CN112033157A - Lithium ion battery negative electrode material carbonization treatment method and carbonization furnace thereof - Google Patents
Lithium ion battery negative electrode material carbonization treatment method and carbonization furnace thereof Download PDFInfo
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Abstract
The invention discloses a carbonization treatment method of a lithium ion battery cathode material, which comprises the following steps: a. laying a heat insulation pad in the carbonization furnace; b. abutting one end of a first conductive graphite felt against the inner wall of a furnace end of the carbonization furnace and disconnecting the other end of the first conductive graphite felt from the inner wall of a furnace tail of the carbonization furnace at intervals; c. uniformly placing graphite crucibles filled with first cathode materials on the first conductive graphite felt at the same intervals, and filling second cathode materials between the graphite crucibles and the side wall of the carbonization furnace; d. laying a second conductive graphite felt on the graphite crucible layer, wherein one end of the second conductive graphite felt is abutted against the inner wall of the furnace tail of the carbonization furnace and the other end of the second conductive graphite felt is disconnected with the inner wall of the furnace head of the carbonization furnace at intervals; e. paving the furnace top on the second conductive graphite felt; f. feeding power to the carbonization furnace; g. monitoring the temperature field of the carbonization furnace; h. stopping power transmission, and performing heat dissipation and temperature reduction; i. and finishing the carbonization treatment of the first cathode material, and collecting the second cathode material as the first cathode material of the next carbonization treatment.
Description
Technical Field
The invention relates to a carbonization treatment method of a lithium ion battery cathode material, and also relates to a carbonization furnace.
Background
In the industrial production of carbon cathode materials for lithium ion batteries, the powdery carbon intermediate is often subjected to a heat treatment at 900-1400 ℃, which is commonly referred to as carbonization treatment in the industry, and the corresponding equipment is referred to as a carbonization furnace. After carbonization treatment, part of the carbon-like intermediates can be directly used as a negative electrode material for use or sale, and the other part of the carbon-like intermediates can be used only by graphitization treatment at a higher temperature. The graphitization treatment belongs to a production process with high energy consumption and high cost. The pre-carbonization treatment of the raw materials before graphitization can obviously improve the material loading density, improve the single-furnace yield of the graphitization furnace and reduce the production cost of graphitization treatment.
The traditional carbonization treatment device inserts the heating plate in the negative electrode material, and the two ends of the heating plate are electrified to ensure that the heating plate generates heat, and then the negative electrode materials on the two sides of the heating plate are heated and carbonized. However, because the thickness of the negative electrode material is thick, the negative electrode materials at different thickness positions are carbonized to different degrees, and the negative electrode materials in a large range are simultaneously carbonized, so that the energy consumption is high, and the period is long. And the heating plate is not contacted with the cathode material tightly enough due to the rigidity, so that the carbonization efficiency is not high.
Disclosure of Invention
The invention aims to provide a lithium ion battery cathode material carbonization treatment method which is lower in energy consumption, shorter in period and higher in efficiency, and also provides a carbonization furnace for realizing the method.
In order to solve the technical problem, the carbonization treatment method of the lithium ion battery cathode material comprises the following steps:
a. laying a heat insulation pad in the carbonization furnace;
b. laying a first conductive graphite felt on the heat insulation pad, wherein one end of the first conductive graphite felt is abutted against the inner wall of a furnace end of the carbonization furnace, and the other end of the first conductive graphite felt is disconnected from the inner wall of a furnace tail of the carbonization furnace at intervals;
c. uniformly placing graphite crucibles filled with first cathode materials on the first conductive graphite felt at the same intervals, enabling the openings of the graphite crucibles to face upwards, and filling second cathode materials between the graphite crucibles and between the graphite crucibles and the side wall of the carbonization furnace to form a graphite crucible layer;
d. laying a second conductive graphite felt on the graphite crucible layer, covering the graphite crucible opening of the graphite crucible layer, and abutting one end of the second conductive graphite felt against the inner wall of the furnace tail of the carbonization furnace and disconnecting the other end of the second conductive graphite felt from the inner wall of the furnace head of the carbonization furnace at intervals;
e. paving a refractory fiber felt furnace top with an exhaust port on the second conductive graphite felt;
f. the carbonization furnace is electrified, so that current passes through the furnace end, the first conductive graphite felt, the graphite crucible layer, the second conductive graphite felt and the furnace tail in sequence, and the carbonization furnace is electrically heated;
g. monitoring the temperature field of the carbonization furnace by a platinum-rhodium thermocouple at the temperature measuring point of the carbonization furnace;
h. when the temperature field meets the process requirements, stopping power supply, removing the furnace top, dissipating heat and cooling;
i. and taking out the second conductive graphite felt, the graphite crucible, the first conductive graphite felt and the heat insulation pad to finish the carbonization treatment of the first cathode material, and collecting the second cathode material as the first cathode material of the next carbonization treatment.
Repeating the a to d steps after the d step to form a plurality of graphite crucible layers in the carbonization furnace.
Further comprising the step of collecting waste gas from the furnace top exhaust port and performing a harmless treatment.
The method also comprises the steps of arranging two layers of furnace tops and staggering the exhaust ports of the two layers of furnace tops.
The method also comprises a step of reserving a first abutting part used for abutting against the inner wall of the furnace end in parallel at one end of the first conductive graphite felt and a step of reserving a second abutting part used for abutting against the inner wall of the furnace end in parallel at one end of the second conductive graphite felt.
In order to solve the technical problem, the carbonization furnace comprises a furnace end, a furnace tail, a furnace top, a furnace bottom, a furnace side wall, a heat insulation pad, a first conductive graphite felt, a graphite crucible and a second conductive graphite felt; the furnace head and the furnace tail are both made of graphite bricks and are built by conductive adhesives; the outer side walls of the furnace head and the furnace tail are respectively provided with a graphite electrode; the furnace bottom and the furnace side wall are both made of insulating refractory bricks and refractory cement; a cubic furnace chamber is formed among the furnace end, the furnace tail, the furnace top, the furnace bottom and the furnace side wall; the heat insulation pad is horizontally laid on the bottom wall of the furnace chamber; the first conductive graphite felt is laid on the heat insulation pad in the furnace cavity, one end of the first conductive graphite felt is abutted to the inner wall of the furnace end, and the other end of the first conductive graphite felt is disconnected with the inner wall of the furnace tail at intervals; the graphite crucibles are uniformly placed on the first conductive graphite felt in the furnace cavity at the same intervals, and the openings of the graphite crucibles are upward; gaps between the graphite crucible and between the graphite crucible and the furnace side wall are used for preliminary carbonization of the negative electrode material, and an inner cavity of the graphite crucible is used for further carbonization of the negative electrode material; the second conductive graphite felt is laid on the graphite crucible in the furnace cavity and covers the opening of the graphite crucible, one end of the second conductive graphite felt is abutted against the inner wall of the furnace tail, and the other end of the second conductive graphite felt is disconnected with the inner wall of the furnace head at intervals; the furnace top covers the second conductive graphite felt, and the furnace top is a refractory fiber felt provided with an exhaust port; the carbonization furnace is provided with a plurality of temperature measuring points, the temperature measuring points are provided with platinum-rhodium thermocouples, and the platinum-rhodium thermocouples are connected with a temperature field monitoring system.
The heat insulation and preservation cushion, the first conductive graphite felt, the graphite crucible and the second conductive graphite felt are sequentially arranged from bottom to top to form a set of carbonization treatment layer, and a plurality of sets of carbonization treatment layers are arranged in the furnace chamber from bottom to top.
The gas collecting cover is arranged above the gas outlet of the furnace top and connected with a draught fan, and the draught fan is connected with a waste gas purification system.
The furnace top is provided with two layers, and the exhaust ports of the two layers of furnace tops are staggered.
One end of the first conductive graphite felt is provided with a first abutting part which is used for abutting against the inner wall of the furnace end in parallel, one end of the second conductive graphite felt is provided with a second abutting part which is used for abutting against the inner wall of the furnace tail in parallel, the first abutting part faces upwards, and the second abutting part faces downwards.
By adopting the method and the structure, the two conductive graphite felts are adopted in the carbonization furnace to respectively electrify the graphite crucible from the upper end and the lower end, the resistance of the conductive graphite felts is smaller, the graphite crucible is enabled to fully heat between the upper conductive graphite felt and the lower conductive graphite felt, the performance of the conductive graphite felts is stable, the conductive graphite felts can be recycled, and the conductive graphite felts can not be mixed with a negative electrode material to be carbonized; the second negative electrode material to be carbonized is filled in the gap outside the graphite crucible, and the second negative electrode material can fully absorb the residual heat in the carbonization furnace for preliminary carbonization, so that more energy is saved; the second negative electrode material in the previous carbonization process is used as the first negative electrode material in the current carbonization process and is filled in a graphite crucible to be heated and carbonized, and the carbonization period is shorter; the opening at the top of the graphite crucible is covered by the second conductive graphite felt, so that the first cathode material and the second cathode material in the graphite crucible can be prevented from being mixed, the air permeability of the graphite crucible can be better, the second conductive graphite felt can be in contact with the first cathode material in the graphite crucible for electrification, the first cathode material is electrified to actively generate heat and be carbonized, the carbonization efficiency is higher, and the carbonization is more uniform; graphite crucibles are uniformly arranged between the two layers of conductive graphite felts at the same intervals, and a plurality of carbonization treatment layers are laid in the carbonization furnace from bottom to top, so that the carbonization yield of each time is larger; the furnace top is provided with two layers, and exhaust ports of the two layers of furnace tops are staggered, so that heat loss can be reduced, and heat preservation is realized; reserve the first butt portion that is used for parallel butt furnace end inner wall in the one end of first electrically conductive graphite felt, reserve the second butt portion that is used for parallel butt furnace tail inner wall in the one end of the electrically conductive graphite felt of second for first electrically conductive graphite felt is connected inseparabler with the furnace end, and the electrically conductive graphite felt of second is connected inseparabler with the furnace tail.
Drawings
FIG. 1 is a schematic view of a structure of a carbonization furnace according to the present invention.
In the figure: 1-graphite electrode, 2-furnace end, 3-furnace side wall, 4-furnace bottom, 5-heat insulation pad, 6-first conductive graphite felt, 7-graphite crucible, 8-second conductive graphite felt, 9-furnace tail, 10-graphite electrode, 11-exhaust port and 12-furnace top.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
The invention discloses a carbonization treatment method of a lithium ion battery cathode material, which comprises the following steps:
a. laying a heat insulation pad in the carbonization furnace; the heat insulation pad can be made of ceramic fiber refractory cotton or refractory heat insulation bricks, so that the heat insulation pad not only can insulate heat, but also is insulating, and has better adaptability and buffering performance.
b. Laying a first conductive graphite felt on the heat insulation pad, wherein one end of the first conductive graphite felt is abutted against the inner wall of a furnace end of the carbonization furnace, and the other end of the first conductive graphite felt is disconnected from the inner wall of a furnace tail of the carbonization furnace at intervals; the first conductive graphite felt is used for connecting current of the furnace end to the bottom of the graphite crucible. The conductive graphite felt can be laid in a whole piece, or a plurality of pieces can be lapped end to end; the conductive graphite felt is thin in thickness, small in occupied space, capable of elastically deforming well and convenient to be tightly connected with the graphite crucible and the cathode material.
c. Uniformly placing graphite crucibles filled with first cathode materials on the first conductive graphite felt at the same intervals, enabling the openings of the graphite crucibles to face upwards, and filling second cathode materials between the graphite crucibles and between the graphite crucibles and the side wall of the carbonization furnace to form a graphite crucible layer; the resistance of the graphite crucible is greater than the resistance of the first conductive graphite felt and the resistance of the second conductive graphite felt, and the average carbonization degree of the first negative electrode material is higher than that of the second negative electrode material, so that the first negative electrode material is heated and carbonized preferentially; the top of the graphite crucible is provided with an opening, so that the ventilation is facilitated, the first cathode material is directly contacted and electrified with the second conductive graphite felt, the first cathode material can be heated and carbonized by the graphite crucible, and meanwhile, the first cathode material can be actively heated and carbonized by self electrification, so that the first cathode material is more fully and uniformly carbonized; the second cathode material can play roles in filling, supporting and heat preservation, and simultaneously fully absorbs heat emitted outwards by the graphite crucible, the first conductive graphite felt and the second conductive graphite felt to carry out primary carbonization, so that more energy is saved.
d. Laying a second conductive graphite felt on the graphite crucible layer, covering the graphite crucible opening of the graphite crucible layer, supporting the graphite crucible and a second cathode material filled in the side part of the graphite crucible, and abutting one end of the second conductive graphite felt against the inner wall of the furnace tail of the carbonization furnace and disconnecting the other end of the second conductive graphite felt from the inner wall of the furnace head of the carbonization furnace at intervals; the second conductive graphite felt is used for connecting the current of the furnace tail to the top of the graphite crucible. The material and the electric conductivity of the second conductive graphite felt are the same as those of the first conductive graphite felt; the second conductive graphite felt covers the top opening of the graphite crucible, so that the second negative electrode material can be prevented from being mixed with the first negative electrode material in the crucible, the first negative electrode material is independently carbonized in the graphite crucible, and the carbonization degree of the first negative electrode material is more uniform.
e. Paving a refractory fiber felt furnace top with an exhaust port on the second conductive graphite felt; the refractory fiber felt can be graphite felt, carbon felt, ceramic fiber cotton and the like; the refractory fiber felt has better heat preservation performance and light weight; the exhaust port is used for exhausting volatile gas generated in the heating carbonization process of the negative electrode material.
f. Feeding electricity to the carbonization furnace, preferably selecting direct current, applying variable voltage according to carbonization requirements, enabling the current to sequentially pass through the furnace head, the first conductive graphite felt, the graphite crucible layer, the second conductive graphite felt and the furnace tail, and electrically heating the carbonization furnace; the current mainly passes through the furnace head, the first conductive graphite felt, the graphite crucible layer, the second conductive graphite felt and the furnace tail, and then passes through the first cathode material, and the current passing through the second cathode material is the minimum; the graphite crucible is preferentially heated, and the first negative electrode material in the graphite crucible is preferentially carbonized.
g. Monitoring the temperature field of the carbonization furnace by a platinum-rhodium thermocouple at the temperature measuring point of the carbonization furnace; the temperature field monitoring system is connected with the platinum-rhodium thermocouple and used for acquiring temperature field data of the carbonization furnace; the temperature measuring point is used for monitoring the temperature of the graphite crucible, the temperature of the conductive graphite felt, the temperature of the cathode material and the temperature of the inner wall of the furnace.
h. When the temperature field meets the process requirements, stopping power supply, removing the furnace top, dissipating heat and cooling;
i. and taking out the second conductive graphite felt, the graphite crucible, the first conductive graphite felt, the heat insulation pad and the second cathode material layer by layer from top to bottom, taking out the first cathode material from the graphite crucible, completing the carbonization treatment of the first cathode material, taking out the second cathode material from the carbonization furnace, and collecting the second cathode material as the first cathode material for the next carbonization treatment.
Repeating steps a to d after step d to form a plurality of graphite crucible layers in the carbonization furnace. Namely, the bottom of each layer of graphite crucible layer is provided with a first conductive graphite felt and a heat insulation pad, the top of each layer of graphite crucible layer is provided with a second conductive graphite felt, and each layer of graphite crucible layer is heated and carbonized independently. The carbonization furnace is internally provided with a plurality of graphite crucible layers for carbonization, so that the single carbonization yield of the carbonization furnace is higher. In the structure of the multilayer graphite crucible layer, due to the filling of the second cathode material, the support and stabilization effects can be better achieved, and the collapse can be reduced.
The method also comprises the step of collecting waste gas from the exhaust port at the top of the furnace and carrying out innocent treatment, wherein the innocent treatment mainly comprises the treatment steps of cyclone dust removal, water washing, temperature reduction and the like, so that the air pollution can be reduced, and the method is more environment-friendly.
The method also comprises the steps of arranging two layers of furnace tops and mutually staggering the exhaust ports of the two layers of furnace tops, so that part of dust can be retained, the door of the carbonization furnace is prevented from being opened greatly, and heat loss is reduced.
The method also comprises a step of reserving a first abutting part used for abutting against the inner wall of the furnace end in parallel at one end of the first conductive graphite felt and a step of reserving a second abutting part used for abutting against the inner wall of the furnace end in parallel at one end of the second conductive graphite felt. The first butt joint portion and the parallel butt of furnace end inner wall of first electrically conductive graphite felt tip, the second butt joint portion and the parallel butt of stove tail inner wall of the electrically conductive graphite felt tip of second for the contact surface is bigger, and the circular telegram performance is better more stable, and reserve as the butt is reserve, can avoid leading to the disconnection of butt because of the second cathode material sinks.
As shown in fig. 1, the carbonization furnace for implementing carbonization of the lithium ion battery cathode material comprises a furnace end, a furnace tail, a furnace top, a furnace bottom, a furnace side wall, a heat insulation pad, a first conductive graphite felt, a graphite crucible and a second conductive graphite felt. The furnace head and the furnace tail are positioned at two ends of the carbonization furnace, the furnace side walls are positioned at two sides of the carbonization furnace, the furnace top is positioned at the top of the carbonization furnace, and the furnace top is positioned at the bottom of the carbonization furnace. The furnace end, the furnace tail and the furnace side wall are all fixedly connected with the furnace bottom. The graphite crucible is a cuboid or cylindrical pot, and the top of the graphite crucible is provided with a circular pot opening.
The furnace head and the furnace tail are both made of graphite bricks and are built by conductive adhesive; the inner walls of the furnace head and the furnace tail are both conductive; the outer side walls of the furnace head and the furnace tail are respectively provided with a graphite electrode which is used for connecting a power supply; the furnace bottom and the furnace side wall are both made of insulating refractory bricks and refractory cement; a cubic furnace chamber is formed among the furnace end, the furnace tail, the furnace top, the furnace bottom and the furnace side wall;
the heat insulation pad at the bottommost layer is horizontally laid on the bottom wall of the furnace chamber; the heat insulation pad can be made of ceramic fiber refractory cotton or refractory heat insulation bricks, so that the heat insulation pad not only can insulate heat, but also is insulating, and has better adaptability and buffering performance.
A first conductive graphite felt is laid on the heat insulation pad in the furnace cavity, one end of the first conductive graphite felt is abutted with the inner wall of the furnace end, and the other end of the first conductive graphite felt is disconnected with the inner wall of the furnace tail at intervals; the first conductive graphite felt is used for connecting current of the furnace end to the bottom of the graphite crucible. The conductive graphite felt can be laid in a whole piece, or a plurality of pieces can be lapped end to end; the conductive graphite felt is thin in thickness, small in occupied space, capable of elastically deforming well and convenient to be tightly connected with the graphite crucible and the cathode material.
The graphite crucibles are uniformly placed on the first conductive graphite felt in the furnace cavity at the same intervals, and the openings of the graphite crucibles are upward; gaps between the graphite crucible and between the graphite crucible and the furnace side wall are used for preliminary carbonization of the cathode material, and an inner cavity of the graphite crucible is used for further carbonization of the cathode material; when the graphite crucible is used, the inside and the outside of the graphite crucible are filled with the negative electrode material, but the negative electrode material filled in the graphite crucible is the negative electrode material filled in the gap outside the graphite crucible in the previous carbonization treatment process. The resistance of the graphite crucible is greater than the resistance of the first conductive graphite felt and the resistance of the second conductive graphite felt, the average carbonization degree of the first negative electrode material in the graphite crucible is higher than the average carbonization degree of the second negative electrode material outside the graphite crucible, so that the first negative electrode material is heated and carbonized preferentially; the top of the graphite crucible is provided with an opening, so that the ventilation is facilitated, the first cathode material is directly contacted and electrified with the second conductive graphite felt, the first cathode material can be heated and carbonized by the graphite crucible, and meanwhile, the first cathode material can be actively heated and carbonized by self electrification, so that the first cathode material is more fully and uniformly carbonized; the second cathode material can play roles in filling, supporting and heat preservation, and simultaneously fully absorbs heat emitted outwards by the graphite crucible, the first conductive graphite felt and the second conductive graphite felt to carry out primary carbonization, so that more energy is saved.
The second conductive graphite felt is laid on the graphite crucible in the furnace cavity and covers the opening of the graphite crucible, one end of the second conductive graphite felt is abutted against the inner wall of the furnace tail, and the other end of the second conductive graphite felt is disconnected with the inner wall of the furnace head at intervals; the second conductive graphite felt is used for connecting the current of the furnace tail to the top of the graphite crucible. The material and the electric conductivity of the second conductive graphite felt are the same as those of the first conductive graphite felt; the second conductive graphite felt covers the top opening of the graphite crucible, so that the second negative electrode material can be prevented from being mixed with the first negative electrode material in the crucible, the first negative electrode material is independently carbonized in the graphite crucible, and the carbonization degree of the first negative electrode material is more uniform.
The furnace top covers the second conductive graphite felt, and the furnace top is a refractory fiber felt provided with an exhaust port; the refractory fiber felt can be graphite felt, carbon felt, ceramic fiber cotton and the like; the refractory fiber felt has better heat preservation performance and light weight; the exhaust port is used for exhausting volatile gas generated in the heating carbonization process of the negative electrode material. The carbonization furnace is provided with a plurality of temperature measuring points which are respectively arranged at the side part and the top part. The temperature measuring point is provided with a platinum-rhodium thermocouple for collecting temperature field data of the carbonization furnace, and the platinum-rhodium thermocouple is connected with a temperature field monitoring system.
When the electric heating carbonization furnace is used, power is supplied to the carbonization furnace, direct current is preferably selected, variable voltage is applied according to carbonization requirements, and the electric current sequentially passes through the furnace end, the first conductive graphite felt, the graphite crucible layer, the second conductive graphite felt and the furnace tail to electrically heat the carbonization furnace; the current mainly passes through the furnace head, the first conductive graphite felt, the graphite crucible layer, the second conductive graphite felt and the furnace tail, and then passes through the first cathode material, and the current passing through the second cathode material is the minimum; the graphite crucible is preferentially heated, and the first negative electrode material in the graphite crucible is preferentially carbonized. When the temperature field meets the process requirements, stopping power supply, removing the furnace top, dissipating heat and cooling; and taking out the second conductive graphite felt, the graphite crucible, the first conductive graphite felt, the heat insulation pad and the second cathode material layer by layer from top to bottom, taking out the first cathode material from the graphite crucible, completing the carbonization treatment of the first cathode material, taking out the second cathode material from the carbonization furnace, and collecting the second cathode material as the first cathode material for the next carbonization treatment.
As shown in fig. 1, the heat insulation pad, the first conductive graphite felt, the graphite crucible and the second conductive graphite felt are sequentially arranged from bottom to top to form a set of carbonization treatment layers, and a plurality of sets of carbonization treatment layers are arranged from bottom to top in the furnace chamber. Each set of carbonization treatment layer is relatively independently heated and carbonized. A plurality of carbonization treatment layers are arranged in the carbonization furnace for carbonization treatment, so that the single carbonization treatment yield of the carbonization furnace is higher. In the structure of the multilayer carbonization treatment layer, due to the filling and supporting of the second cathode material, the stability is better, and the collapse can be reduced.
As shown in fig. 1, a gas collecting cover is arranged above the gas outlet of the furnace top, the gas collecting cover is connected with a draught fan, and the draught fan is connected with a waste gas purification system. The waste gas purification system comprises a cyclone dust collector, a water washing cooling center and other equipment, so that air pollution can be reduced, and the waste gas purification system is more environment-friendly.
As shown in fig. 1, the furnace top is provided with two layers, and the exhaust ports of the two layers of furnace tops are staggered with each other, so that part of dust can be retained, meanwhile, the door of the carbonization furnace is prevented from being opened greatly, and heat loss is reduced.
As shown in fig. 1, one end of the first conductive graphite felt is provided with a first abutting portion for abutting against the inner wall of the furnace end in parallel, one end of the second conductive graphite felt is provided with a second abutting portion for abutting against the inner wall of the furnace end in parallel, the first abutting portion faces upwards, and the second abutting portion faces downwards. Parallel butt makes the contact surface bigger, and the circular telegram performance is better more steady, and first butt portion and second butt portion reserve for use as the butt, can avoid leading to the disconnection of butt because of the second negative pole material sinks.
Claims (10)
1. A carbonization treatment method for a lithium ion battery cathode material is characterized by comprising the following steps:
a. laying a heat insulation pad in the carbonization furnace;
b. laying a first conductive graphite felt on the heat insulation pad, wherein one end of the first conductive graphite felt is abutted against the inner wall of a furnace end of the carbonization furnace, and the other end of the first conductive graphite felt is disconnected from the inner wall of a furnace tail of the carbonization furnace at intervals;
c. uniformly placing graphite crucibles filled with first cathode materials on the first conductive graphite felt at the same intervals, enabling the openings of the graphite crucibles to face upwards, and filling second cathode materials between the graphite crucibles and between the graphite crucibles and the side wall of the carbonization furnace to form a graphite crucible layer;
d. laying a second conductive graphite felt on the graphite crucible layer, covering the graphite crucible opening of the graphite crucible layer, and abutting one end of the second conductive graphite felt against the inner wall of the furnace tail of the carbonization furnace and disconnecting the other end of the second conductive graphite felt from the inner wall of the furnace head of the carbonization furnace at intervals;
e. paving a refractory fiber felt furnace top with an exhaust port on the second conductive graphite felt;
f. the carbonization furnace is electrified, so that current passes through the furnace end, the first conductive graphite felt, the graphite crucible layer, the second conductive graphite felt and the furnace tail in sequence, and the carbonization furnace is electrically heated;
g. monitoring the temperature field of the carbonization furnace by a platinum-rhodium thermocouple at the temperature measuring point of the carbonization furnace;
h. when the temperature field meets the process requirements, stopping power supply, removing the furnace top, dissipating heat and cooling;
i. and taking out the second conductive graphite felt, the graphite crucible, the first conductive graphite felt and the heat insulation pad to finish the carbonization treatment of the first cathode material, and collecting the second cathode material as the first cathode material of the next carbonization treatment.
2. The carbonization treatment method of the lithium ion battery negative electrode material according to claim 1, characterized in that: repeating the a to d steps after the d step to form a plurality of graphite crucible layers in the carbonization furnace.
3. The carbonization treatment method of the lithium ion battery negative electrode material according to claim 1, characterized in that: further comprising the step of collecting waste gas from the furnace top exhaust port and performing a harmless treatment.
4. The carbonization treatment method of the lithium ion battery negative electrode material according to claim 1, characterized in that: the method also comprises the steps of arranging two layers of furnace tops and staggering the exhaust ports of the two layers of furnace tops.
5. The carbonization treatment method of the lithium ion battery negative electrode material according to claim 1, characterized in that: the method also comprises a step of reserving a first abutting part used for abutting against the inner wall of the furnace end in parallel at one end of the first conductive graphite felt and a step of reserving a second abutting part used for abutting against the inner wall of the furnace end in parallel at one end of the second conductive graphite felt.
6. A retort for carrying out the method of claim 1, characterized in that: the furnace comprises a furnace end, a furnace tail, a furnace top, a furnace bottom, a furnace side wall, a heat insulation pad, a first conductive graphite felt, a graphite crucible and a second conductive graphite felt;
the furnace head and the furnace tail are both made of graphite bricks and are built by conductive adhesives; the outer side walls of the furnace head and the furnace tail are respectively provided with a graphite electrode; the furnace bottom and the furnace side wall are both made of insulating refractory bricks and refractory cement; a cubic furnace chamber is formed among the furnace end, the furnace tail, the furnace top, the furnace bottom and the furnace side wall;
the heat insulation pad is horizontally laid on the bottom wall of the furnace chamber;
the first conductive graphite felt is laid on the heat insulation pad in the furnace cavity, one end of the first conductive graphite felt is abutted to the inner wall of the furnace end, and the other end of the first conductive graphite felt is disconnected with the inner wall of the furnace tail at intervals;
the graphite crucibles are uniformly placed on the first conductive graphite felt in the furnace cavity at the same intervals, and the openings of the graphite crucibles are upward; gaps between the graphite crucible and between the graphite crucible and the furnace side wall are used for preliminary carbonization of the negative electrode material, and an inner cavity of the graphite crucible is used for further carbonization of the negative electrode material;
the second conductive graphite felt is laid on the graphite crucible in the furnace cavity and covers the opening of the graphite crucible, one end of the second conductive graphite felt is abutted against the inner wall of the furnace tail, and the other end of the second conductive graphite felt is disconnected with the inner wall of the furnace head at intervals;
the furnace top covers the second conductive graphite felt, and the furnace top is a refractory fiber felt provided with an exhaust port; the carbonization furnace is provided with a plurality of temperature measuring points, the temperature measuring points are provided with platinum-rhodium thermocouples, and the platinum-rhodium thermocouples are connected with a temperature field monitoring system.
7. Carbonization furnace according to claim 6, characterized in that: the heat insulation and preservation cushion, the first conductive graphite felt, the graphite crucible and the second conductive graphite felt are sequentially arranged from bottom to top to form a set of carbonization treatment layer, and a plurality of sets of carbonization treatment layers are arranged in the furnace chamber from bottom to top.
8. Carbonization furnace according to claim 6, characterized in that: the gas collecting cover is arranged above the gas outlet of the furnace top and connected with a draught fan, and the draught fan is connected with a waste gas purification system.
9. Carbonization furnace according to claim 6, characterized in that: the furnace top is provided with two layers, and the exhaust ports of the two layers of furnace tops are staggered.
10. Carbonization furnace according to claim 6, characterized in that: one end of the first conductive graphite felt is provided with a first abutting part which is used for abutting against the inner wall of the furnace end in parallel, one end of the second conductive graphite felt is provided with a second abutting part which is used for abutting against the inner wall of the furnace tail in parallel, the first abutting part faces upwards, and the second abutting part faces downwards.
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| CN202011081661.3A CN112033157A (en) | 2020-10-12 | 2020-10-12 | Lithium ion battery negative electrode material carbonization treatment method and carbonization furnace thereof |
| PCT/CN2020/123528 WO2022077550A1 (en) | 2020-10-12 | 2020-10-26 | Carbonization treatment method for negative electrode material of lithium ion battery and carbonization furnace thereof |
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| CN116281995B (en) * | 2023-03-22 | 2024-01-30 | 宁夏碳谷能源科技股份有限公司 | Graphitization pretreatment method for negative electrode material |
| CN117263177B (en) * | 2023-09-26 | 2024-05-17 | 连云港埃纳硅业有限公司 | Internal string graphitizing furnace for artificial graphite negative electrode material |
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| JPH11233111A (en) * | 1998-02-18 | 1999-08-27 | Petoca Ltd | Manufacture of graphite for lithium ion secondary battery negative electrode |
| CN103964423B (en) * | 2014-05-04 | 2017-01-11 | 郴州市三晶科贸有限公司 | Production method of artificial graphite cathode materials in manner of inner tandem graphitization and graphitization furnace |
| CN107416821A (en) * | 2017-09-12 | 2017-12-01 | 韶关市新弘立冶金实业有限公司 | A kind of production method that carburant is produced using graphitizing furnace |
| CN108439391A (en) * | 2018-05-15 | 2018-08-24 | 邓华强 | The method for obtaining coal measures graphite using silicon carbide furnace transformer and matched resistance furnace |
| CN109179399A (en) * | 2018-10-09 | 2019-01-11 | 重庆卡森科技有限公司 | A kind of combination graphitization processing technique of negative electrode material and carburant |
| CN111595151A (en) * | 2020-05-27 | 2020-08-28 | 郴州杉杉新材料有限公司 | Carbonization furnace for carbonizing lithium ion battery negative electrode material |
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