CN116083960A - Graphitized cathode carbon block for aluminum electrolysis and preparation method thereof - Google Patents
Graphitized cathode carbon block for aluminum electrolysis and preparation method thereof Download PDFInfo
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- 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
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Abstract
The application discloses a graphitized cathode carbon block for aluminum electrolysis and a preparation method thereof, wherein raw materials are weighed according to the mass portion ratio, the electric forging anthracite is 15-45 portions, and the grain diameter is less than or equal to 6mm; 40-60 parts of petroleum coke after forging, and the grain diameter is less than or equal to 6mm; 15-20 parts of modified asphalt serving as a binder, wherein the dry mixing time is 5-10min, the temperature is 130-150 ℃, the wet mixing time is 60-80min, and the temperature is 180-200 ℃; crushing graphite into 10-15 parts with particle size less than or equal to 2mm; 5-10 parts of NbN additive and H 3 BO 3 5-10 parts of additives which are all chemically pure. The preparation method comprises the steps of crushing, screening, material mixing, kneading, forming, roasting, dipping, secondary roasting and processing. The application adds NbN and H 3 BO 3 Obviously reduces the resistivity of the cathode carbon block, improves the corrosion resistance and the compressive strength of the cathode carbon block, and improves the cathode carbon to a great extentThe lifetime of the block.
Description
Technical Field
The invention belongs to the technical field of aluminum electrolysis, and particularly relates to a graphitized cathode carbon block for aluminum electrolysis and a preparation method thereof.
Background
As one of the main methods for producing aluminum, an aluminum electrolysis method is one in which a strong current is applied to a cathode and an anode in an aluminum electrolysis cell, and the electrolysis is performed at a high temperature of about 950 ℃. The main cathode materials at present are common cathode carbon blocks, semi-graphite cathode carbon blocks and full-graphite cathode carbon blocks.
With the development of the aluminum electrolysis cell towards the high current density, high current intensity and large-scale in recent years, the development of the cathode carbon block caters to the development of the aluminum electrolysis cell, and the development of the cathode carbon block mainly comprises the continuous improvement of electric conductivity, thermal shock resistance, sodium erosion resistance, wear resistance, volume density, true density and compressive strength, and meanwhile, the aluminum electrolysis cell design requirement is gradually met in the aspect of specification and size. The cathode carbon block as the aluminum electrolysis cell conductor and substrate material should have good conductivity and high corrosion resistance to the electrolyte. However, the traditional cathode carbon block has higher resistivity and extremely large pressure drop, and increases the reaction energy consumption. In addition, the conventional cathode carbon block has low mechanical strength and poor resistance to attack by electrolyte solution. Typically these cathode carbon blocks have a relatively short life, and the life of the cell is typically dependent on the cathode block. The average life of large pre-baked cells is short, from 1300 days to 1500 days, even less than 1000 days. Therefore, in order to solve the above problems, it is important in the current research to change the preparation process and formulation of graphitized cathode carbon blocks, improve the thermal stability and chemical stability thereof, and make them have higher conductivity and superconductivity.
The invention aims to add metal ions and novel auxiliary agents in the preparation process, enhance the conductivity and corrosion resistance of the graphitized cathode carbon block and prolong the whole service life of the cathode carbon block. This is the main object of the present invention.
Disclosure of Invention
The technical problems to be solved are as follows:
aiming at the defects of the prior art, the application provides a graphitized cathode carbon block for aluminum electrolysis and a preparation method thereof, which solve the problems of higher resistivity, poorer corrosion resistance, shorter overall service life of the cathode carbon block and the like existing at present.
The technical scheme is as follows:
in order to achieve the above purpose, the present application is implemented by the following technical schemes:
the graphitized cathode carbon block for aluminum electrolysis consists of the following raw materials in parts by weight: 15-45 parts of electric forging anthracite; 40-60 parts of petroleum coke after forging; 15-20 parts of modified asphalt; crushing 10-15 parts of graphite; 5-10 parts of NbN additive; h 3 BO 3 0-10 parts of additive.
Preferably, the granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm.
Preferably, the electric forging anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃.
Preferably, the modified asphalt is a modified asphalt β -resin.
Preferably, the NbN additive and H 3 BO 3 The additives are all chemically pure.
The application also discloses a preparation method of the graphitized cathode carbon block for aluminum electrolysis, which comprises the following steps:
s1: crushing the electric forging anthracite and the petroleum coke after forging;
s2: screening crushed electric forging anthracite and forged petroleum coke to below 6mm;
s3: according to the mass portion ratio, the electric forging anthracite, the petroleum coke after forging, nbN additive and H 3 BO 3 The additive is put into a kneading pot;
s4: dry-mixing at 130-150deg.C for 5-10min at rotation speed of 30 r/min;
s5: heating the kneading pot to 180 ℃, adding 80% modified asphalt, and wet mixing at the rotating speed of 30r/min and the temperature of 180-200 ℃ for 60-80min;
s6: placing the wet mixed sample into a vibration molding machine for molding, wherein the molding specification is phi 60mm multiplied by 120mm;
s7: roasting the molded sample, wherein the primary roasting temperature is 1000-1200 ℃, the roasting time is 12 hours, then, 20% modified asphalt is used for high-pressure impregnation, the secondary roasting temperature is 1800-1900 ℃, and the roasting time is 10 hours;
s8: and (3) forming the roasted sample by a vibration forming machine, wherein the specification is phi 30mm multiplied by 40mm, and obtaining a finished product.
Preferably, the high-pressure impregnation pressure is 1.5-1.8MPa, and the dwell time is 6h.
The principle of the invention:
adding organic adhesive H into cathode carbon block 3 BO 3 The method can improve the tightness of the internal connection of the carbon blocks, greatly increase the mechanical strength of the carbon blocks, strengthen the corrosion resistance of the cathode carbon blocks to sodium ions in electrolyte solution, and remarkably improve the service life of the cathode carbon blocks. NbN, which is a metal-type nitride formed by direct combination of a transition element and nitrogen, is added to the cathode carbon block. Nitrogen atoms occupy vacancies in the metal lattice and are typical B-1 compounds. The compound is generally high in hardness, high in melting point, stable in chemical property and conductive. The NbN is added into the cathode carbon block, so that the thermal stability and chemical stability of the cathode carbon block are remarkably improved, and the cathode carbon block has higher conductivity and superconductivity.
The beneficial effects are that:
the application provides a graphitized cathode carbon block for aluminum electrolysis and a preparation method thereof, and the graphitized cathode carbon block has the following beneficial effects:
1. provides a high-conductivity graphitized cathode carbon block material and application thereof. NbN is added into the cathode carbon block for the first time, so that the carbon block has excellent conductivity, the voltage drop of the cathode is reduced, and the power consumption is greatly reduced.
2. The addition of the metal Nb obviously improves the mechanical strength and corrosion resistance of the cathode carbon block, improves the wear resistance of the cathode carbon block and reduces the erosion effect of the aluminum electrolyte on the cathode carbon block.
3. Using H 3 BO 3 As an additive, the catalytic material is graphitized, so that the compactness, conductivity and strength of the material are improved.
4. The resistivity of the material can reach below 3 mu omega/m, compared with the resistivity of the current cathode carbon block of about 30 mu omega/m, the material can be obviously reduced, the highest compressive strength can reach 35MPa, and the material is improved compared with the current state of the art.
Description of the drawings:
FIG. 1 is an electron microscopic view of graphitized cathode carbon blocks for aluminum electrolysis according to example 3 of the present application;
FIG. 2 is an electron microscopic view of graphitized cathode carbon blocks for aluminum electrolysis according to example 4 of the present application;
FIG. 3 is an electron micrograph of a high conductivity graphitized cathode carbon block of comparative example 1 of the present application;
fig. 4 is an electron micrograph of a high conductivity graphitized cathode carbon block of comparative example 2 of the present application.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
the graphitized cathode carbon block for aluminum electrolysis consists of the following raw materials in parts by weight: 25 parts of electric forging anthracite; 45 parts of petroleum coke after forging; 15 parts of modified asphalt; crushing 10 parts of graphite; 5 parts of NbN additive, wherein the granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm; the forged anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the forged petroleum coke is obtained by calcining petroleum coke in a high-temperature graphitization furnace at 2000 ℃, so that the resistivity of the petroleum coke is reduced, and the density and strength of the petroleum coke are increased; the modified asphalt is modified asphalt beta-resin which is used as a binder to tightly adhere the components together; the NbN additive is chemically pure.
The application also discloses a preparation method of the graphitized cathode carbon block for aluminum electrolysis, which comprises the following steps:
s1: crushing the electric forging anthracite and the petroleum coke after forging;
s2: screening crushed electric forging anthracite and forged petroleum coke to below 6mm;
s3: according to the mass portion ratio, the electric forging anthracite, the petroleum coke after forging and the NbN additive are put into a kneading pot;
s4: dry-mixing at 130-150deg.C for 5-10min at rotation speed of 30 r/min;
s5: heating the kneading pot to 180 ℃, adding 80% modified asphalt, and wet-mixing at 180-200 ℃ for 60-80min at the rotating speed of 30 r/min;
s6: putting the kneaded sample into a vibration molding machine for molding, wherein the molding specification is phi 60mm multiplied by 120mm;
s7: roasting the molded sample, wherein the primary roasting temperature is 1000-1200 ℃, the roasting time is 12 hours, then, 20% modified asphalt is used for high-pressure impregnation, the secondary roasting temperature is 1800-1900 ℃, and the roasting time is 10 hours;
s8: and (3) forming the roasted sample by a vibration forming machine, wherein the specification is phi 30mm multiplied by 40mm, and obtaining a finished product.
The high-pressure impregnation pressure is 1.5-1.8MPa, and the dwell time is 6h.
Example 2:
the graphitized cathode carbon block for aluminum electrolysis consists of the following raw materials in parts by weight: 20 parts of electric forging anthracite; 40 parts of petroleum coke after forging; 15 parts of modified asphalt; crushing 10 parts of graphite; 10 parts of NbN additive, wherein the granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm; the forged anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃; the modified asphalt is modified asphalt beta-resin which is used as a binder to tightly adhere the components together; the NbN additive is chemically pure. The specific preparation procedure is the same as in example 1.
Example 3:
a graphitized cathode carbon block for aluminum electrolysis is prepared from the following raw materials in parts by weightThe material composition comprises: 15 parts of electric forging anthracite; 50 parts of petroleum coke after forging; 15 parts of modified asphalt; crushing 10 parts of graphite; nbN additive 5 parts, H 3 BO 3 10% of additive, and the granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm; the forged anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃; the modified asphalt is modified asphalt beta-resin which is used as a binder to tightly adhere the components together; nbN additive and H 3 BO 3 The additives are all chemically pure.
The preparation method of the graphitized cathode carbon block for aluminum electrolysis comprises the following steps:
s1: crushing the electric forging anthracite and the petroleum coke after forging;
s2: screening crushed electric forging anthracite and forged petroleum coke to below 6mm;
s3: according to the mass portion ratio, the electric forging anthracite, the petroleum coke after forging, nbN additive and H 3 BO 3 The additive is put into a kneading pot;
s4: dry-mixing at 130-150deg.C for 5-10min at rotation speed of 30 r/min;
s5: heating the kneading pot to 180 ℃, adding 80% modified asphalt, and wet-mixing at 180-200 ℃ for 60-80min at the rotating speed of 30 r/min;
s6: placing the wet mixed sample into a vibration molding machine for molding, wherein the molding specification is phi 60mm multiplied by 120mm;
s7: roasting the molded sample, wherein the primary roasting temperature is 1000-1200 ℃, the roasting time is 12 hours, then, 20% modified asphalt is used for high-pressure impregnation, the secondary roasting temperature is 1800-1900 ℃, and the roasting time is 10 hours;
s8: and (3) forming the roasted sample by a vibration forming machine, wherein the specification is phi 30mm multiplied by 40mm, and obtaining a finished product.
The high-pressure impregnation pressure is 1.5-1.8MPa, and the dwell time is 6h.
Example 4:
the graphitized cathode carbon block for aluminum electrolysis consists of the following raw materials in parts by weight: 15 parts of electric forging anthracite; petroleum coke after forging50 parts; 15 parts of modified asphalt; crushing 10 parts of graphite; nbN additive 5 parts, H 3 BO 3 5% of additive, and the granularity of the electric forging anthracite and the forged petroleum coke is less than or equal to 6mm; the forged anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃; the modified asphalt is modified asphalt beta-resin which is used as a binder to tightly adhere the components together; nbN additive and H 3 BO 3 The additives are all chemically pure. The specific preparation procedure is the same as in example 3.
Example 5:
the graphitized cathode carbon block for aluminum electrolysis consists of the following raw materials in parts by weight: 15 parts of electric forging anthracite; 45 parts of petroleum coke after forging; 15 parts of modified asphalt; crushing 10 parts of graphite; nbN additive 5 parts, H 3 BO 3 10% of additive, and the granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm; the forged anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃; the modified asphalt is modified asphalt beta-resin which is used as a binder to tightly adhere the components together; nbN additive and H 3 BO 3 The additives are all chemically pure. The specific preparation procedure is the same as in example 3.
Example 6:
the graphitized cathode carbon block for aluminum electrolysis consists of the following raw materials in parts by weight: 15 parts of electric forging anthracite; 40 parts of petroleum coke after forging; 15 parts of modified asphalt; 15 parts of graphite particles; 10 parts of NbN additive, H 3 BO 3 5% of additive, and the granularity of the electric forging anthracite and the forged petroleum coke is less than or equal to 6mm; the forged anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃; the modified asphalt is modified asphalt beta-resin which is used as a binder to tightly adhere the components together; nbN additive and H 3 BO 3 The additives are all chemically pure. The specific preparation procedure is the same as in example 3.
Comparative example 1
The high-conductivity graphitized cathode carbon block consists of the following raw materials in parts by weight: 15 parts of electric forging anthracite, 60 parts of petroleum coke after forging, 15 parts of modified asphalt and 10 parts of crushed graphite.
The application also discloses a preparation method of the high-conductivity graphitized cathode carbon block, which comprises the following steps:
s1: crushing the electric forging anthracite and the petroleum coke after forging;
s2: screening crushed electric forging anthracite and forged petroleum coke to below 6mm;
s3: according to the mass portion ratio, the electric forging anthracite, the petroleum coke after forging and the graphite are crushed and put into a kneading pot;
s4: dry-mixing at 130-150deg.C for 5-10min at rotation speed of 30 r/min;
s5: heating the kneading pot to 180 ℃, adding 80% modified asphalt, and wet-mixing at 180-200 ℃ for 60-80min at the rotating speed of 30 r/min;
s6: putting the kneaded sample into a vibration molding machine for molding, wherein the molding specification is phi 80mm multiplied by 120mm;
s7: roasting the molded sample, wherein the primary roasting temperature is 1000-1200 ℃, the roasting time is 12 hours, then, 20% modified asphalt is used for high-pressure impregnation, the secondary roasting temperature is 1800-1900 ℃, and the roasting time is 10 hours;
s8: and (3) machining the roasted sample, wherein the specification is phi 30mm multiplied by 40mm, and a finished product is obtained.
Preferably, the high-pressure impregnation pressure is 1.5-1.8MPa, and the dwell time is 6h.
Comparative example 2
The high-conductivity graphitized cathode carbon block consists of the following raw materials in parts by weight: 35% of electric forging anthracite, 40% of petroleum coke after forging, 15% of modified asphalt and 10% of graphite crushed. The granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm; the electric forging anthracite is obtained by calcining at 1300-1800 ℃ in a high-temperature graphitization furnace, and the petroleum coke after forging is obtained by calcining at 2000 ℃ in the high-temperature graphitization furnace; the modified asphalt is modified asphalt beta-resin. The specific procedure was as in comparative example 1.
Comparison table of physicochemical property indexes and other similar products
As can be seen from FIGS. 1-4, nbN and H are added 3 BO 3 The surface structure of the cathode carbon block is compact, which shows that the compressive strength is improved. As can be seen from the table, the graphitized cathode carbon blocks for aluminum electrolysis prepared in examples 1 to 6 have higher compressive strength and lower resistivity than the comparative examples. The prepared cathode carbon block solves the problems of higher resistivity and poorer conductivity of the cathode carbon block of the aluminum electrolysis cell in the current industrial application. The electrolyte erosion resistance of the cathode carbon block is improved, and the industrial service life of the cathode carbon block is greatly prolonged. In addition, the preparation method can effectively solve the problem of high-temperature graphitization energy consumption in the manufacturing process, and has great economic benefit.
While the invention has been described in detail with reference to the foregoing embodiments, the implementation of the invention is not limited to the foregoing embodiments, but rather, it should be understood that those skilled in the art, based on the teachings herein, should make improvements, substitutions and modifications without departing from the spirit and scope of the invention.
Claims (7)
1. The graphitized cathode carbon block for aluminum electrolysis is characterized by comprising the following raw materials in parts by weight: 15-45 parts of electric forging anthracite; 40-60 parts of petroleum coke after forging; 15-20 parts of modified asphalt; crushing 10-15 parts of graphite; 5-10 parts of NbN additive; h 3 BO 3 0-10 parts of additive.
2. The graphitized cathode carbon block for aluminum electrolysis according to claim 1, wherein: the granularity of the electric forging anthracite and the petroleum coke after forging is less than or equal to 6mm.
3. The graphitized cathode carbon block for aluminum electrolysis according to claim 1, wherein: the electric forging anthracite is obtained by calcining anthracite in a high-temperature graphitization furnace at 1300-1800 ℃, and the petroleum coke after forging is obtained by calcining petroleum coke in the high-temperature graphitization furnace at 2000 ℃.
4. The graphitized cathode carbon block for aluminum electrolysis according to claim 1, wherein: the modified asphalt is modified asphalt beta-resin.
5. The graphitized cathode carbon block for aluminum electrolysis according to claim 1, wherein: the NbN additive and H 3 BO 3 The additives are all chemically pure.
6. A method for preparing graphitized cathode carbon blocks for aluminum electrolysis according to any one of claims 1 to 5, characterized in that the method comprises the following steps:
s1: crushing the electric forging anthracite and the petroleum coke after forging;
s2: screening crushed electric forging anthracite and forged petroleum coke to below 6mm;
s3: according to the mass portion ratio, the electric forging anthracite, the petroleum coke after forging, nbN additive and H 3 BO 3 The additive is put into a kneading pot;
s4: dry-mixing at 130-150deg.C for 5-10min at rotation speed of 30 r/min;
s5: heating the kneading pot to 180 ℃, adding 80% modified asphalt, and wet-mixing at 180-200 ℃ for 60-80min at the rotating speed of 30 r/min;
s6: placing the wet mixed sample into a vibration molding machine for molding, wherein the molding specification is phi 60mm multiplied by 120mm;
s7: roasting the molded sample, wherein the primary roasting temperature is 1000-1200 ℃, the roasting time is 12 hours, then, 20% modified asphalt is used for high-pressure impregnation, the secondary roasting temperature is 1800-1900 ℃, and the roasting time is 10 hours;
s8: and (3) forming the roasted sample by a vibration forming machine, wherein the specification is phi 30mm multiplied by 40mm, and obtaining a finished product.
7. The method for preparing graphitized cathode carbon blocks for aluminum electrolysis according to claim 6, wherein: the high-pressure impregnation pressure is 1.5-1.8MPa, and the dwell time is 6h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949034A (en) * | 2010-09-30 | 2011-01-19 | 广西强强碳素股份有限公司 | Cathode graphitizing current stop block for aluminum electrolysis |
| US20130004410A1 (en) * | 2010-01-19 | 2013-01-03 | Elkem Carbon As | Method for the production of graphite bodies |
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- 2022-12-16 CN CN202211623972.7A patent/CN116083960A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130004410A1 (en) * | 2010-01-19 | 2013-01-03 | Elkem Carbon As | Method for the production of graphite bodies |
| CN101949034A (en) * | 2010-09-30 | 2011-01-19 | 广西强强碳素股份有限公司 | Cathode graphitizing current stop block for aluminum electrolysis |
Non-Patent Citations (1)
| Title |
|---|
| 中国冶金百科全书总编辑委员会《有色金属冶金》卷编辑委员会等: "《中国冶金百科全书 有色金属冶金》", 中国矿业大学出版社, pages: 225 - 226 * |
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