CN113716544B - Preparation method of low-cost high-magnification anode material coke - Google Patents
Preparation method of low-cost high-magnification anode material coke Download PDFInfo
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- CN113716544B CN113716544B CN202110959559.7A CN202110959559A CN113716544B CN 113716544 B CN113716544 B CN 113716544B CN 202110959559 A CN202110959559 A CN 202110959559A CN 113716544 B CN113716544 B CN 113716544B
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- 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
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
Abstract
The invention relates to a preparation method of low-cost high-magnification anode material coke, which takes coal-based soft asphalt as a raw material, and the raw material is put into a temperature cutting tower from a soft asphalt storage tank to be cut to remove heavy components, thus obtaining clean asphalt; asphalt-based carbon particles are taken as raw materials, and are pumped into a sedimentation deacidification tank from a carbon particle storage tank and dehydrated by a particle dryer; mixing and stirring clean asphalt and carbon particles; entering an intermediate phase regulation thermal reaction tower, and finally cutting the coke with water vapor to obtain anode material coke; after the coke is dried, a part of the coke is separated into two types of negative electrode raw coke; the other part is divided into two types of cathode coke through carbonization treatment; the light component steam in the temperature cutting tower and the intermediate phase regulating and controlling thermal reaction tower respectively enter respective condensers for liquidation treatment, and finally enter respective storage tanks. According to the invention, the modification step of the anode material is omitted, carbon particles are added into the soft asphalt, the multiplying power performance of the anode material is improved, and the method has the advantages of low cost and high multiplying power.
Description
Technical Field
The invention belongs to the field of lithium ion battery anode materials, and particularly relates to a preparation method of low-cost high-magnification anode material coke.
Background
Lithium ion batteries have been attracting attention in recent years due to their small size, high energy density, low cost, no pollution, and the like. Due to the recent technological leaps of digital products, there are raised requirements and expectations for the performance of batteries. The improvement of the battery performance depends on the development and perfection of electrode materials, so that the selection of the anode material with low irreversible capacity and good rate capability for the first time is important.
The current lithium ion battery cathode material is mainly made of artificial graphite material, the positive electrode material is mainly made of transition metal oxide, and the common characteristic of the material is that the cost is too high, so that the research and development of the low-cost cathode material under the condition of not affecting the performance of the lithium ion battery are improved.
The cost is reduced under the condition of not affecting the performance of the lithium ion battery, the mass production and large-scale industrialization of the anode material can be promoted, most means for improving the performance of the lithium ion battery anode material at the present stage are to carry out the modification of the anode material by pelleting, coating and the like, and the modification process is omitted if the anode material precursor coke with excellent performance is prepared, so that the preparation cost of the lithium ion battery is greatly reduced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of low-cost high-magnification anode material coke, which adopts cheap coal-based soft asphalt and asphalt carbon particles as raw materials to prepare isotropic anode material coke, omits an additional modification step of anode material, and reduces cost and improves magnification performance of the anode material by adding the carbon particles into the soft asphalt.
In order to achieve the above purpose, the present invention is realized by the following technical scheme:
a preparation method of low-cost high-magnification anode material coke comprises the following steps:
1) Preparing raw materials: taking coal-based maltene as a raw material, and pumping the raw material into a temperature cutting tower from a maltene storage tank to cut raw material components to remove heavy components, thereby obtaining clean asphalt;
asphalt-based carbon particles are taken as raw materials, and are pumped into a sedimentation deacidification tank from a carbon particle storage tank and dehydrated by a particle dryer;
clean pitch and dried carbon particles were mixed according to a ratio of 1:1 to 5:1, and mixing and stirring in a raw material stirring tank;
2) Intermediate phase regulating thermal reaction process: pumping clean asphalt into an asphalt preheater for preheating, mixing and stirring with carbon particles, keeping the preheating temperature, entering an intermediate phase regulation and control thermal reaction tower, and finally cutting coke with water vapor to obtain anode material coke;
3) And (3) product and subsequent treatment: after the coke is dried, a part of the coke is separated into two specifications of negative electrode raw coke through a granularity sieving device, and finally packaged and sold; the other part is carbonized, and then is divided into two specifications of cathode coke through a granularity sieving device, and finally packaged and sold;
and the light component steam in the temperature cutting tower and the intermediate phase regulating and controlling thermal reaction tower respectively enter respective condensers to be subjected to liquidation treatment, and finally enter respective storage tanks to be packed and sold.
The cutting temperature in the step 1) is 300-400 ℃, and the alpha resin in the clean asphalt is less than or equal to 0.05 percent and the beta resin is more than or equal to 6 percent.
In the step 1), one or a mixture of two of KOH and NaOH solutions is adopted in the sedimentation deacidification tank.
The temperature of the asphalt preheater in the step 2) is 300-400 ℃.
The intermediate phase in the step 2) regulates the pressure of the thermal reaction tower to be 0-5 Mpa, the heating rate to be 3-5 ℃/min and the final temperature of the thermal reaction to be 500-600 ℃.
In the carbonization treatment process of the step 3), the carbonization temperature is 800-1500 ℃, and the shielding gas is one of argon, nitrogen and helium.
One of the two specifications of coke described in step 3) has a particle size of 5 to 10mm.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses cheap coal-based soft asphalt and asphalt carbon particles to prepare the isotropic anode material coke, can omit the extra modification step of the anode material, and can lead the microscopic structure after coke molding to be a mosaic structure by adding the carbon particles into the soft asphalt. The invention prepares the low-cost high-magnification anode material coke by a pilot-scale delayed coking device, and adjusts the production value and the product performance by adjusting parameters such as temperature, pressure and the like.
Drawings
FIG. 1 is a pilot plant delayed coking unit and process flow diagram of the present invention.
Fig. 2 is a schematic diagram of a coke of "mosaic" structure.
Fig. 3 is a schematic diagram II of a coke of "mosaic" structure.
Fig. 4 is a schematic diagram III of a coke of "mosaic" structure.
Fig. 5 is a schematic diagram four of a coke of "mosaic" structure.
Fig. 6 is a schematic diagram five of a coke of "mosaic" structure.
In the figure: 1 carbon particle storage tank, 2 soft asphalt storage tank, 3 sedimentation deacidification pond, 4 steam condenser, 5 granule desicators, 6 temperature cutting tower, 7 pitch preheater, 8 raw materials agitator tank, 9 intermediate phase regulation and control thermal reaction tower, 10 product dryer, 11 temperature cutting upper oil storage tank, 12 coking light component oil storage tank, 13 temperature cutting light component steam condenser, 14 coking light component condenser, 15 granularity screening device, 16 calcining device, 17 dust removal air blower, 18 cistern, 19 granularity screening device.
Detailed Description
The present invention will be described in detail below with reference to the drawings of the specification, but it should be noted that the practice of the present invention is not limited to the following embodiments.
Referring to fig. 1, the device atmosphere is carried out under a certain pressure value and is slowly heated to a certain temperature. Maintaining the temperature at the highest temperature for a certain time to obtain a cathode Jiao Shengjiao, and screening a part of raw coke into two specifications of cathode raw coke products; and the other part of the negative electrode coke is calcined by a calciner, and the negative electrode coke is screened into negative electrode coke products of other two specifications by a particle size screening device. The method specifically comprises the following steps:
1) The carbon particle storage tank is opened and is sent to a sedimentation deacidification tank through a closed conveyor belt, acidic substances influencing the coking process are removed after sedimentation for 5-10 hours in the sedimentation deacidification tank, the carbon particle storage tank is pumped into a particle dryer through an extraction pump, after drying for 1-3 hours in the particle dryer, water vapor flows back to the deacidification tank through a vapor condenser, and the dried carbon particles are pumped into a raw material stirring tank and clean asphalt by a pump for stirring.
Clean asphalt: cutting coal-based soft asphalt at the boiling point temperature in a raw material component cutting tower to remove components which prevent the asphalt from forming coke;
2) Pumping the coal-series soft asphalt preheated to a fluid state from a soft asphalt storage tank into a temperature cutting tower by a pump, wherein the temperature in the tower is 300-400 ℃, the pressure is 0-0.2 MPa, light component steam before 300-400 ℃ enters the upper oil storage tank for temperature cutting through a steam condenser, packaging and selling are carried out, and clean asphalt after 300-400 ℃ is pumped into a raw material stirring tank for stirring with carbon particles.
3) The mixed raw materials enter an asphalt preheater, the preheating temperature is 400-500 ℃, the raw materials are preheated and then are pumped into an intermediate phase regulation and control thermal reaction tower, intermediate phase thermal reaction is carried out under the environment of 0-5 MPa (0 MPa means normal pressure) through a temperature rising program of 400-550 ℃, light component steam in the thermal reaction process enters a coking light component condenser, and enters a coking light component oil storage tank after condensation, and the packaging and selling are carried out similarly.
After the intermediate phase is completely subjected to the thermal reaction, the coke is cut by utilizing water vapor, the removed impurities are toluene, quinoline insoluble matters or other element compounds, the purpose of removing the coke is realized, the coke is sent into a product dryer through a conveyor belt, and a part of the coke after drying enters a particle size screening device for particle size screening, and finally, the coke is produced by the two low-cost high-magnification anode materials with different specifications.
The other part of the calcined coke enters a high-temperature calciner to be calcined at a high temperature of 800-1500 ℃ under the condition of one of protective gas of nitrogen, argon and helium, then enters a dust removal blower to be subjected to dust removal treatment, and is subjected to particle size separation by a particle size separator after dust removal, so that calcined coke of the two low-cost high-magnification anode materials with different specifications is obtained.
Example 1
Mixing coal-based soft asphalt with carbon particles according to a proportion of 3:1, entering an asphalt preheater at 400 ℃ after mixing, entering an intermediate phase regulation and control thermal reaction tower under the condition that the coking tower parameter is 2MPa and the temperature is 420 ℃, rising to 530 ℃ at the heating rate of 5 ℃/h, entering the obtained raw coke part into a calciner, finally obtaining calcined anode material coke, adjusting the particle size separator parameter to 10mm, separating the calcined anode material coke, and carrying out electrochemical performance test by graphitizing the calcined anode material coke at 2800 ℃;
example 2
Mixing coal-based soft asphalt with carbon particles according to a proportion of 4:1, entering an asphalt preheater at 400 ℃ after mixing, entering an intermediate phase regulation and control thermal reaction tower under the condition that the coking tower parameter is 2MPa and the temperature is 420 ℃, rising to 540 ℃ at the heating rate of 4 ℃/h, entering the obtained raw coke part into a calciner, finally obtaining calcined anode material coke, adjusting the particle size separator parameter to 10mm, separating the calcined anode material coke, and carrying out electrochemical performance test by graphitizing the calcined anode material coke at 2800 ℃;
example 3
Mixing coal-based soft asphalt with carbon particles according to a proportion of 5:1, entering an asphalt preheater at 400 ℃ after mixing, entering an intermediate phase regulation and control thermal reaction tower under the conditions that the coking tower parameter is 2MPa and the temperature is 420 ℃, rising to 550 ℃ at the heating rate of 10 ℃/h, entering the obtained raw coke part into a calciner, finally obtaining calcined anode material coke, adjusting the particle size separator parameter to 10mm, separating the calcined anode material coke, and carrying out electrochemical performance test by graphitizing the calcined anode material coke at 2800 ℃;
example 4
Mixing coal-based soft asphalt with carbon particles according to a ratio of 2:1, entering an asphalt preheater at 400 ℃ after mixing, entering an intermediate phase regulation and control thermal reaction tower under the condition that the coking tower parameter is 3MPa and the temperature is 420 ℃, rising to 520 ℃ at the heating rate of 5 ℃/h, entering the obtained raw coke part into a calciner, finally obtaining calcined anode material coke, adjusting the particle size separator parameter to 10mm, separating the calcined anode material coke, and carrying out electrochemical performance test by graphitizing the calcined anode material coke at 2800 ℃;
example 5
Mixing coal-based soft asphalt with carbon particles according to a proportion of 3:2, mixing the raw coke and the calcined anode material coke in proportion, then, feeding the mixture into a pitch preheater at 400 ℃, feeding the mixture into an intermediate phase regulation and control thermal reaction tower at the temperature of 420 ℃ under the normal pressure state of the coking tower parameters, heating the mixture to 530 ℃ at the heating rate of 8 ℃/h, feeding the obtained raw coke into a calciner, wherein the temperature of the calciner is 1200 ℃, finally obtaining the calcined anode material coke, adjusting the granularity separator parameters to 10mm, separating the calcined anode material coke, and carrying out electrochemical performance test by graphitizing the calcined anode material coke at the temperature of 2800 ℃;
the final results are shown in Table 1:
table 1 electrochemical properties table of the anode material obtained in example after being coked into half cell
According to the invention, impurity removal and cutting are carried out on coal-series soft asphalt, sedimentation and acid removal are carried out on carbon particles, two raw materials are mixed for intermediate-phase regulation and control thermal reaction, and then low-cost high-magnification anode material coke is finally obtained through calcination, crushing and graphitization. The raw materials used in the invention are cheap coal-based soft asphalt and asphalt-based carbon particles, and carbon particles are added into the soft asphalt to form coke with a mosaic structure, as shown in figures 2-6, the coke with the mosaic structure has isotropy, a secondary granulating process in the preparation process of the anode material can be omitted, the multiplying power performance of the anode material is improved, and the method has wide application prospects in the field of anode materials of lithium ion batteries.
Claims (5)
1. The preparation method of the low-cost high-magnification anode material coke is characterized by comprising the following steps of:
1) Preparing raw materials: asphalt-based carbon particles are taken as raw materials, and are pumped into a sedimentation deacidification tank from a carbon particle storage tank and dehydrated by a particle dryer;
cutting coal-based soft asphalt at the boiling point temperature in a raw material component cutting tower to remove components which prevent the asphalt from forming coke;
pumping the coal-based soft asphalt preheated to a fluid state into a temperature cutting tower from a soft asphalt storage tank by a pump, enabling light component steam at the temperature of 300-400 ℃ and the pressure of 0-0.2 MPa in the tower and before 300-400 ℃ to enter a temperature cutting upper oil storage tank through a steam condenser, and packaging and selling; clean asphalt at 300-400 ℃ and dried carbon particles are mixed according to the proportion of 1:1 to 5:1, and mixing and stirring in a raw material stirring tank;
2) The mixed raw materials enter an asphalt preheater, the preheating temperature is 400-500 ℃, the raw materials are preheated and then are fed into an intermediate phase regulation and control thermal reaction tower, the heating rate is 3-5 ℃/min under the environment of 0-5 MPa, and the final temperature of the thermal reaction is 500-600 ℃; the light component steam in the thermal reaction process enters a coking light component condenser, enters a coking light component oil storage tank after being condensed, and is packaged and sold as well;
3) And (3) product and subsequent treatment: after the coke is dried, a part of the coke is separated into two specifications of negative electrode raw coke through a granularity sieving device, and finally packaged and sold; and the other part is carbonized, and then is separated into two specifications of cathode coke through a granularity screening device, and finally packaged and sold.
2. The method for preparing the low-cost high-magnification anode material coke, which is disclosed in claim 1, wherein the alpha resin in the clean asphalt in the step 1) is less than or equal to 0.05%, and the beta resin is more than or equal to 6%.
3. The method for preparing the low-cost high-magnification anode material coke, according to claim 1, wherein the sedimentation deacidification tank in the step 1) is one or a mixture of two of KOH and NaOH solutions.
4. The method for preparing the low-cost high-magnification anode material coke according to claim 1, wherein in the carbonization treatment process of the step 3), the carbonization temperature is 800-1500 ℃, and the shielding gas is one of argon, nitrogen and helium.
5. The method for preparing the low-cost high-magnification anode material coke according to claim 1, wherein the granularity of one of the two specifications of the coke in the step 3) is 5-10 mm.
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