CN107946593A - A kind of method that coal tar pitch prepares lithium cell negative pole material needle coke - Google Patents
A kind of method that coal tar pitch prepares lithium cell negative pole material needle coke Download PDFInfo
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- CN107946593A CN107946593A CN201711246219.XA CN201711246219A CN107946593A CN 107946593 A CN107946593 A CN 107946593A CN 201711246219 A CN201711246219 A CN 201711246219A CN 107946593 A CN107946593 A CN 107946593A
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- needle coke
- coal tar
- tower
- phase component
- coke
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- 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
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- 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)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Coke Industry (AREA)
Abstract
The invention discloses a kind of method that coal tar pitch prepares lithium cell negative pole material needle coke, include the following steps：By petroleum solvent, coal measures solvent proportionally 1:1 progress mixing preparation is uniform；Using coal tar pitch as raw material, deployed mixed solvent is extractant, together squeezes into subsider and carries out extraction sedimentation, and the light phase component on upper strata and the heavy phase component of lower floor are obtained after separation；Light phase component prepares refined bitumen, while recycling design after being distilled；Heavy phase component is evaporated under reduced pressure, recycling design, and obtains byproduct carbolineum and caking property pitch；Obtained refined bitumen is heated to 470 500 DEG C by heating furnace and squeezes into coke drum progress coking, while is passed through softened water, the miscella of coking tower cracks in tower, generates needle coke and coking gas, coking gas enter the isolated coker light oil of fractionating column.Preparation method of the present invention is simple, its performance of the coal-based needle coke prepared fully meets lithium cell negative pole material requirement.
Description
Technical field
The present invention relates to lithium cell negative pole material technical field, more particularly to prepare lithium cell negative pole material needle-shaped for a kind of coal tar pitch
Burnt method.
Background technology
Needle coke is a kind of silver gray of invention the 1970s, has the carbon material of metallic luster, since it has
Relatively low thermal coefficient of expansion and resistance, mainly for the production of steel-making high power graphite electrode, ultra high power graphite electrode.In addition
Needle coke also has the characteristics that good electric conductivity and easily graphited, can also be applied to production lithium as a kind of soft charcoal material
Cell negative pole material.Needle coke is divided into petroleum needle coke and coal-based needle coke according to the difference of raw materials for production.Using petroleum residual oil as
The needle coke of raw material production is oil system needle coke, and the needle coke produced using coal tar asphalt and cut is coal-based needle coke.Mesh
The technology of the high-quality needle coke of preceding production mainly rests in the U.S., Japan and Britain, domestic needle coke development there has also been it is certain into
Exhibition, the needle coke of home and abroad enterprise all cannot completely meet the requirement of lithium cell negative pole material.
STUDY OF NEEDLE COKE TECHNOLOGY is generally pretreatment of raw material, delayed coking and calcining, and the purpose of pretreatment of raw material is to remove raw material
Impurity (mainly primary quinoline beautiful jade insoluble matter PQI) in maltha produces refined bitumen.Expect that the result of pretreatment directly determines
The success or failure of needle coke coking, are a processes mostly important in whole technique.Preprocessing method of raw materials has the way of distillation, centrifugation
Method, solvent method and flash method, the way of distillation cut out the impurity in pitch with vacuum separator by vacuum separation, technique it is simple but
Be material asphalt yield it is relatively low.The mechanical equipment such as centrifugal process centrifuge or filter is divided coal tar asphalt by centrifugation
From the centrifugate of the residue rich in QI and removing QI, the yield of material asphalt is substantially increased, but the needle coke quality prepared
Do not reach far it is excellent, and invest it is huge.Aliphatic hydrocarbon and aromatic hydrocarbon solvent are configured to mix according to a certain percentage molten by solvent method
Agent, is then together extracted into separator with coal tar asphalt, prepares needle-shape coke raw material pitch.Delayed coking is exactly needle-shaped
The process of burnt coking, is the generation, growth and conversion process of Carbonaceous mesophase, the needle coke before this process is formed and forged.Calcine rank
Section is will to forge preceding Jiao and be delivered in rotary kiln to be calcined, and ultimately forms ripe Jiao.The needle coke that above technology is formed can expire
The demand of foot production graphite electrode, but can't fully meet used in lithium cell negative pole material.
The content of the invention
It is above-mentioned to solve it is an object of the invention to provide a kind of method that coal tar pitch prepares lithium cell negative pole material needle coke
Technical problem.
The present invention uses following technical scheme to achieve the above object：A kind of coal tar pitch prepares lithium cell negative pole material needle coke
Method, include the following steps：
1）By petroleum solvent, coal measures solvent proportionally 1:1 progress mixing preparation is uniform；
2）Using coal tar pitch as raw material, with step 1）Deployed mixed solvent is extractant, together squeezes into subsider and is extracted
Sedimentation, obtains the light phase component on upper strata and the heavy phase component of lower floor after separation；
3）Light phase component prepares refined bitumen, while recycling design after being distilled；
4）Heavy phase component is evaporated under reduced pressure, recycling design, and obtains byproduct carbolineum and caking property pitch；
5）By step 3）Obtained refined bitumen is heated to 470-500 DEG C by heating furnace and squeezes into coke drum progress coking, at the same time
Softened water is passed through, the miscella of coking tower cracks in tower, generates needle coke and coking gas, coking gas are separated into fractionating column
To coker light oil.
As the further scheme of the present invention, the step 2）Middle coal tar pitch be heated to 80 DEG C squeeze into subsider carry out it is 24 small
When extraction sedimentation, during which keep subsider in 80 DEG C of mixed material temperature.
As the further scheme of the present invention, the light phase component liquid of the step 3) at the middle and upper levels is by heating stove heat 320
DEG C enter light phase tower in carry out distillation recovery solvent after, control 230 DEG C of tower top temperature, remaining material is refined bitumen；
As the further scheme of the present invention, the step 4）The heavy phase component of middle lower floor is by the 320 DEG C of entrance of heating stove heat
Solvent is distilled to recover in heavy phase tower, control pressure 65kpa, 200 DEG C of tower top temperature, obtains by-product carbolineum and caking property pitch.
As the further scheme of the present invention, the step 5）Particular content stirs for refined bitumen by asphalt tank is interior,
It is heated to 120 DEG C to mix with carbolineum, mixed proportion 1:1, then heated by two heating equipments of pre-add hot stove and heating furnace
Enter to 470-500 DEG C in coke drum and carry out pyrogenetic reaction, while inject softened water, the combined amount of softened water and pitch and carbolineum
Ratio is 0.02:1,20 it is small when after, stop bitumen feed and carry out drawing Jiaozhuo industry, carbolineum is heated in injection coke drum, when drawing burnt
Between control 8 it is small when, the control of coke tower pressure interior force be 0.2Mpa, obtains needle coke, then carry out hydraulic decoking, by easy in reaction tower
The oil gas of volatilization is discharged into fractionating column by coke drum top to be separated, and obtains coker light oil and wax oil.
The beneficial effects of the invention are as follows：Preparation method of the present invention is simple, its performance of the coal-based needle coke prepared is completely full
Sufficient lithium cell negative pole material requirement.
Embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this area
Art personnel all other embodiments obtained without making creative work, belong to the model that the present invention protects
Enclose.
Embodiment 1
By washing oil and aviation kerosine according to 1:1 ratio is uniformly mixed, and it is heavy then together to be squeezed into the coal tar pitch for being heated to 80 DEG C
Extraction sedimentation when drop groove progress 24 is small, during which keeps 80 DEG C of mixed material temperature in subsider.Upper lower leaf, upper strata after extraction
Liquid controls 230 DEG C of tower top temperature after carrying out distillation recovery solvent in 320 DEG C of entrance light phase towers of heating stove heat, remaining
Material is refined bitumen；Subnatant enters the interior distillation recovery solvent of heavy phase tower for 320 DEG C by heating stove heat, and control pressure is
65kpa, 200 DEG C of tower top temperature, obtains by-product carbolineum and caking property pitch.
Refined bitumen is stirred by asphalt tank is interior, is heated to 120 DEG C and is mixed with carbolineum, mixed proportion 1:1, then pass through
Two heating equipments of pre-add hot stove and heating furnace are heated to 470-500 DEG C and enter progress pyrogenetic reaction in coke drum, inject at the same time
The combined amount ratio of softened water, softened water and pitch and carbolineum is 0.02:1；20 it is small when after, stop bitumen feed carrying out drawing Jiaozhuo
Industry, carbolineum is heated in injection coke drum, and when drawing burnt time control 8 small, the control of coke tower pressure interior force is 0.2Mpa, is obtained needle-shaped
Jiao, then hydraulic decoking is carried out, it is discharged into fractionating column and is separated by coke drum top by oil gas volatile in reaction tower, is obtained
To coker light oil and wax oil.
Pass through needle coke performance made from the present embodiment：Volatile matter 6.8%.
Embodiment 2
By coal measures solvent and oil series solvent mixing preparation, mixed solvent virtue fat ratio reaches 0.75.Pitch and mixed solvent are pressed
According to 1:1 ratio squeeze into subsider carry out sedimentation 6 it is small when, the quinoline insolubles of upper liquid, which reaches 0.1%, to be emptied, upper liquid
Heated 320 DEG C of stove heat enters light phase destilling tower and carries out recycling design, and residue is maltha.The heated stove of subnatant adds
Heat keeps negative-pressure operation recycling design, obtains caking property pitch to 320 DEG C into heavy phase tower, heavy phase tower.
Maltha is heated to 120 DEG C with heavy oil according to 1:1 ratio is mixed, then with third component additive according still further to
The ratio mixing of 0.1-0.5%, mixed liquor are heated to 480 DEG C of -500 DEG C of feeding coke drums, and 20 start to draw Jiao when small, and control is drawn burnt
500-510 DEG C of temperature, draws burnt pressure 0.3Mpa.30 it is small when after steam blowing 1 it is small when, treat that temperature is down to less than 60 DEG C in coke drum,
Hydraulic decoking is carried out, is discharged into fractionating column and is separated by coke drum top by oil gas volatile in reaction tower, obtain Jiao
Change light oil and wax oil.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of changes, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of method that coal tar pitch prepares lithium cell negative pole material needle coke, it is characterised in that include the following steps：
1）By petroleum solvent, coal measures solvent proportionally 1:1 progress mixing preparation is uniform；
2）Using coal tar pitch as raw material, with step 1）Deployed mixed solvent is extractant, together squeezes into subsider and is extracted
Sedimentation, obtains the light phase component on upper strata and the heavy phase component of lower floor after separation；
3）Light phase component prepares refined bitumen, while recycling design after being distilled；
4）Heavy phase component is evaporated under reduced pressure, recycling design, and obtains byproduct carbolineum and caking property pitch；
5）By step 3）Obtained refined bitumen is heated to 470-500 DEG C by heating furnace and squeezes into coke drum progress coking, at the same time
Softened water is passed through, the miscella of coking tower cracks in tower, generates needle coke and coking gas, coking gas are separated into fractionating column
To coker light oil.
2. the method that a kind of coal tar pitch according to claim 1 prepares lithium cell negative pole material needle coke, it is characterised in that institute
State step 2）Middle coal tar pitch be heated to 80 DEG C squeeze into subsider carry out 24 it is small when extraction sedimentation, during which keep subsider in mixing
80 DEG C of temperature of charge.
3. the method that a kind of coal tar pitch according to claim 1 prepares lithium cell negative pole material needle coke, it is characterised in that institute
The light phase component liquid of step 3) at the middle and upper levels is stated after carrying out distillation recovery solvent in 320 DEG C of entrance light phase towers of heating stove heat,
230 DEG C of tower top temperature is controlled, remaining material is refined bitumen.
4. the method that a kind of coal tar pitch according to claim 1 prepares lithium cell negative pole material needle coke, it is characterised in that institute
State step 4）The heavy phase component of middle lower floor enters distillation recovery solvent, control pressure in heavy phase tower for 320 DEG C by heating stove heat
For 65kpa, 200 DEG C of tower top temperature, obtains by-product carbolineum and caking property pitch.
5. the method that a kind of coal tar pitch according to claim 1 prepares lithium cell negative pole material needle coke, it is characterised in that institute
State step 5）Particular content stirs for refined bitumen by asphalt tank is interior, is heated to 120 DEG C and is mixed with carbolineum, mixed proportion 1:
1, it is anti-then progress coking in 470-500 DEG C of entrance coke drum to be heated to by two heating equipments of pre-add hot stove and heating furnace
Should, while softened water is injected, softened water and the combined amount ratio of pitch and carbolineum are 0.02:1,20 it is small when after, stop pitch into
Material carries out drawing Jiaozhuo industry, and carbolineum is heated in injection coke drum, and when drawing burnt time control 8 small, the control of coke tower pressure interior force is
0.2Mpa, obtains needle coke, then carries out hydraulic decoking, and fractionation is discharged into by coke drum top by oil gas volatile in reaction tower
Separated in tower, obtain coker light oil and wax oil.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711246219.XA CN107946593A (en) | 2017-12-01 | 2017-12-01 | A kind of method that coal tar pitch prepares lithium cell negative pole material needle coke |
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| CN201711246219.XA CN107946593A (en) | 2017-12-01 | 2017-12-01 | A kind of method that coal tar pitch prepares lithium cell negative pole material needle coke |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109319758A (en) * | 2018-10-10 | 2019-02-12 | 中钢集团鞍山热能研究院有限公司 | A kind of mesocarbon microspheres, the joint production process method of negative electrode material coke |
| CN109401783A (en) * | 2018-12-14 | 2019-03-01 | 中冶焦耐(大连)工程技术有限公司 | A kind of comprehensive utilization process device with coal tar production needle-shape coke raw material |
| CN110265645A (en) * | 2019-06-25 | 2019-09-20 | 郑州中科新兴产业技术研究院 | A kind of pitch base carbon nanometer sheet composite negative pole material, preparation method and applications |
| CN111453721A (en) * | 2020-04-30 | 2020-07-28 | 中钢集团鞍山热能研究院有限公司 | Preparation method and device of wide-area sheet-shaped structure cathode material special for lithium ion battery |
| CN114695846A (en) * | 2020-12-30 | 2022-07-01 | 宝武碳业科技股份有限公司 | Preparation method of needle coke and silicon-containing negative electrode material thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109319758A (en) * | 2018-10-10 | 2019-02-12 | 中钢集团鞍山热能研究院有限公司 | A kind of mesocarbon microspheres, the joint production process method of negative electrode material coke |
| CN109401783A (en) * | 2018-12-14 | 2019-03-01 | 中冶焦耐(大连)工程技术有限公司 | A kind of comprehensive utilization process device with coal tar production needle-shape coke raw material |
| CN109401783B (en) * | 2018-12-14 | 2024-01-30 | 中冶焦耐(大连)工程技术有限公司 | Comprehensive utilization process device for producing needle coke raw materials from coal tar |
| CN110265645A (en) * | 2019-06-25 | 2019-09-20 | 郑州中科新兴产业技术研究院 | A kind of pitch base carbon nanometer sheet composite negative pole material, preparation method and applications |
| CN110265645B (en) * | 2019-06-25 | 2021-03-23 | 郑州中科新兴产业技术研究院 | Asphalt-based carbon nanosheet composite negative electrode material, and preparation method and application thereof |
| CN111453721A (en) * | 2020-04-30 | 2020-07-28 | 中钢集团鞍山热能研究院有限公司 | Preparation method and device of wide-area sheet-shaped structure cathode material special for lithium ion battery |
| CN114695846A (en) * | 2020-12-30 | 2022-07-01 | 宝武碳业科技股份有限公司 | Preparation method of needle coke and silicon-containing negative electrode material thereof |
| CN114695846B (en) * | 2020-12-30 | 2023-11-17 | 宝武碳业科技股份有限公司 | Preparation method of needle coke and silicon-containing anode material thereof |
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Application publication date: 20180420 |