reactor, obtaining low-softening-point mesophase pitch at the bottom, directly selling a part of mesophase pitch products as products according to market needs, feeding a part of mesophase pitch into a coking tower for coking, heating and pulling the mesophase pitch by superheated steam with a thermal medium, controlling the temperature in the coking tower to be 530 ℃, coking the pressure to be 1MPa for 2 hours, obtaining needle coke products, and carrying out property analysis on the calcined needle coke products, wherein the properties of the mesophase pitch and the needle coke (calcined) are shown in table 1.
Example 2
Heating high-temperature coal tar with 6% of asphaltene, 0.37% of sulfur, 75% of aromatic hydrocarbon and 0.04% of ash content, then feeding the heated high-temperature coal tar into a thermal polymerization reactor, controlling the reaction temperature of the thermal polymerization reactor to 400 ℃, controlling the reaction pressure to 2.5Mpa, feeding the heated high-temperature coal tar into a settling tank after reacting for 20 hours, controlling the temperature of the settling tank to 350 ℃, setting the settling pressure to normal pressure, mixing isotropic asphalt at the upper part of the settling tank with raw materials, heating the mixture, feeding the mixture into the thermal polymerization reactor, obtaining low-softening-point mesophase pitch at the bottom, according to market requirements,part of the intermediate phase asphalt product is directly sold as a product, and part of the intermediate phase asphalt enters a coking tower to be coked, and is superheated N through a heat medium 2 Heating and drawing the mesophase pitch, controlling the temperature in a coking tower to be 500 ℃, controlling the pressure to be 0.5MPa, and coking for 6 hours to obtain needle coke products, wherein the properties of the calcined needle coke products are analyzed, and the properties of the mesophase pitch and the needle coke (after calcination) are shown in table 1.
Example 3
Heating ethylene tar with 5% of asphaltene, 0.35% of sulfur, 65% of aromatic hydrocarbon and 0.01% of ash content, then feeding the heated ethylene tar into a thermal polymerization reactor, controlling the reaction temperature of the thermal polymerization reactor to 450 ℃, controlling the reaction pressure to 5.5Mpa, feeding the heated ethylene tar into a settling tank after reacting for 10 hours, controlling the temperature of the settling tank to 400 ℃, setting the settling pressure to normal pressure, mixing isotropic asphalt at the upper part of the settling tank with raw materials, heating the mixture, feeding the mixture into the thermal polymerization reactor, obtaining low-softening-point mesophase pitch at the bottom, directly selling a part of mesophase pitch products as products according to market requirements, feeding a part of mesophase pitch into a coking tower for coking, heating and pulling the mesophase pitch by using superheated gasoline with a thermal medium, controlling the temperature in the coking tower to 490 ℃ and the pressure to 0MPa, coking for 8 hours, obtaining needle coke products, calcining the needle coke products, and then carrying out property analysis on the mesophase pitch and the needle coke (calcined) properties are shown in table 1.
Example 4
Heating heavy petroleum fractions with 3% of asphaltene, 0.35% of sulfur, 72% of aromatic hydrocarbon and 0.01% of ash content, then feeding the heavy petroleum fractions into a thermal polymerization reactor, controlling the reaction temperature of the thermal polymerization reactor to 450 ℃, controlling the reaction pressure to 1.0Mpa, feeding the heavy petroleum fractions into a settling tank after reacting for 30 hours, controlling the temperature of the settling tank to 420 ℃, setting the settling pressure to normal pressure, mixing isotropic asphalt at the upper part of the settling tank with raw materials, heating the mixture, feeding the mixture into the thermal polymerization reactor, obtaining low-softening-point mesophase asphalt at the bottom, directly selling a part of mesophase asphalt products as products according to market requirements, feeding a part of mesophase asphalt into a coking tower for coking, heating and pulling the mesophase asphalt by using hot medium-carrying overheated methane, controlling the temperature in the coking tower to 520 ℃ and the pressure to 0.2MPa, coking for 4 hours, obtaining needle coke products, calcining the needle coke products, and carrying out property analysis on the mesophase asphalt and the needle coke (calcined) properties are shown in table 1.
Comparative example 1
Heating heavy petroleum fraction with 3% of asphaltene, 0.35% of sulfur, 72% of aromatic hydrocarbon and 0.01% of ash content by a heating furnace, entering a coking tower, controlling the temperature in the coking tower to 520 ℃ and the pressure to 0.2MPa, coking for 4 hours to obtain needle coke products, calcining the needle coke products, and performing property analysis, wherein the properties of the needle coke (calcined) are shown in table 1.
Comparative example 2
Heating heavy petroleum fractions with 3% of asphaltene content, 0.35% of sulfur content, 72% of aromatic hydrocarbon content and 0.01% of ash content, then feeding the heavy petroleum fractions into a thermal polymerization reactor, controlling the reaction temperature of the thermal polymerization reactor to 450 ℃, controlling the reaction pressure to 1.0Mpa, feeding the heavy petroleum fractions into a settling tank after 30 hours of reaction, controlling the temperature of the settling tank to 420 ℃, setting the settling pressure to normal pressure, mixing isotropic asphalt at the upper part of the settling tank with raw materials, heating the mixture into the thermal polymerization reactor, obtaining low-softening-point mesophase asphalt at the bottom, directly selling a part of mesophase asphalt products as products according to market requirements, feeding a part of mesophase asphalt into a coking tower for coking, heating the mesophase asphalt to 520 ℃ through a heating furnace, controlling the pressure to 0.2Mpa, coking for 4 hours, obtaining needle coke products, calcining the needle coke products, and carrying out property analysis on the mesophase asphalt and the needle coke (calcined) properties are shown in table 1.
Table 1 mesophase pitch and needle coke (calcined) properties
Claims (10)
1. A method for co-producing mesophase pitch and high-quality needle coke uses heavy oil as raw material, adopts a thermal polymerization-sedimentation-coking three-step method to co-produce mesophase pitch and needle coke, utilizes thermal polymerization and sedimentation separation technology to obtain mesophase pitch with anisotropic structure content of more than 90%, and makes the mesophase pitch enter a coking tower after being heated by a heating furnace, and utilizes the actions of pulling coke with heat medium and supplementing heat to prepare high-quality needle coke;
the method is characterized by comprising the following steps of:
s1, heating heavy oil to 350-450 ℃ by a heating furnace, and entering a thermal polymerization reactor to obtain mesophase pitch with an anisotropic structure of 20-50%;
s2: feeding 20-50% of mesophase pitch with an anisotropic structure into a settling tank to obtain low-softening-point mesophase pitch with the anisotropic structure content of more than 90%, and mixing the upper-layer pitch with heavy oil to be used as a feed of a thermal polymerization reactor;
s3: a part of the mesophase pitch is directly extracted from the bottom of the settling tank and is used as a mesophase pitch product; heating a part of mesophase pitch to 490-530 ℃ by a heating furnace, and then entering a coking tower; meanwhile, introducing a high-temperature belt heating medium at 500-550 ℃ into the bottom of the coking tower, and carrying out coke pulling and heat supplementing on mesophase pitch, so that high-quality needle coke is obtained, and the needle coke is discharged from a discharge port at the bottom of the coking tower after hydraulic decoking;
s4: oil gas and a coke pulling medium generated in the coking reaction process are discharged from the top of the reactor.
2. The method for co-producing mesophase pitch and high-quality needle coke as claimed in claim 1, wherein the preparation process of mesophase pitch and needle coke adopts a thermal polymerization-sedimentation-coking three-step method.
3. The method for co-producing mesophase pitch and high-quality needle coke as claimed in claim 1, wherein said mesophase pitch is produced by thermal polymerization and sedimentation separation techniques.
4. The method for co-producing mesophase pitch and high-quality needle coke according to claim 1, wherein the needle coke is prepared by heating low-softening point mesophase pitch with anisotropic structure content of more than 90%, and then feeding the low-softening point mesophase pitch into a coking tower, and carrying out coke pulling and heat supplementing by using a heat medium.
5. The method for co-producing mesophase pitch and high-quality needle coke according to claim 1, wherein the heated medium is water, N 2 At least one of methane, ethane, propane, butane, liquefied gas, natural gas, dry gas, coker gas, gasoline, aviation kerosene, kerosene and diesel oil.
6. The method for co-producing mesophase pitch and high-quality needle coke according to claim 1, wherein the heavy oil is at least one selected from the group consisting of medium-low temperature coal tar, high temperature coal tar and fractions thereof, naphthalene compounds, ethylene cracking tar and petroleum heavy fractions.
7. The method for co-producing mesophase pitch and high-quality needle coke of claim 1, wherein said heavy oil has an asphaltene content of less than 10%, a sulfur content of less than 0.5%, an aromatic hydrocarbon content of more than 50% and an ash content of less than 0.05%.
8. The method for co-producing mesophase pitch and high-quality needle coke according to claim 1, wherein the thermal polymerization reaction temperature is 350-450 ℃, the reaction pressure is 0.5-5.5MPa, and the reaction time is 10-50h.
9. The method for co-producing mesophase pitch and high-quality needle coke according to claim 1, wherein the temperature of the materials in the settling tank is 300-400 ℃, the pressure is normal pressure, and the settling time is 2-5h.
10. The method for co-producing mesophase pitch and high-quality needle coke according to claim 1, wherein the temperature in the coking tower is 490-530 ℃, the pressure is 0-1Mpa, and the coking time is 2-8h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311460113.5A CN117264646A (en) | 2023-11-03 | 2023-11-03 | Method for co-producing mesophase pitch and high-quality needle coke |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311460113.5A CN117264646A (en) | 2023-11-03 | 2023-11-03 | Method for co-producing mesophase pitch and high-quality needle coke |
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| CN202311460113.5A Pending CN117264646A (en) | 2023-11-03 | 2023-11-03 | Method for co-producing mesophase pitch and high-quality needle coke |
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| Country | Link |
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| CN (1) | CN117264646A (en) |
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