CN212174460U - Device for preparing wide-area sheet-shaped structure cathode material special for lithium ion battery - Google Patents
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Abstract
The device for preparing the wide-area sheet-structure cathode material special for the lithium ion battery comprises a solvent tank, a raw material asphalt tank, a mixer, a purification tank, a distillation tower, a low-temperature carbonization furnace, a reaction kettle, a byproduct oil tank, a heating furnace, a coking tower, a crusher, a screening machine and a graphitization furnace, wherein the solvent tank and the raw material asphalt tank are connected with an inlet of the purification tank through the mixer, an outlet of the purification tank is connected with the distillation tower, a light phase outlet of the distillation tower is connected with the solvent tank, a heavy phase outlet of the distillation tower is connected with the low-temperature carbonization furnace, a heavy phase outlet of the low-temperature carbonization furnace is connected with the reaction kettle, a heavy phase outlet of the reaction kettle is connected with the coking tower, the reaction kettle is connected with the heating furnace, a heavy phase outlet of the coking tower. The invention effectively reduces the problems of inconsistent orientation degree, expansion of the cathode material and the like after the cathode material is assembled into the lithium ion battery, and omits the processes of granulation coating and the like in the production process of the cathode material. Low cost of raw materials and simple process.
Description
Technical Field
The utility model belongs to the technical field of the special negative electrode material production of lithium ion battery, especially, relate to a device of special wide area sheet structure negative electrode material of preparation lithium ion battery.
Background
Lithium ion batteries are favored by various industries due to their high energy density, high specific energy, long cycle life, small self-discharge, good safety performance, no memory effect, and environmental friendliness, and are gradually moving from applications such as 3C electronic products, electric tools, medical electronics, energy storage devices, and the like to the transportation fields such as pure electric vehicles, hybrid electric vehicles, rail transit, aerospace, and the like. At present, China has become the biggest manufacturing base of lithium ion batteries in the world and the second largest producing country and export country of lithium ion batteries, and the market of the lithium ion batteries is entering the golden period.
In lithium ion batteries, the negative electrode material is one of the important factors affecting the battery capacity and service life. Lithium electricity cathode material is as one kind of lithium electricity consumptive material, along with the continuous promotion of lithium ion battery output, the cathode material demand is also in high-speed the growth. The ideal negative electrode material has higher specific capacity, charge-discharge efficiency, cycle performance and safety performance and lower cost. At present, needle coke, petroleum coke, metallurgical coke and the like are subjected to shaping, granulation, coating and other treatments, so that the defects of natural graphite are improved to a certain extent, and particularly, the needle coke is accepted by the industry due to the excellent characteristics of easy graphitization, high conductivity, low ash content and the like, and has relatively high market share. However, needle coke is a streamline fiber structure, and carbon materials such as needle coke, petroleum coke, metallurgical coke and the like are mainly suitable for the fields of graphite electrodes, carburant, steel smelting and the like, are not specially developed and produced for negative electrode materials, have certain defects in the application aspect of lithium ion batteries, and the streamline fiber structures of the needle coke, the petroleum coke, the metallurgical coke and the like are easy to expand due to different orientation degrees in all directions after being assembled into the lithium ion batteries, so that the initial coulombic efficiency is low and the rate capability is poor. Many products with high performance requirements can meet the requirements only by taking needle coke as a raw material through processes such as secondary granulation coating and the like, which cannot meet the higher requirements of future lithium ion battery development on negative electrode materials. Therefore, the development of the negative electrode material which is specially used for the lithium ion battery and has high first charge-discharge efficiency, high specific capacity, good rate capability and good cycle performance is of great significance.
SUMMERY OF THE UTILITY MODEL
The utility model provides a device of special wide area sheet structure negative pole material of preparation lithium ion battery has realized effectively reducing orientation degree inconsistent, negative pole material inflation scheduling problem after the negative pole material assembles into lithium ion battery, saves technologies such as granulation cladding in the negative pole material production process. Low raw material cost, simple process, good product quality and high enterprise profit.
In order to achieve the above object, the utility model adopts the following technical scheme:
device for preparing special wide area sheet structure cathode material of lithium ion battery, including solvent jar, raw materials pitch jar, blender, purification jar, distillation column, low temperature retort, reation kettle, by-product oil jar, heating furnace, coking tower, breaker, screening machine, graphitizing furnace, solvent jar and raw materials pitch jar pass through the entry that the blender connects the purification jar, the exit linkage distillation column of purification jar, the light phase exit linkage solvent jar of distillation column, the heavy phase exit linkage low temperature retort of distillation column, the light phase exit linkage by-product oil jar of low temperature retort, the heavy phase exit linkage reation kettle of low temperature retort, the light phase exit linkage by-product oil jar of reation kettle, the heavy phase exit linkage coking tower of reation kettle, reation kettle connects the heating furnace, the light phase exit linkage by-product oil jar of coking tower, the heavy phase export of coking tower pay-off to the breaker, the crusher feeds materials to the screening machine, and the screening machine feeds materials to the graphitization furnace.
Compared with the prior art, the beneficial effects of the utility model are that:
1) the utility model discloses the technology that is suitable for is with coal pitch as the raw materials, and coal pitch obtains easily, and the low price, the pitch raw materials that obtains after purification and low temperature carbomorphism, the ash content is low, can form wide area large sheet structure negative pole material precursor coke, and gained negative pole material product has excellent electrochemical performance, added value height to raw materials cost is low, simple process, product quality are good, the enterprise profit is high.
2) Through the utility model discloses an anode material of device development is wide area sheet structure, no matter from the microscale to macrostructure all be homogeneous, can effectively reduce orientation degree inconsistent, the anode material inflation scheduling problem after anode material assembles into lithium ion battery, the utility model discloses processes such as granulation cladding in the anode material production process can be saved to the unique structure of well anode material.
3) The utility model discloses the negative electrode material for lithium ion battery development of production is the special negative electrode material of lithium ion battery that first charge-discharge efficiency is high, specific capacity is high, the multiplying power performance is good, the cycle performance is good.
Drawings
FIG. 1 is a process route diagram of the present invention;
fig. 2 is a photograph of a polarizing microscope of a wide-area mesophase structure produced by the present invention;
fig. 3 is a scanning electron microscope picture of the cathode material produced by the present invention.
In the figure: 1-solvent tank, 2-raw material asphalt tank, 3-mixer, 4-purification tank, 5-distillation tower, 6-low temperature carbonization furnace, 7-reaction kettle, 8-byproduct oil tank, 9-heating furnace, 10-coking tower, 11-crusher, 12-sieving machine, 13-graphitization furnace, 14-finished product bin and 15-packing scale.
Detailed Description
The following embodiments are further described in detail:
as shown in fig. 1, a preparation method of a wide-area sheet-shaped negative electrode material special for a lithium ion battery is provided, which uses coal pitch as a raw material, and comprises the steps of purifying and carbonizing the coal pitch at a low temperature, forming a mesophase, coking, drying, crushing, screening, graphitizing, and demagnetizing the obtained coke to obtain the wide-area sheet-shaped negative electrode material.
The method comprises the following steps:
1) and (3) purifying coal tar pitch: mixing the coal tar pitch and the organic solvent in a mixer 3, conveying the mixed material to a purification tank 4, controlling the temperature and time of the purification tank 4, carrying out a complex reaction between the organic solvent and metal or mechanical impurities in the coal tar pitch to extract heavy components in the coal tar pitch and deposit the heavy components at the bottom of the purification tank 4, pumping the purified asphalt at the upper layer into a distillation tower 5 by using a pump, and distilling the residual solvent in the distillation tower 5 to obtain a purified asphalt product.
The reaction temperature of the purification tank 4 is 80-150 ℃ and the reaction time is 2-8 h.
The organic solvent is one or more of quinoline, pyridine, toluene and tetrahydrofuran.
Metal or mechanical impurities in the asphalt can be removed through coal asphalt purification, the internal resistance of the lithium ion battery can be increased due to the existence of the impurities, and the performance of the lithium ion battery as a terminal product is seriously influenced, so that the quantity of the impurities is strictly controlled from the raw material, the ash content is reduced, the coke structure of a precursor of the negative electrode material is irregular due to the existence of the impurities, a wide-area structure cannot be formed, and the raw material asphalt is purified to ensure that the negative electrode material with excellent performance is produced.
2) Low-temperature carbonization treatment: and (3) carrying out low-temperature carbonization on the purified asphalt product in a low-temperature carbonization furnace 6, and controlling the low-temperature carbonization temperature and time to obtain the low-temperature carbonized asphalt raw material.
The low-temperature carbonization temperature is 100-250 ℃, and the low-temperature carbonization time is 5-10 h; controlling the softening point of the pitch after low-temperature carbonization to be 60-90 ℃, controlling the hydrogen content to be more than 5 wt% and controlling the carbon content to be less than 90 wt%.
Part of light tar in the raw material asphalt can be removed through low-temperature carbonization, and the tar has low coking rate and is not suitable to be used as a raw material of precursor coke of a wide-area sheet-shaped negative electrode material. And simultaneously controlling the purification and low-temperature carbonization processes to obtain the raw material asphalt with hydrogen content of more than 5 wt% and carbon content of less than 90 wt%, wherein hetero atoms in the raw material asphalt can promote component condensation during low-temperature carbonization, and the raw material asphalt is prepared for forming wide-area sheet-shaped negative electrode material precursor coke. If the low-temperature carbonization process is not carried out, the high-temperature carbonization is directly carried out, the obtained coke structure tends to a streamline structure, and finally the anode material precursor coke with a wide area sheet structure cannot be obtained. Therefore, the pitch with hydrogen content of more than 5 wt% and carbon content of less than 90 wt% obtained after low-temperature carbonization is a necessary condition for preparing wide-area sheet-shaped negative electrode material precursor coke, and the low-temperature carbonization plays a key role in controlling the composition structure of the raw materials.
3) Intermediate phase formation: conveying a low-temperature carbonized asphalt raw material into a reaction kettle 7, circularly heating materials in the reaction kettle 7 through a heating furnace 9, completing the intermediate phase formation process of coal asphalt in the reaction kettle 7 by the heated materials, taking high-purity nitrogen or argon as shielding gas, heating the materials to coking temperature, and conveying the intermediate phase product reaching the coking temperature into a coking tower for coking; coking the wide area intermediate phase structure product in a delayed coking tower, removing coke and drying after coking production to obtain a wide area sheet structure coke product, and taking the coking oil product generated in the coking process as a byproduct oil product for extraction and sale.
The temperature raising procedure is adjusted to be a temperature changing procedure so as to be suitable for the formation of the intermediate phase and enable the intermediate phase to be a wide-area intermediate phase structure. Adjusting a heating furnace temperature change control system to ensure that the temperature of the material in the reaction kettle 7 is increased from 150-200 ℃ to 380-450 ℃ at the temperature increase speed of 10-20 ℃/h, then preserving the temperature to form an intermediate phase, and the reaction time is 3-20 h; and adjusting the temperature schedule of the heating furnace 9, heating the materials in the reaction kettle 7 to 480-540 ℃ at the heating speed of 3-8 ℃/h, and feeding the materials into a coking tower for coking at the temperature, wherein the coking temperature in the coking tower is 480-530 ℃, the coking pressure is 0-1.0 MPa, and the coking time is 16-40 h.
4) And crushing a coke product with a wide area sheet structure obtained after coking by using a mechanical mill, screening to obtain carbon powder with D50 of 10-20 mu m, graphitizing in a graphitization furnace at 2500-2800 ℃, and demagnetizing to obtain the special negative electrode material for the lithium ion battery with the wide area sheet structure. The ash content in the negative electrode material is 0-0.3 wt%, and the graphitization degree is more than or equal to 96%.
Device for preparing special wide area sheet structure cathode material of lithium ion battery, including solvent jar 1, raw materials pitch jar 2, blender 3, purification jar 4, distillation column 5, low temperature retort 6, reation kettle 7, by-product oil jar 8, heating furnace 9, coking tower 10, breaker 11, screening machine 12, graphitizing furnace 13, solvent jar 1 and raw materials pitch jar 2 pass through the entry that the blender 3 connects purification jar 4, the exit linkage distillation column 5 of purification jar 4, the light phase exit linkage solvent jar 1 of distillation column 5, the heavy phase exit linkage low temperature retort 6 of distillation column 5, the light phase exit linkage by-product oil jar 8 of low temperature retort 6, the heavy phase exit linkage reation kettle 7 of low temperature retort 6, the light phase exit linkage by-product oil jar 8 of reation kettle 7, the heavy phase exit linkage coking tower 10 of reation kettle 7, reation kettle 7 connects heating furnace 9, the light phase outlet of the coking tower 10 is connected with a byproduct oil tank 8, the heavy phase outlet of the coking tower 10 feeds materials to a crusher 11, the crusher 11 feeds materials to a sieving machine 12, and the sieving machine 12 feeds materials to a graphitization furnace 14. The purification tank 4 is a reaction kettle provided with a stirrer inside.
Example 1:
mixing coal tar pitch and a toluene solvent in a mixer, conveying the mixture to a reaction kettle, reacting for 3 hours at the temperature of 80 ℃, standing for 3 hours, extracting a coal tar pitch sample with the upper layer accounting for 80 wt% of the mixture, and distilling the solvent to obtain the purified coal tar pitch. Conveying the purified coal pitch to a low-temperature carbonization furnace by a pump, wherein the temperature of the low-temperature carbonization furnace is 150 ℃, and the heat preservation time is 5 hours, so that the pitch after low-temperature carbonization is obtained, and the pitch has the softening point of 65 ℃, the hydrogen content of 5.5 wt% and the carbon content of 88 wt%. Conveying the low-temperature carbonized asphalt raw material into a reaction kettle by a pump, circularly heating the material in the reaction kettle by a heating furnace, taking high-purity nitrogen as protective gas, heating the temperature of the heating furnace from 150 ℃ to 400 ℃ by a temperature-raising system of 10 ℃/h, and keeping the temperature of the material in the reaction kettle for 15h to form the wide-area mesophase structure asphalt. And then, the outlet temperature of the heating furnace is increased to 480 ℃ at the heating speed of 5 ℃/h, the materials in the reaction kettle are input into a coking tower by a pump for coking reaction, the coking temperature is 480 ℃, the coking pressure is 0.3-0.5 MPa, the coking time is 24h, and the coke is discharged and dried. And (3) crushing and screening coke, controlling the D50 to be 10-20 mu m, and carrying out graphitization high-temperature treatment for 24h at 2800 ℃ under the protection of inert gas to obtain the wide-area sheet lithium ion battery cathode material. The button cell is assembled by taking the lithium sheet as the anode and the cathode, and the electrochemical performance of the button cell is tested. The negative electrode material and the property index after assembling the button cell are shown in table 1.
Example 2:
mixing coal tar pitch and a toluene solvent in a mixer, conveying the mixture to a reaction kettle, reacting for 5 hours at the temperature of 80 ℃, standing for 5 hours, extracting a coal tar pitch sample with the upper layer accounting for 80 wt% of the mixture, and distilling the solvent to obtain the purified coal tar pitch. Conveying the purified coal pitch to a low-temperature carbonization furnace by a pump, wherein the temperature of the carbonization furnace is 180 ℃, and the heat preservation time is 7 hours, so that the pitch after low-temperature carbonization is obtained, and the pitch has the softening point of 75 ℃, the hydrogen content of 6 wt% and the carbon content of 85 wt%. Conveying the low-temperature carbonized asphalt raw material into a reaction kettle by a pump, circularly heating the material in the reaction kettle by a heating furnace, taking high-purity argon as protective gas, heating the temperature of the heating furnace from 150 ℃ to 380 ℃ by a temperature-raising system of 15 ℃/h, and conveying the material into the reaction kettle for 18h to form the wide-area mesophase structure asphalt. And then, the temperature of the outlet of the heating furnace is increased to 500 ℃ at the heating speed of 4 ℃/h, the materials in the reaction kettle are input into a coking tower by a pump for coking reaction, the coking temperature is 500 ℃, the coking pressure is 0.5-0.8 MPa, the coking time is 36h, and the coke is discharged and dried. And (3) crushing and screening coke, controlling the D50 to be 10-20 mu m, and carrying out graphitization high-temperature treatment for 24h at 2800 ℃ under the protection of inert gas to obtain the wide-area sheet lithium ion battery cathode material. The button cell is assembled by taking the lithium sheet as the anode and the cathode, and the electrochemical performance of the button cell is tested. The negative electrode material and the property index after assembling the button cell are shown in table 1.
Example 3:
mixing coal tar pitch and quinoline solvent in a mixer, conveying the mixture to a reaction kettle, reacting for 4 hours at the temperature of 150 ℃, standing for 4 hours, extracting an upper layer 80 wt% coal tar pitch sample, and distilling the solvent to obtain the purified coal tar pitch. Conveying the purified coal pitch to a low-temperature carbonization furnace by a pump, wherein the temperature of the carbonization furnace is 180 ℃, and the heat preservation time is 9 hours, so as to obtain the pitch after low-temperature carbonization, and the pitch has a softening point of 82 ℃, a hydrogen content of 6 wt% and a carbon content of 88 wt%. Conveying the low-temperature carbonized asphalt raw material into a reaction kettle by a pump, circularly heating the material in the reaction kettle by a heating furnace, taking high-purity nitrogen as protective gas, heating the temperature of the heating furnace from 150 ℃ to 430 ℃ by a temperature-raising system of 12 ℃/h, and conveying the material into the reaction kettle for 10h to form the wide-area mesophase structure asphalt. And then, the temperature of the outlet of the heating furnace is increased to 520 ℃ at the heating speed of 8 ℃/h, the materials in the reaction kettle are input into a coking tower by a pump for coking reaction, the coking temperature is 520 ℃, the coking pressure is 0.3-0.6 MPa, the coking time is 20h, and the coke is discharged and dried. And (3) crushing and screening coke, controlling the D50 to be 10-20 mu m, and carrying out graphitization high-temperature treatment for 24h at 2800 ℃ under the protection of inert gas to obtain the wide-area sheet lithium ion battery cathode material. The button cell is assembled by taking the lithium sheet as the anode and the cathode, and the electrochemical performance of the button cell is tested. The negative electrode material and the property index after assembling the button cell are shown in table 1.
Example 4:
mixing coal tar pitch and a pyridine solvent in a mixer, conveying the mixture to a reaction kettle, reacting for 6 hours at the temperature of 80 ℃, standing for 5 hours, extracting a coal tar pitch sample with the upper layer accounting for 80 wt% of the mixture, and distilling the solvent to obtain the purified coal tar pitch. Conveying the purified coal pitch to a low-temperature carbonization furnace by a pump, keeping the temperature of the low-temperature carbonization furnace at 200 ℃ for 6 hours to obtain the pitch carbonized at the low temperature, wherein the pitch softening point is 80 ℃, the hydrogen content is 6.5 wt% and the carbon content is 84 wt%. Conveying the low-temperature carbonized asphalt raw material into a reaction kettle by a pump, circularly heating the material in the reaction kettle by a heating furnace, taking high-purity nitrogen as protective gas, heating the temperature of the heating furnace from 200 ℃ to 400 ℃ by a temperature-raising system of 12 ℃/h, and conveying the material into the reaction kettle for 18h to form the wide-area mesophase structure asphalt. And then, the temperature of the outlet of the heating furnace is increased to 540 ℃ at the heating speed of 6 ℃/h, the materials in the reaction kettle are input into a coking tower by a pump for coking reaction, the coking temperature is 530 ℃, the coking pressure is 0.3-0.8 MPa, the coking time is 36h, and the coke is discharged and dried. And (3) crushing and screening coke, controlling the D50 to be 10-20 mu m, and carrying out graphitization high-temperature treatment for 24h at 2800 ℃ under the protection of inert gas to obtain the wide-area sheet lithium ion battery cathode material. The button cell is assembled by taking the lithium sheet as the anode and the cathode, and the electrochemical performance of the button cell is tested. The negative electrode material and the property index after assembling the button cell are shown in table 1.
Example 5:
mixing coal tar pitch and quinoline solvent in a mixer, conveying the mixture to a reaction kettle, reacting for 3 hours at 120 ℃, standing for 5 hours, extracting an upper layer 80 wt% coal tar pitch sample, and distilling the solvent to obtain the purified coal tar pitch. Conveying the purified coal pitch to a low-temperature carbonization furnace by a pump, wherein the temperature of the low-temperature carbonization furnace is 250 ℃, and the heat preservation time is 9 hours, so that the pitch after low-temperature carbonization is obtained, and the pitch has the softening point of 90 ℃, the hydrogen content of 5.5 wt% and the carbon content of 89 wt%. Conveying the low-temperature carbonized asphalt raw material into a reaction kettle by a pump, circularly heating the material in the reaction kettle by a heating furnace, taking high-purity argon as protective gas, heating the temperature of the heating furnace from 200 ℃ to 420 ℃ by a temperature-raising system of 20 ℃/h, and conveying the material into the reaction kettle for 13h to form the wide-area mesophase structure asphalt. And then, the temperature of the outlet of the heating furnace is increased to 510 ℃ at the heating speed of 5 ℃/h, the materials in the reaction kettle are input into a coking tower by a pump for coking reaction, the coking temperature is 510 ℃, the coking pressure is 0.2-0.5 MPa, the coking time is 30h, and the coke is discharged and dried. And (3) crushing and screening coke, controlling the D50 to be 10-20 mu m, and carrying out graphitization high-temperature treatment for 24h at 2800 ℃ under the protection of inert gas to obtain the wide-area sheet lithium ion battery cathode material. The button cell is assembled by taking the lithium sheet as the anode and the cathode, and the electrochemical performance of the button cell is tested. The negative electrode material and the property index after assembling the button cell are shown in table 1.
TABLE 1 examples negative electrode materials and property indexes after assembling into button cell
Claims (1)
1. The device for preparing the wide-area sheet-structure cathode material special for the lithium ion battery is characterized by comprising a solvent tank, a raw material asphalt tank, a mixer, a purification tank, a distillation tower, a low-temperature carbonization furnace, a reaction kettle, a byproduct oil tank, a heating furnace, a coking tower, a crusher, a screening machine and a graphitization furnace, wherein the solvent tank and the raw material asphalt tank are connected with an inlet of the purification tank through the mixer, an outlet of the purification tank is connected with the distillation tower, a light phase outlet of the distillation tower is connected with the solvent tank, a heavy phase outlet of the distillation tower is connected with the low-temperature carbonization furnace, a light phase outlet of the low-temperature carbonization furnace is connected with the byproduct oil tank, a heavy phase outlet of the low-temperature carbonization furnace is connected with the reaction kettle, a light phase outlet of the reaction kettle is connected with the oil byproduct tank, a heavy phase outlet of the reaction kettle is connected with the coking tower, the reaction kettle is connected with the heating furnace, the crusher feeds materials to the screening machine, and the screening machine feeds materials to the graphitization furnace.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN111453721B (en) * | 2020-04-30 | 2024-08-27 | 中钢集团鞍山热能研究院有限公司 | Preparation method and device of wide-area flaky structure anode material special for lithium ion battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111453721B (en) * | 2020-04-30 | 2024-08-27 | 中钢集团鞍山热能研究院有限公司 | Preparation method and device of wide-area flaky structure anode material special for lithium ion battery |
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