CN109082301B - Production process and production device of anode material coke - Google Patents
Production process and production device of anode material coke Download PDFInfo
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- CN109082301B CN109082301B CN201811039657.3A CN201811039657A CN109082301B CN 109082301 B CN109082301 B CN 109082301B CN 201811039657 A CN201811039657 A CN 201811039657A CN 109082301 B CN109082301 B CN 109082301B
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- coking
- heavy oil
- graphite powder
- oil
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- 239000000571 coke Substances 0.000 title claims abstract description 36
- 239000010405 anode material Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 238000004939 coking Methods 0.000 claims abstract description 78
- 239000000295 fuel oil Substances 0.000 claims abstract description 69
- 239000003921 oil Substances 0.000 claims abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 230000003111 delayed effect Effects 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000010406 cathode material Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000007773 negative electrode material Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 8
- 239000010426 asphalt Substances 0.000 claims description 8
- 238000005235 decoking Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 4
- 239000003034 coal gas Substances 0.000 claims description 4
- 238000005194 fractionation Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 7
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 229910021383 artificial graphite Inorganic materials 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 239000011331 needle coke Substances 0.000 description 4
- 239000002006 petroleum coke Substances 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000002931 mesocarbon microbead Substances 0.000 description 3
- 229910021382 natural graphite Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010724 circulating oil Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G55/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one refining process and at least one cracking process
- C10G55/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one refining process and at least one cracking process plural serial stages only
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Coke Industry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The production process of negative electrode material coke includes adding high purity graphite powder into delayed coking mixed oil, and coking to obtain negative electrode material coke; the heavy oil recovery device comprises a fractionating tower, and is characterized by further comprising a heavy oil intermediate tank, wherein a heavy oil inlet of the heavy oil intermediate tank is connected with a heavy oil extraction outlet of the fractionating tower, a material outlet of the heavy oil intermediate tank is connected with an inlet at the bottom of the fractionating tower through a pipeline and a heavy oil pump, the heavy oil intermediate tank is provided with a tank heater and a stirrer, and a graphite powder feed inlet is further formed in the heavy oil intermediate tank. The invention adds high-purity graphite powder, adopts low-quinoline insoluble and low-ash raw materials, and ensures the purity of the anode material coke. The coking process of the raw materials is changed by adjusting the proportion of the high-purity graphite powder, the microstructure of the anode material coke is changed, and the production requirements of different types of anode materials are met. The device is improved on the basis of the existing mature device, can realize continuous production of cathode material coke, and has high production efficiency.
Description
Technical Field
The invention relates to the field of production of anode materials, in particular to a production process and a production device of anode material coke.
Background
The lithium ion battery has the advantages of high specific energy, long cycle life, no memory effect and the like, and along with the rapid development of various electronic products and the policy encouragement of the national policy on new energy automobile industry, the lithium ion battery industry is bound to continuously develop at high speed in the future, and brings greater opportunity for the cathode material industry, but also brings higher requirements.
The cathode material is one of key factors for determining the performance of the lithium ion battery, and the main market of the cathode material is carbon cathode materials at present, and the carbon cathode materials mainly comprise natural graphite, mesocarbon microbeads (MCMB), needle coke, petroleum coke, metallurgical coke and the like. The natural graphite particles have uneven surface reactivity, larger grain size, easily damaged crystal structure in the charge and discharge process, have the defects of low first cycle efficiency, poor rate capability and the like, and can basically meet the requirements of consumer electronic products on the performance of small batteries through technical treatments such as coating, surface modification and the like. The MCMB particle has the advantages of uniform graphite structure edge, uniform reactivity, high first cycle efficiency, excellent multiplying power performance and the like, but has no obvious advantage compared with artificial graphite in overall performance, high manufacturing cost and low market occupation ratio. The existing artificial graphite obtained by high-temperature graphitization of needle coke, petroleum coke, metallurgical coke and the like is modified, the defect of natural graphite is improved to a certain extent, the market share is relatively high, but the artificial graphite raw material needle coke, petroleum coke, metallurgical coke and other carbon materials are mainly applicable to the fields of graphite electrodes, carburant, iron and steel smelting and the like due to the special microstructure and performance of the artificial graphite raw material needle coke, petroleum coke, metallurgical coke and other carbon materials, are not specially developed and produced for negative electrode materials, and the inherent material structure of the artificial graphite is used for making the artificial graphite have certain defect in the aspect of lithium ion battery application, cannot meet the higher requirements of the future lithium ion battery development on the negative electrode materials, particularly cannot meet the requirements of higher capacity, longer cycle life, higher safety performance and the like in the aspect of power battery application, so that the special carbon material with a more stable structure and more applicable to the negative electrode materials needs to be developed.
Disclosure of Invention
The invention provides a production process and a production device of anode material coke aiming at the defects of the existing anode material. The process is characterized in that the device is improved on the basis of a mature delayed coking process, high-purity graphite powder is added into the delayed coking mixed oil, the anode material coke is obtained through coking, the produced anode material coke has high purity and is easy to graphitize, and the prepared anode material has the advantages of stable structure, high capacity, good multiplying power performance, high safety performance and the like in the application process of the lithium ion battery, and meets the higher requirements of the development of the lithium ion battery.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a production process of anode material coke comprises the steps of adding high-purity graphite powder into delayed coking mixed oil, and coking to obtain the anode material coke, wherein the specific process comprises the following steps:
1) Preheating raw materials: the coking raw material is pumped out by a pump through a coking raw material tank, preheated by a heating furnace and enters the bottom of a fractionating tower;
2) Adding graphite powder and mixing: adding high-purity graphite powder into a heavy oil intermediate tank, uniformly mixing the high-purity graphite powder with coked heavy oil extracted from a fractionating tower, pumping the mixture to the bottom of the fractionating tower, and mixing the mixture with coked raw materials and heavy oil at the bottom of the fractionating tower to obtain coked mixed oil;
3) Delayed coking: the mixed oil is pumped to a coking heating furnace, heated by the heating furnace and enters a delayed coking tower for coking;
4) Fractionating by a fractionating tower and mixing coking raw oil: high-temperature oil gas generated by coking in a coking tower enters the bottom of a fractionating tower, coked heavy oil, light oil and coal gas are obtained through fractionation, part of the heavy oil is extracted to a heavy oil intermediate tank, and the other part of the heavy oil is extracted as a byproduct;
5) Decoking: and (3) after feeding the material for 24 to 72 hours in the delayed coking tower, stopping feeding, and carrying out hydraulic decoking and drying to obtain the cathode material coke.
The granularity of the high-purity graphite powder is 0-20 mu m, and the purity is more than 99%.
The adding proportion of the high-purity graphite powder is 0.1-30% of the heavy oil mass.
The coking raw material is one or two of coal-series asphalt and petroleum-series asphalt.
The quinoline insoluble content of the coking raw material is 0-0.5%, and the ash content is 0-0.5%.
In the step 3), the main technological parameters of the delayed coking are as follows: the coking temperature in the coking tower is 450-550 ℃, the coking pressure is 0-1.0 MPa, and the circulation ratio is 0.2-2.
The device comprises a coking tower, a heating furnace and a fractionating tower; the heavy oil recovery device comprises a fractionating tower, and is characterized by further comprising a heavy oil intermediate tank, wherein a heavy oil inlet of the heavy oil intermediate tank is connected with a heavy oil extraction outlet of the fractionating tower, a material outlet of the heavy oil intermediate tank is connected with an inlet at the bottom of the fractionating tower through a pipeline and a heavy oil pump, the heavy oil intermediate tank is provided with a tank heater and a stirrer, and a graphite powder feed inlet is further formed in the heavy oil intermediate tank.
The number of the heavy oil intermediate tanks is two, and the mixing materials and the feeding materials are alternately used.
Compared with the prior art, the invention has the beneficial effects that:
1) High-purity graphite powder is added, and raw materials with low quinoline insoluble substances and low ash are adopted, so that the purity of the anode material coke is ensured.
2) The coking process of the raw materials is changed by adjusting the proportion of the high-purity graphite powder, the microstructure of the anode material coke is changed, and the production requirements of different types of anode materials are met.
3) The device is improved on the basis of the existing mature device, can realize continuous production of cathode material coke, and has high production efficiency.
Drawings
Fig. 1 is a process flow diagram of the present invention.
In the figure: 1-heating furnace, 2-coking tower, 3-fractionating tower, 4-heavy oil intermediate tank, 5-coking raw material tank, 6-heavy oil pump, 7-coking raw material pump, 8-feeding pump, 9-circulating oil pump, 10-heavy oil pipeline, 11-heavy oil extraction line, 12-light oil, gas extraction line, 13-negative electrode material coke, 14-oil gas line and 15-graphite powder feed inlet.
Detailed Description
Embodiments of the present invention are further described below with reference to the accompanying drawings:
as shown in fig. 1, a process for producing anode material coke comprises adding high-purity graphite powder into delayed coking mixed oil, and coking to obtain anode material coke, wherein the specific process comprises the following steps:
1) Preheating raw materials: the coking raw materials are pumped out by a pump through a coking raw material tank 5, preheated by a heating furnace 1 and then enter the bottom of a fractionating tower 3;
2) Adding graphite powder and mixing: adding high-purity graphite powder into a heavy oil intermediate tank 4, uniformly mixing with coked heavy oil extracted from a fractionating tower 3, pumping to the bottom of the fractionating tower 3, and mixing with coked raw materials and heavy oil at the bottom of the fractionating tower to obtain coked mixed oil;
3) Delayed coking: the mixed oil is pumped to a coking heating furnace 1, heated by the heating furnace 1 and enters a delayed coking tower 2 for coking;
4) Fractionating tower 3 fractionates and coked raw oil is mixed: high-temperature oil gas generated by coking in the coking tower 2 enters the bottom of the fractionating tower 3, coked heavy oil, light oil and coal gas are obtained through fractionation, part of the heavy oil is extracted to the heavy oil intermediate tank 4, and the other part is extracted as a byproduct;
5) Decoking: and (3) after feeding the material for 24 to 72 hours in the delayed coking tower 2, stopping feeding, and obtaining the cathode material coke after hydraulic decoking and drying.
The granularity of the high-purity graphite powder is 0-20 mu m, and the purity is more than 99%.
The adding proportion of the high-purity graphite powder is 0.1-30% of the heavy oil mass.
The coking raw material is one or two of coal-series asphalt and petroleum-series asphalt. Wherein the petroleum asphalt comprises petroleum asphalt, catalytic cracking slurry oil, ethylene residue oil and the like.
The quinoline insoluble content of the coking raw material is 0-0.5%, and the ash content is 0-0.5%.
In the step 3), the main technological parameters of the delayed coking are as follows: the coking temperature in the coking tower 2 is 450-550 ℃, the coking pressure is 0-1.0 MPa, and the circulation ratio is 0.2-2.
The device used in the production process of the cathode material coke comprises a coking tower 2, a heating furnace 1 and a fractionating tower 3; the heavy oil recycling device is characterized by further comprising a heavy oil intermediate tank 4, wherein a heavy oil inlet of the heavy oil intermediate tank 4 is connected with a heavy oil extraction line of the fractionating tower 3, a mixed oil recycling pipeline formed by a recycling oil pump 9 and a recycling pipeline is arranged at the bottom of the fractionating tower 3, a material outlet of the heavy oil intermediate tank 4 is connected with the mixed oil recycling pipeline at the bottom of the fractionating tower 3 through a pipeline and a heavy oil pump 6, the heavy oil intermediate tank 4 is provided with a tank heater and a stirrer, and a graphite powder feeding port 15 is further arranged on the heavy oil intermediate tank 4.
The number of the heavy oil intermediate tanks 4 is two, and the mixing materials and the feeding materials are alternately used.
The coking raw material tank 5 is connected with the heating furnace 1 through the coking raw material pump 7, and a coking raw material outlet of the heating furnace 1 is connected with a coking raw material inlet at the bottom of the fractionating tower 3 through a pipeline. The mixed oil outlet at the bottom of the fractionating tower 3 is connected with the heating furnace 1 through a pipeline and the feed pump 8, and the mixed oil outlet of the heating furnace 1 is connected with the coking tower 2 through a pipeline. The oil gas line 14 of the coking tower 2 is connected with a high-temperature oil gas inlet at the bottom of the fractionating tower 3, and the bottom of the coking tower 2 is provided with negative electrode material coke.
Adding high-purity graphite powder into a heavy oil intermediate tank 4, uniformly mixing with coked heavy oil, conveying the mixture to the bottom of a fractionating tower 3 through a heavy oil pump 6, uniformly mixing coked raw materials at the bottom of the fractionating tower 3 and heavy oil containing the high-purity graphite powder through a circulating oil pump 9, mixing the mixture into coked mixed oil, heating the coked mixed oil through a heating furnace 1, and conveying the coked mixed oil into a coking tower 2 for delayed coking.
The heavy oil is extracted to the No. 2 tank, high-purity graphite powder enters from a graphite powder feeding port 15 on the top of the No. 2 tank, and the heavy oil and the high-purity graphite powder are mixed according to a proportion and are uniformly mixed for standby by tank stirring; and after the feeding of the No. 1 tank is finished, the feeding of the No. 2 tank is switched, the No. 1 tank is a batching tank, and the No. 2 tank is a feeding tank, so that the continuous feeding of graphite powder and heavy oil is realized alternately.
High-temperature oil gas generated by coking in a coking tower 2 enters the bottom of a fractionating tower 3, coked heavy oil, light oil and coal gas are obtained through fractionation, part of heavy oil is extracted to a heavy oil intermediate tank 4 through a heavy oil pipeline 10, and part of heavy oil is extracted as a byproduct by a heavy oil extraction line 11; the light oil and gas are extracted from the light oil and gas extraction line 12.
[ example ]
The production process and the production device of the anode material coke, provided by the invention, record main indexes of 6 batches as shown in table 1:
table 1 raw materials and main index for each batch
Examples delayed coking main process parameters are shown in table 2:
TABLE 2 Main Process parameters for delayed coking
The main indexes of the anode material coke products obtained in the example 6 batches are shown in Table 3:
TABLE 3 Main index of cathode material coke
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the invention in any way, and any simple modification, equivalent changes and variations made according to the technical spirit and concept of the present invention will still fall within the scope of the technical solutions of the present invention, unless the technical solutions of the present invention are separated.
Claims (4)
1. A production process of anode material coke is characterized in that high-purity graphite powder is added into delayed coking mixed oil, and the anode material coke is obtained through coking, and the specific process steps comprise:
1) Preheating raw materials: the coking raw material is pumped out by a pump through a coking raw material tank, preheated by a heating furnace and enters the bottom of a fractionating tower;
2) Adding graphite powder and mixing: adding high-purity graphite powder into a heavy oil intermediate tank, uniformly mixing the high-purity graphite powder with coked heavy oil extracted from a fractionating tower, pumping the mixture to the bottom of the fractionating tower, and mixing the mixture with coked raw materials and heavy oil at the bottom of the fractionating tower to obtain coked mixed oil;
3) Delayed coking: the mixed oil is pumped to a coking heating furnace, heated by the heating furnace and enters a delayed coking tower for coking;
4) Fractionating by a fractionating tower and mixing coking raw oil: high-temperature oil gas generated by coking in a coking tower enters the bottom of a fractionating tower, coked heavy oil, light oil and coal gas are obtained through fractionation, part of the heavy oil is extracted to a heavy oil intermediate tank, and the other part of the heavy oil is extracted as a byproduct;
5) Decoking: feeding the material for 24-72 hours in a delayed coking tower, stopping feeding, and performing hydraulic decoking and drying to obtain cathode material coke;
the granularity of the high-purity graphite powder is 0-20 mu m, and the purity is more than 99%;
the adding proportion of the high-purity graphite powder is 0.1-30% of the heavy oil.
2. The process for producing a negative electrode material coke according to claim 1, wherein the coking raw material is one or two of coal-based asphalt and petroleum-based asphalt.
3. The process for producing the anode material coke according to claim 1, wherein the quinoline insoluble content of the coking raw material is 0-0.5%, and the ash content is 0-0.5%.
4. The process for producing anode material coke according to claim 1, wherein in the step 3), the delayed coking process parameters are: the coking temperature in the coking tower is 450-550 ℃, the coking pressure is 0-1.0 MPa, and the circulation ratio is 0.2-2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811039657.3A CN109082301B (en) | 2018-09-06 | 2018-09-06 | Production process and production device of anode material coke |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811039657.3A CN109082301B (en) | 2018-09-06 | 2018-09-06 | Production process and production device of anode material coke |
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| CN109082301A CN109082301A (en) | 2018-12-25 |
| CN109082301B true CN109082301B (en) | 2023-12-26 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1624956A (en) * | 2004-12-02 | 2005-06-08 | 辽宁弘光科技集团有限公司 | Production method of carbon nagtive electrode material of lithium ion cell |
| CN106635102A (en) * | 2016-12-09 | 2017-05-10 | 山东益大新材料有限公司 | Process for producing negative electrode material coke by taking supercritical extraction oil slurry as raw material and application of process |
| CN208857216U (en) * | 2018-09-06 | 2019-05-14 | 中钢集团鞍山热能研究院有限公司 | A kind of process units of negative electrode material coke |
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- 2018-09-06 CN CN201811039657.3A patent/CN109082301B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1624956A (en) * | 2004-12-02 | 2005-06-08 | 辽宁弘光科技集团有限公司 | Production method of carbon nagtive electrode material of lithium ion cell |
| CN106635102A (en) * | 2016-12-09 | 2017-05-10 | 山东益大新材料有限公司 | Process for producing negative electrode material coke by taking supercritical extraction oil slurry as raw material and application of process |
| CN208857216U (en) * | 2018-09-06 | 2019-05-14 | 中钢集团鞍山热能研究院有限公司 | A kind of process units of negative electrode material coke |
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