CN108866575B - Preparation method of graphite anode - Google Patents
Preparation method of graphite anode Download PDFInfo
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- CN108866575B CN108866575B CN201810689678.3A CN201810689678A CN108866575B CN 108866575 B CN108866575 B CN 108866575B CN 201810689678 A CN201810689678 A CN 201810689678A CN 108866575 B CN108866575 B CN 108866575B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
- C25C3/12—Anodes
- C25C3/125—Anodes based on carbon
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method of a graphite anode. The method comprises the following steps: step one, placing an unqualified product of a prebaked anode in a graphitization pretreatment device for pretreatment for 1-2 hours to obtain a material A; step two, placing the materials A in a graphitization furnace for series connection, wrapping the periphery of the materials A in series connection by using a filling material, and then electrifying the materials A for 10-15 hours under the condition of isolating air, so that the temperature in the furnace is gradually increased from normal temperature to 2200-3000 ℃ to obtain materials B; and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode. According to the invention, the unqualified product of the prebaked anode is placed in the graphitization pretreatment device for pretreatment, so that the acne burnt on the surface of the unqualified product of the prebaked anode, the residue bulge and impurities which are transversely cracked in the surface of the unqualified product of the prebaked anode can be effectively removed, and the graphitization pretreatment device is beneficial to improving the true density and the compressive strength.
Description
Technical Field
The invention relates to the technical field of graphite anode production, in particular to a preparation method of a graphite anode.
Background
The electricity consumption is the largest production cost of aluminum electrolysis manufacturers. The largest factors affecting electricity consumption are directly related to the structure and configuration of the electrolyzer, as well as the quality, structure and configuration of the anode and cathode. The influence of the internal quality of the anode and the cathode on the working resistivity of the electrolytic cell is one of the important factors, and the graphitized cathode is the conductive material used for the cathode of the aluminum electrolytic cell and represents the development direction of the electrolytic aluminum industry. With the technical progress and development of the electrolytic aluminum industry, the electrolytic tank is developed to a large capacity of more than 300 kilowatts, and the requirement on cathode materials is higher. For graphitized cathodes with better production quality, the high standard raw materials used are critical, and how to obtain high standard raw materials at low cost is a current research problem. Aiming at the difficult problem, the inventor finds that the graphite anode with low resistivity, less internal transverse crack, high compressive strength, low ash content and other excellent performances is obtained by preprocessing the unqualified product of the baked anode and then carrying out power transmission treatment of the graphitization furnace, thereby changing waste into valuables, reducing waste emission in the graphitization production process, reducing the raw material production cost and realizing the synergy of enterprises. The graphite anode can also be used as aggregate of a graphite cathode for rapidly producing high-quality graphite cathodes.
Disclosure of Invention
It is an object of the present invention to address at least the above-mentioned drawbacks and to provide at least the advantages to be described later.
To achieve these objects and other advantages and in accordance with the purpose of the invention, a method for preparing a graphite anode is provided, comprising the steps of:
step one, placing an unqualified product of a prebaked anode in a graphitization pretreatment device for pretreatment for 1-2 hours to obtain a material A;
step two, placing the materials A in a graphitization furnace for series connection, wrapping the periphery of the materials A in series connection by using a filling material, and then electrifying the materials A for 10-15 hours under the condition of isolating air, so that the temperature in the furnace is gradually increased from normal temperature to 2200-3000 ℃ to obtain materials B;
and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode.
Preferably, the condition of isolating air in the step two is that the graphitization furnace is vacuumized.
Preferably, the filler is calcined coke particles.
Preferably, the graphitization pretreatment device includes:
the upper opening square container is provided with an inlet and an outlet on the side wall of the lower part, and is correspondingly provided with a switch door capable of sealing and closing the inlet and the outlet, and the bottom of the container is provided with a water inlet and drainage valve;
the elastic coiled plates are alternately arranged on the inner walls of the left side and the right side of the upper part of the square container in a staggered manner, the elastic coiled plates are arc-shaped plates which are bent upwards, the chord length of each arc-shaped plate is greater than one half of the distance from the left side to the right side of the square container and less than two thirds of the distance from the left side to the right side of the square container, and the corresponding angle of each arc-shaped plate is greater than 100 degrees and less than 180 degrees;
a plurality of vibrators fixed below the elastic coiled plate;
the net box with an upper opening is tightly and movably embedded at the lower part of the square container in an up-and-down moving way;
the telescopic rod is arranged at the bottom of the square container and connected with the bottom of the net cage to push the net cage to move up and down in the square container.
Preferably, naphtha immersed in the net cage is contained in the lower part of the square container.
Preferably, the upper opening of the square container is a funnel inlet.
Preferably, the plurality of elastic coiled plates are four elastic coiled plates, two elastic coiled plates are alternately arranged on the left side wall and the right side wall of the upper part of the square container respectively, a first elastic coiled plate is arranged on the left side from top to bottom, a second elastic coiled plate is arranged 10-20cm lower than the first elastic coiled plate on the right side, a third elastic coiled plate is arranged 10-20cm lower than the second elastic coiled plate on the left side, a fourth elastic coiled plate is arranged 10-20cm lower than the third elastic coiled plate on the right side, the plurality of vibrators are four vibrators, one vibrator is fixed below each elastic coiled plate, and the vibrators are positioned between the middle part of the elastic coiled plates and a square fixed point and between the front wall and the rear wall of the square container.
Preferably, the upper surface of the elastic coiled plate is provided with circular bulges, the meshes of the side wall of the net cage are triangular meshes, the thickness of the bottom of the net cage is 0.5-2cm, and the meshes of the bottom are conical holes from bottom to top. The conical holes enable the net cage to generate larger impact force on unqualified products of the prebaked anode in the up-and-down movement process, the triangular meshes effectively prevent the net cage from deforming, the up-and-down movement obstacle is reduced, and the operation efficiency is improved.
Preferably, the telescopic rod is a telescopic magnetic rod, and the bottom of the net cage is made of soft magnetic materials, so that the telescopic magnetic rod can fix the net cage through magnetic force in an electrified state and can push the net cage to move up and down in the square container. The unqualified product of the prebaked anode can continuously cut activated atoms in a magnetic field environment, which is favorable for orderly converting a disordered layer structure into a graphite crystal structure in the graphitization process.
Preferably, in the first step, the specific operation of placing the unqualified product of the prebaked anode in the graphitization pretreatment device for pretreatment is as follows: the unqualified products of the prebaked anode are added into a graphitization pretreatment device from the upper opening of the square container, continuously rubbed and collided by a plurality of elastic coiled plates, then enter a net cage, the unqualified products of the prebaked anode are driven by the net cage to be continuously soaked and impacted in naphtha for 1-2 hours, then power is cut off for a telescopic rod, filtered naphtha is discharged, and then the material A is taken out from a side wall inlet and outlet of the square container.
The invention at least comprises the following beneficial effects: according to the invention, the unqualified product of the prebaked anode is placed in the graphitization pretreatment device for pretreatment, so that the acne burnt on the surface of the unqualified product of the prebaked anode, the residue bulge and impurities which are transversely cracked in the surface of the unqualified product of the prebaked anode can be effectively removed, and the graphitization pretreatment device is beneficial to improving the true density and the compressive strength. And then, carrying out series connection and electrifying heating on the pretreated material A, so that internal transverse cracks are densely fused, ash content and resistivity are reduced, and compressive strength is improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
Fig. 1 is a schematic structural view of a graphitization pretreatment apparatus according to the present invention.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
Example 1
A preparation method of a graphite anode comprises the following steps:
firstly, placing an unqualified product of a prebaked anode in a graphitization pretreatment device for pretreatment for 1 hour to obtain a material A;
step two, placing the materials A in a graphitizing furnace for serial connection, wrapping the periphery of the serial materials A by using a filling material, and electrifying the materials A for 10 hours under the condition of isolating air, so that the temperature in the furnace is gradually increased from normal temperature to 2200 ℃ to obtain materials B;
and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode.
Example 2
A preparation method of a graphite anode comprises the following steps:
firstly, placing an unqualified product of a prebaked anode in a graphitization pretreatment device for pretreatment for 2 hours to obtain a material A;
step two, placing the material A in a graphitization furnace for serial connection, wrapping the periphery of the serial material A by calcined coke particles, and electrifying the material A for 15 hours after vacuumizing the graphitization furnace, so that the temperature in the furnace is gradually increased to 3000 ℃ from normal temperature to obtain a material B;
and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode.
Example 3
A preparation method of a graphite anode comprises the following steps:
firstly, placing an unqualified product of a prebaked anode in a graphitization pretreatment device for pretreatment for 1.5 hours to obtain a material A;
step two, placing the material A in a graphitization furnace for serial connection, wrapping the periphery of the serial material A by calcined coke particles, and electrifying the material A for 10 hours after vacuumizing the graphitization furnace, so that the temperature in the furnace is gradually increased to 2500 ℃ from normal temperature to obtain a material B;
and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode.
Example 4
A preparation method of a graphite anode comprises the following steps:
firstly, adding an unqualified product of a prebaked anode into a graphitization pretreatment device from an upper opening of a square container, continuously rubbing and colliding the unqualified product of the prebaked anode through a plurality of elastic coiled plates, entering a net cage, continuously soaking and impacting the unqualified product of the prebaked anode in naphtha by the net cage for 2 hours, powering off a telescopic rod, discharging filtered naphtha, and taking out a material A from a side wall inlet and outlet of the square container;
step two, placing the material A in a graphitization furnace for serial connection, wrapping the periphery of the serial material A by calcined coke particles, and electrifying the material A for 15 hours after vacuumizing the graphitization furnace, so that the temperature in the furnace is gradually increased to 2800 ℃ from normal temperature to obtain a material B;
and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode.
Wherein fig. 1 shows a specific implementation form of the graphitization pretreatment device, which comprises:
the square container with an upper opening, the side wall of the lower part of the square container is provided with an inlet and an outlet, and a switch door capable of sealing and closing the inlet and the outlet is correspondingly arranged, and the bottom of the square container is provided with a water inlet and outlet valve 8;
the elastic coiled plates 4 are alternately arranged on the left side wall and the right side wall of the upper part of the square container in a staggered manner, the elastic coiled plates 4 are arc-shaped plates which are bent upwards, the chord length of each arc-shaped plate is greater than one half of the distance from the left side to the right side of the square container and less than two thirds of the distance from the left side to the right side of the square container, and the corresponding angle of each arc-shaped plate is greater than 100 degrees and less than 180 degrees;
a plurality of vibrators 2 fixed below the elastic coiled plate 4;
a net cage 5 with an upper opening, which is tightly and movably embedded at the lower part of the square container;
and the telescopic rod 7 is arranged at the bottom of the square container and is connected with the bottom of the net cage 5 to push the net cage 5 to move up and down in the square container.
Further, naphtha immersed in the net cage 5 is contained in the lower part of the square container.
Further, the upper opening of the square container is a funnel inlet 1.
Further, the plurality of elastic coiled plates 4 are four elastic coiled plates 4, two elastic coiled plates are arranged on the left side wall and the right side wall of the upper portion of the square container alternately, the two elastic coiled plates are arranged from top to bottom, a first elastic coiled plate 4 is arranged on the left side, a second elastic coiled plate 4 is arranged 10 cm to 20cm lower than the first elastic coiled plate on the right side, a third elastic coiled plate 4 is arranged 10 cm to 20cm lower than the second elastic coiled plate on the left side, a fourth elastic coiled plate 4 is arranged 10 cm to 20cm lower than the third elastic coiled plate on the right side, the plurality of vibrators 2 are four vibrators, one vibrator 2 is fixed below each elastic coiled plate 4, and the vibrators are located between the middle of the elastic coiled plate 4 and a fixed point of the square container wall and are located between the front wall and the rear wall of the square container.
Further, the upper surface of the elastic coiled plate 4 is provided with circular bulges 3, meshes on the side wall of the net cage 5 are triangular meshes, the thickness of the bottom of the net cage 5 is 0.5-2cm, and the meshes on the bottom are conical holes 6 from bottom to top. The conical holes 6 enable the net cage to generate larger impact force on unqualified products of the prebaked anode in the up-and-down movement process, effectively prevent the net cage from deforming, reduce up-and-down movement disorder and improve operation efficiency.
Further, the telescopic rod 7 is a telescopic magnetic rod, and the bottom of the net cage 5 is made of soft magnetic materials, so that the telescopic magnetic rod can fix the net cage 5 through magnetic force in an electrified state and can push the net cage to move up and down in the square container. The unqualified product of the prebaked anode can continuously cut the activation atoms of the magnetic induction lines in the magnetic field environment, which is favorable for orderly converting the disordered layer structure into the graphite crystal structure in the graphitization process.
Example 5
A preparation method of a graphite anode comprises the following steps:
firstly, adopting the graphitization pretreatment device, adding the unqualified product of the prebaked anode into the graphitization pretreatment device from the upper opening of the square container, enabling the unqualified product of the prebaked anode to roll back and forth on the first elastic coiled plate, combining vibration of a vibrator, increasing rolling and jumping frequency of the unqualified product of the prebaked anode on the first elastic coiled plate, after the unqualified product of the prebaked anode of the first elastic coiled plate is accumulated to a certain weight, rolling the unqualified product with the prebaked anode to the second elastic coiled plate continuously, rolling and jumping for the second time until the unqualified product with the prebaked anode rolls into a net cage soaked with naphtha from the fourth elastic coiled plate, then starting a telescopic magnetic rod to move, enabling the net cage made of soft magnetic materials to be fixed by magnetic force generated by electrifying the telescopic magnetic rod, enabling the net cage with the unqualified product of the prebaked anode to move up and down in naphtha, enabling the net cage with the unqualified product of the prebaked anode to move up and down continuously, enabling naphtha to roll down in the naphtha to be washed for 1 hour, then discharging the naphtha from the side wall of the square container to be discharged from the side wall of the square container;
step two, placing the material A in a graphitization furnace for serial connection, wrapping the periphery of the serial material A by calcined coke particles, and electrifying the material A for 10 hours after vacuumizing the graphitization furnace, so that the temperature in the furnace is gradually increased from normal temperature to 2200 ℃ to obtain a material B;
and thirdly, cooling the material B, and discharging the material B to obtain the graphite anode.
Comparative example 1: the graphite anodes were prepared from the same quality and same amount of defective products of the prebaked anodes, but without pretreatment, and the other steps were the same as in example 1, and the average values of the internal transverse crack ratio, true density, room temperature resistivity, compressive strength, ash content of the graphite anodes prepared in example 1 and comparative example 1 were as shown in table 1.
Comparative example 2: the graphite anode was prepared from the same quality and same amount of defective products of the prebaked anode, but the series-connected material a was not wrapped around with calcined coke particles, and the graphitization furnace was not evacuated, and the other steps were the same as in example 2, and the average values of the internal transverse crack ratio, true density, room temperature resistivity, compressive strength, and ash content of the graphite anodes prepared in example 2 and comparative example 2 were as shown in table 2.
Comparative example 3: the graphite anodes were prepared from the same quality and same amount of defective products of the prebaked anodes, but without pretreatment by the graphitization pretreatment apparatus of the present invention, the other steps were the same as in example 5, and the average values of the internal transverse crack ratio, true density, room temperature resistivity, compressive strength, ash content of the graphite anodes prepared in example 5 and comparative example 3 were shown in table 23.
Table 1:
table 2:
table 3:
although embodiments of the invention have been disclosed above, they are not limited to the use listed in the specification and embodiments. It can be applied to various fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art.
Claims (4)
1. The preparation method of the graphite anode is characterized by comprising the following steps:
step one, placing an unqualified product of a prebaked anode in a graphitization pretreatment device for pretreatment for 1-2 hours to obtain a material A;
step two, placing the materials A in a graphitization furnace for series connection, wrapping the periphery of the materials A in series connection by using a filling material, and then electrifying the materials A for 10-15 hours under the condition of isolating air, so that the temperature in the furnace is gradually increased from normal temperature to 2200-3000 ℃ to obtain materials B;
step three, cooling the material B, and discharging to obtain a graphite anode;
wherein, the graphitization pretreatment device comprises:
the upper opening square container is provided with an inlet and an outlet on the side wall of the lower part, and is correspondingly provided with a switch door capable of sealing and closing the inlet and the outlet, and the bottom of the container is provided with a water inlet and drainage valve; the upper opening of the square container is a funnel inlet;
the four elastic coiled plates are alternately arranged on the inner walls of the left side and the right side of the upper part of the square container in a staggered manner, the elastic coiled plates are arc-shaped plates which are bent upwards, the chord length of each arc-shaped plate is greater than one half of the distance from the left side to the right side of the square container and less than two thirds of the distance from the left side to the right side of the square container, and the corresponding angle of each arc-shaped plate is greater than 100 degrees and less than 180 degrees; the staggered arrangement is that two left and right side walls of the upper part of the square container are respectively arranged, a first elastic coiled plate is arranged on the left side from top to bottom, a second elastic coiled plate is arranged on the right side 10-20cm lower than the first elastic coiled plate, a third elastic coiled plate is arranged on the left side 10-20cm lower than the second elastic coiled plate, a fourth elastic coiled plate is arranged on the right side 10-20cm lower than the third elastic coiled plate, a vibrator is fixed below each elastic coiled plate, and the vibrator is positioned between the middle part of the elastic coiled plate and a fixed point of the square container wall and is positioned between the front wall and the rear wall of the square container; the upper surface of the elastic coiled plate is provided with a circular bulge;
the net box with an upper opening is tightly and movably embedded at the lower part of the square container in an up-and-down moving way; naphtha immersed in the net cage is arranged at the lower part of the square container, the meshes on the side wall of the net cage are triangular meshes, the thickness of the bottom of the net cage is 0.5-2cm, and the meshes at the bottom are conical holes from bottom to top;
the telescopic rod is a telescopic magnetic rod, is arranged at the bottom of the square container, and is connected with the bottom of the net cage to push the net cage to move up and down in the square container; the bottom of the net cage is made of soft magnetic materials, so that the telescopic magnetic rod can fix the net cage through magnetic force in an electrified state and can push the net cage to move up and down in the square container.
2. The method of claim 1, wherein the air-blocking condition in the step is to vacuum the graphitization furnace.
3. The method of claim 2, wherein the filler is calcined coke particles.
4. The method for preparing the graphite anode as claimed in claim 3, wherein the specific operation of placing the defective product of the prebaked anode in the graphitization pretreatment device for pretreatment in the first step is as follows: the unqualified products of the prebaked anode are added into a graphitization pretreatment device from the upper opening of the square container, continuously rubbed and collided by four elastic coiled plates, then enter a net cage, continuously soaked and impacted in naphtha for 1-2 hours by the net cage to drive the unqualified products of the prebaked anode, then power is cut off for a telescopic rod, filtered naphtha is discharged, and then the material A is taken out from a side wall inlet and outlet of the square container.
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| CN112299406B (en) * | 2020-11-24 | 2021-09-17 | 烟台美尔森石墨有限公司 | Negative electrode material graphitization preparation process |
| CN112876249B (en) * | 2021-01-13 | 2022-07-08 | 山西沁新能源集团股份有限公司 | Method for preparing prebaked anode, prebaked anode and application thereof |
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| CN102146570A (en) * | 2011-02-26 | 2011-08-10 | 王建军 | Method for producing aluminum anode by using waste cathode carbon block of aluminum cell |
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