CN115180612B - Production process of high-energy-density anode coke - Google Patents
Production process of high-energy-density anode coke Download PDFInfo
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- CN115180612B CN115180612B CN202210910982.2A CN202210910982A CN115180612B CN 115180612 B CN115180612 B CN 115180612B CN 202210910982 A CN202210910982 A CN 202210910982A CN 115180612 B CN115180612 B CN 115180612B
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- 239000000571 coke Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000002667 nucleating agent Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000011331 needle coke Substances 0.000 claims abstract description 19
- 238000004939 coking Methods 0.000 claims abstract description 16
- 238000005336 cracking Methods 0.000 claims abstract description 8
- 238000006482 condensation reaction Methods 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 59
- 230000005855 radiation Effects 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 4
- 238000004523 catalytic cracking Methods 0.000 claims description 3
- 239000010724 circulating oil Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000295 fuel oil Substances 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000002010 green coke Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007773 negative electrode material Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000010692 aromatic oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000011334 petroleum pitch coke Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Coke Industry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to the technical field of needle coke, in particular to a high-energy-density cathode coke production process. Specifically, raw oil and an intermediate phase nucleating agent are mixed and then used as coking raw materials, heat is exchanged with a heat exchanger, then the coking raw materials are heated by a heating furnace, and then the coking raw materials enter a coke tower to undergo cracking and condensation reactions, and the high-energy-density cathode coke is obtained through cracking by heat release and heat absorption. The intermediate phase nucleating agent adopted by the invention can increase the gram capacity of the finally prepared product, quicken the reaction rate and improve the product yield.
Description
Technical Field
The invention relates to the technical field of needle coke, in particular to a high-energy-density cathode coke production process.
Background
In recent years, new energy electric vehicles are rapidly applied and developed, but the endurance mileage is a key factor for restricting the popularization and development of the new energy electric vehicles. The improvement of the energy density of the battery is a necessary condition for helping the battery to extend the endurance, and the performance of the negative electrode material serving as one of the most main components of the power battery pack of the electric automobile directly influences whether the battery pack can work normally or not.
The cathode materials in the market at present are needle coke and common coke petroleum coke or pitch coke. The fish dragons are mixed and have uneven quality. Even if the product is needle coke product, the quality of the products of each manufacturer is uneven; even with the same product, there is a large difference in product quality due to the different locations in the coke drum. The capacity of the common Jiao Ke is below 345mAh/g, the gram capacity of a medium-low grade product in needle coke is below 353mAh/g, and the existing battery has the problem that the energy density and the quality stability are difficult to obtain good balance. In order to meet the requirements of high energy density and stable quality of batteries, in particular to the requirements of new energy power lithium ion batteries, the gram capacity of the negative electrode material is more than 358mAh/g, so that the development of a raw material of the negative electrode material of the lithium ion batteries with more excellent performance, namely a novel high energy density negative electrode coke, is urgent.
Disclosure of Invention
Aiming at the technical problem that the existing needle Jiao Chanpin g capacity is 353mAh/g or less, the invention provides a high-energy density cathode coke production process, and the raw oil is mixed with a mesophase nucleating agent to obtain a lithium battery cathode material with high g capacity.
The technical scheme of the invention is as follows:
The production process of high energy density cathode coke includes mixing material oil and intermediate phase nucleating agent as coking material, heat exchange with heat exchanger, heating in heating furnace, cracking in coke tower and condensation reaction, and heat release and heat absorption to crack.
Further, the raw oil is at least one selected from catalytic cracking oil and petroleum heavy oil.
Furthermore, the raw oil is firstly subjected to multiphase step separation before use, and substances which are unfavorable for generating needle coke, such as catalyst powder, free carbon, impurities, asphaltene, thermally stable low-carbon hydrocarbon and the like are removed.
Further, the mesophase nucleating agent is acicular Jiao Xifen, and is obtained by grinding needle coke by powder grinding equipment.
Further, at least one of needle Jiao Xuanzi needle Jiao Shengjiao, needle Jiao Duan post-coke, or graphite produced from needle coke used for preparing the mesophase nucleating agent is preferably needle coke green coke.
Further, the particle size D50 of the mesophase nucleating agent is 3.+ -. 0.5. Mu.m.
Further, the amount of the mesophase nucleating agent is 0.5% to 1.5%, preferably 1.0% based on the oil mass of the raw material.
Further, the specific steps are as follows:
(1) The raw oil enters a coking device, and then the mixture of the raw oil and the mesophase nucleating agent is sequentially sent into a diesel oil-raw oil heat exchanger and a wax oil-raw oil heat exchanger to exchange heat to 280 ℃;
(2) The mixture enters a raw material buffer tank, is boosted by a raw material pump, enters a convection section of a heating furnace, is preheated to 300 ℃, enters a fractionating tower, is contacted with hot oil gas from the top of the coke tower for heat exchange, and flows into the bottom of the fractionating tower together with heavy fraction above wax oil in the raw material oil and condensed circulating oil in the hot oil gas, is pumped by a feeding pump of the heating furnace, and is sent to a radiation section of the heating furnace for heating;
(3) The materials heated to the required temperature form high-temperature oil gas, and enter a coke tower to carry out cracking and condensation reaction, and finally high-energy density anode coke (needle coke) and coking oil gas are generated.
Further, deoxidized water is injected into the convection section, the radiation section and the radiation section of the heating furnace after the convection section, so as to prevent coking of the furnace tube.
Further, the heating of the radiant section of the heating furnace adopts temperature change control, and the temperature change range is 450-500 ℃, preferably 470-500 ℃.
Further, the coke tower pressure is controlled by pressure variation, the pressure variation range is 0.4-0.5MPa, the circulation ratio is controlled to be 0.4-0.5, and the circulation ratio is adjusted according to different production temperatures and different production pressures.
The invention has the beneficial effects that:
The invention adopts the raw oil and the intermediate phase nucleating agent to mix and prepare the high energy density cathode coke, and the intermediate phase nucleating agent can increase the gram capacity of the finally prepared product, quicken the reaction rate and improve the product yield.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic view of the structure of the coking unit of the present invention.
In the figure, a first raw material oil tank, a second raw material oil tank, a 3-diesel-raw material oil heat exchanger, a 4-wax oil-raw material oil heat exchanger, a 5-raw material buffer tank, a 6-heating furnace, a 7-first coke tower, an 8-second coke tower and a 9-fractionating tower are arranged.
Detailed Description
In order to better understand the technical solutions of the present invention, the following description will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
Example 1
The preparation method comprises the steps of preparing high-energy-density anode coke by taking essential aromatic oil obtained by subjecting catalytic cracking slurry oil to multiphase step separation treatment as raw oil and taking graphite powder manufactured by needle coke as an intermediate phase nucleating agent, wherein the particle size distribution of the intermediate phase nucleating agent meets the following table 1.
TABLE 1 particle size distribution (Unit: μm) of mesophase nucleators
| D10 | D50 | D90 | D[3,2] | D[4,3] | Span of span |
| 1.1 | 3.3 | 7.1 | 2.2 | 3.8 | 1.8 |
The preparation method comprises the following specific steps:
(1) The raw oil enters a first raw oil tank 1 and a second raw oil tank 2 and stays for 4 hours;
Then adding the intermediate phase nucleating agent into a second raw oil tank 2, mixing the intermediate phase nucleating agent with raw oil, and finally mixing the first raw oil tank 1 and the second raw oil tank 2 to obtain a mixture containing 1% of intermediate phase nucleating agent by the total mass of the raw oil, wherein the mixture sequentially enters a diesel-raw oil heat exchanger 3 and a wax oil-raw oil heat exchanger 4 to exchange heat to 280 ℃;
(2) The mixture enters a raw material buffer tank 5, is boosted by a raw material pump, enters a convection section of a heating furnace 6, is preheated to 300 ℃, and enters the bottom of a fractionating tower 9 and a sixth heat exchange plate in two paths to contact and exchange heat with 430 ℃ hot oil gas from the top of a coke tower;
the heavy fraction above wax oil in the raw oil and the condensed circulating oil in the hot oil gas flow into the bottom of the fractionating tower 9 together, are filtered at 340 ℃ and pumped by a feeding pump of a heating furnace, and are sent to a radiation section of the heating furnace 6 for heating;
Oxygen-removing water is respectively injected into the convection section, the radiation section and the radiation section of the heating furnace 6 so as to prevent the furnace tube from coking;
The heating of the radiation section of the heating furnace 6 adopts temperature change control, the temperature change range is 470-500 ℃, the feeding is started at 470 ℃, the temperature is increased to 485 ℃ for 4 hours, the feeding is performed at constant temperature for 9 hours, then the temperature is increased to 500 ℃ for 1 hour, and the feeding is continued at constant temperature for 10 hours;
(3) Through the convection section and the radiation section of the heating furnace 6, the materials are quickly heated to the required temperature and form high-temperature oil gas, the high-temperature oil gas enters the first coke tower 7 and the second coke tower 8 through the four-way valve, the pressure of the coke tower is controlled to be 0.5MPa before 485 ℃, then the pressure is adjusted to be 0.4MPa, the circulation ratio is controlled to be 0.5, the coke generation period is 48 hours, and the high-temperature oil gas is subjected to a series of reactions such as cracking, condensation, generation of mesophase pellets, compound pellets, wide area intermediate equality in the coke tower due to high temperature and long residence time, and anisotropic needle coke and coking oil gas are finally generated, so that the high-energy density cathode coke is obtained.
Example 2
The powder of needle Jiao Shengjiao is used as intermediate phase nucleating agent to prepare high energy density cathode coke, wherein the particle size distribution of the intermediate phase nucleating agent also satisfies table 1, and the raw oil and the specific preparation steps are the same as in example 1.
Example 3
The powder of needle Jiao Duan back coke is used as intermediate phase nucleating agent to prepare high energy density cathode coke, wherein the particle size distribution of the intermediate phase nucleating agent also satisfies table 1, and the raw oil and the specific preparation steps are the same as in example 1.
Comparative example 1
Needle coke was prepared without using mesophase nucleating agents, and the raw oil and the rest of the preparation steps were the same as in example 1.
Needle coke prepared in examples 1 to 3 and comparative example 1 was examined according to GB/T24533, and the results of the examination are shown in Table 2 below.
TABLE 2 needle coke detection results
| Project | True density g/cm3 | Volatile component% | Sulfur% | Graphitization degree% | Gram capacity mAh/g |
| Example 1 | 1.392 | 4.25 | 0.46 | 95.1 | 361.9 |
| Example 2 | 1.389 | 4.28 | 0.45 | 94.8 | 360.1 |
| Example 3 | 1.384 | 4.51 | 0.46 | 94.4 | 355.2 |
| Comparative example 1 | 1.381 | 4.73 | 0.47 | 94.5 | 354.0 |
It can be seen that when the mesophase nucleating agent is 1% acicular Jiao Danmo powder, the graphitization degree and gram capacity of the product are both higher, the requirement of the new energy power lithium ion battery can be met, but the cost of the graphite powder is higher. When the mesophase nucleating agent is 1% acicular Jiao Shengjiao fine powder, the index is basically close, the cost is lower, and the method can be widely applied.
Although the present invention has been described in detail by way of preferred embodiments, the present invention is not limited thereto. Various equivalent modifications and substitutions may be made in the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and it is intended that all such modifications and substitutions be within the scope of the present invention/be within the scope of the present invention as defined by the appended claims.
Claims (8)
1. The production process of the high-energy-density cathode coke is characterized in that raw oil and an intermediate phase nucleating agent are mixed to be used as coking raw materials, heat exchange is carried out between the coking raw materials and a heat exchanger, the coking raw materials are heated by a heating furnace, then the coking raw materials enter a coke tower to undergo cracking and condensation reactions, and the cracking is carried out through heat release and heat absorption to obtain the high-energy-density cathode coke;
Wherein the intermediate phase nucleating agent is acicular Jiao Xifen, and is obtained by grinding needle coke by powder grinding equipment; the dosage of the mesophase nucleating agent is 0.5% -1.5% based on the oil quality of the raw materials; at least one of needle Jiao Xuanzi needle Jiao Shengjiao, needle Jiao Duan post-coke, or graphite made from needle coke used to prepare the mesophase nucleating agent.
2. The process for producing high energy density anode coke according to claim 1, wherein the raw oil is at least one selected from the group consisting of catalytic cracking residual oil and petroleum heavy oil.
3. The process for producing high energy density anode coke according to claim 1, wherein the needle coke used for preparing the mesophase nucleating agent is needle coke green coke.
4. A process for the production of high energy density anode coke as claimed in claim 1, wherein the mesophase nucleating agent has a particle size D50 of 3±0.5 μm.
5. The process for producing a high energy density anode coke according to claim 1, wherein the amount of the mesophase nucleating agent is 1.0% based on the amount of the raw oil.
6. The process for producing the high-energy-density anode coke according to claim 1, which is characterized by comprising the following specific steps:
(1) The raw oil enters a coking device, and then the mixture of the raw oil and the mesophase nucleating agent is sequentially sent into a diesel oil-raw oil heat exchanger and a wax oil-raw oil heat exchanger to exchange heat to 280 ℃;
(2) The mixture enters a raw material buffer tank, is boosted by a raw material pump, enters a convection section of a heating furnace, is preheated to 300 ℃, enters a fractionating tower, is contacted with hot oil gas from the top of the coke tower for heat exchange, and flows into the bottom of the fractionating tower together with heavy fraction above wax oil in the raw material oil and condensed circulating oil in the hot oil gas, is pumped by a feeding pump of the heating furnace, and is sent to a radiation section of the heating furnace for heating;
(3) The materials heated to the required temperature form high-temperature oil gas, and enter a coke tower to carry out cracking and condensation reaction, and finally high-energy density anode coke and coking oil gas are generated.
7. The process for producing high energy density anode coke according to claim 1, wherein deoxygenated water is injected after the convection section, before the radiation section, and in the radiation section of the heating furnace.
8. The process for producing the high-energy-density anode coke according to claim 1, wherein the heating of the radiation section of the heating furnace adopts temperature change control, and the temperature change range is 450-500 ℃; the coke tower pressure is controlled by pressure variation, the pressure variation range is 0.4-0.5MPa, and the circulation ratio is controlled to be 0.4-0.5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560104A (en) * | 2013-10-23 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing needle coke |
| CN113004924A (en) * | 2021-04-15 | 2021-06-22 | 山东京阳科技股份有限公司 | Production process of needle coke for ultrahigh-power graphite electrode connector |
| CN114525153A (en) * | 2022-02-14 | 2022-05-24 | 深圳市翔丰华科技股份有限公司 | Preparation method of isotropic coke for lithium ion battery cathode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7604731B2 (en) * | 2004-06-25 | 2009-10-20 | Indian Oil Corporation Limited | Process for the production of needle coke |
| CN104560152B (en) * | 2013-10-23 | 2017-03-22 | 中国石油化工股份有限公司 | Coking process for production of needle coke |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560104A (en) * | 2013-10-23 | 2015-04-29 | 中国石油化工股份有限公司 | Method for producing needle coke |
| CN113004924A (en) * | 2021-04-15 | 2021-06-22 | 山东京阳科技股份有限公司 | Production process of needle coke for ultrahigh-power graphite electrode connector |
| CN114525153A (en) * | 2022-02-14 | 2022-05-24 | 深圳市翔丰华科技股份有限公司 | Preparation method of isotropic coke for lithium ion battery cathode material |
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