CN111362261B - Method for improving graphitization degree of electrode/joint - Google Patents
Method for improving graphitization degree of electrode/joint Download PDFInfo
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- CN111362261B CN111362261B CN202010271315.5A CN202010271315A CN111362261B CN 111362261 B CN111362261 B CN 111362261B CN 202010271315 A CN202010271315 A CN 202010271315A CN 111362261 B CN111362261 B CN 111362261B
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Abstract
The invention provides a method for improving graphitization degree of an electrode/joint, which comprises the following specific steps: (1) Dispersing nano-grade silicon powder into natural graphite powder at normal temperature to obtain powder; (2) kneading: sequentially adding aggregate petroleum coke, powder and ferric oxide powder, dry-mixing for 15-20 minutes, adding binder modified asphalt and stearic acid, and kneading for 40-45 minutes at 150-170 ℃; (3) roasting, forming and impregnating; (4) graphitization: the maximum temperature is 2200-2500 ℃. According to the invention, the nano-grade silicon powder is firstly dispersed into the natural graphite powder, so that the additive is uniformly dispersed into the electrode or joint body paste, the nano-grade silicon powder can improve the homogeneity of the paste due to volume expansion in the mixing process, and the nano-grade powder improves the volume density and the compressive strength of the product in the roasting process, so that the influence on the final target value of the product is eliminated. The graphitization degree of the invention is improved by 3-6%, the resistivity of the electrode/joint is reduced by 10-25%, the elastic modulus is controlled at 10-15Gpa, and the compressive strength is improved by 100-120%.
Description
Technical Field
The invention belongs to the technical field of graphite electrode/joint materials, and particularly relates to a method for improving graphitization degree of an electrode/joint.
Background
The graphite electrodes/joints are produced for long periods of time and consume large amounts of natural gas and electrical energy. At present, the graphitization degree is influenced by the highest graphitization temperature no matter the graphitization process is conducted by an Acheson furnace or an internal series graphitization furnace. But increasing the temperature to increase the degree of graphitization requires a significant amount of energy. At present, in order to solve the problem of improving the graphitization degree on the premise of not improving the graphitization temperature, an additive is adopted, so that the additive can improve the graphitization degree in the graphitization process, reduce the resistivity and control the elastic modulus range (the index of the graphite electrode requires low resistivity and moderate elastic modulus). However, in practical production, the elastic modulus is always increased continuously while the resistivity is reduced by means of additives, and a balance cannot be achieved. Meanwhile, silicon powder or boron powder cannot be added in the production of the conventional graphite electrode, and silicon powder generates silicon carbide whiskers due to high temperature, so that the resistivity and elastic modulus indexes are affected. In the roasting process, the discharging time is prolonged, the impregnating asphalt is added in an impregnating way, and meanwhile, the acid additive is added, so that the impregnating efficiency is improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for improving the graphitization degree of an electrode/joint aiming at the defects in the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the method for improving the graphitization degree of the electrode/joint comprises the following specific steps:
(1) Dispersing nano-grade silicon powder into natural graphite powder at normal temperature to obtain powder;
(2) Kneading: sequentially adding aggregate petroleum coke, powder and ferric oxide powder, dry-mixing for 15-20 minutes, adding binder modified asphalt and stearic acid, and kneading for 40-45 minutes at 150-170 ℃;
(3) Roasting, forming and soaking;
(4) Graphitizing: isolating air, wherein the highest temperature is 2200-2500 ℃;
wherein the weight portions of the materials are as follows: 1-3 parts of nanoscale silica powder, 10-20 parts of natural graphite powder, 30-40 parts of aggregate petroleum coke, 1-3 parts of ferric oxide powder, 20-30 parts of binder modified asphalt and 3-5 parts of stearic acid.
And (3) heating up the roasting furnace in the step (3) at a heating up rate of 1 ℃/h at 30-500 ℃, at a heating up rate of 2 ℃/h at 500-800 ℃, at a heating up rate of 3 ℃/h at 800-1000 ℃, at a heating up rate of 1000-1270 ℃, at a heating up rate of 4 ℃/h, maintaining for 40-45 hours at 1270 ℃, naturally cooling to normal temperature, and delaying discharging from the furnace for 48 hours.
The roasting furnace is a ring furnace with a cover or an open ring furnace.
The graphitization adopts an Acheson furnace or an inner series graphitization furnace, wherein the filler in the Acheson furnace is metallurgical coke and quartz sand, and the filler in the inner series graphitization furnace is metallurgical coke.
The invention overcomes the technical prejudice that no silicon powder is used in the current electrode, and the additive is uniformly dispersed into the electrode or joint body paste by dispersing the nano silicon powder into the natural graphite powder, so that the nano silicon powder can improve the paste homogeneity due to volume expansion in the mixing and kneading process, and meanwhile, the nano powder improves the volume density and compressive strength of the product in the roasting process, and eliminates the influence on the final target value of the product. And through the graphitization process, the carbon elements in the catalytic electrode are orderly layered, so that the graphitization degree of the electrode is improved, the resistivity and the elastic modulus of the electrode are reduced, and the toughness of the electrode is improved when the graphitization temperature is lower than the conventional graphitization temperature. Meanwhile, when graphitization is completed, the silicon carbide whisker can not be formed by volatilizing under the action of high temperature and can not be formed in the product, the resistivity and elastic modulus index of the product can not be changed by the silicon carbide whisker, and meanwhile, the composition and quality of molten steel can not be influenced when the product is used in a steelmaking electric furnace. The graphitization degree of the invention is improved by 3-6%, the resistivity of the electrode/joint is reduced by 10-25%, the elastic modulus is controlled at 10-15Gpa, and the compressive strength is improved by 100-120%.
Detailed Description
The technical scheme of the present invention will be further described with reference to specific embodiments, but the present invention is not limited to these embodiments.
Example 1
The method for improving the graphitization degree of the electrode/joint comprises the following specific steps:
(1) Dispersing nano-grade silicon powder into natural graphite powder at normal temperature to obtain powder;
(2) Kneading, namely sequentially adding aggregate petroleum coke, powder and ferric oxide powder, dry-mixing for 15 minutes, adding binder modified asphalt and stearic acid, and kneading for 45 minutes at 150 ℃; wherein the weight portions of the materials are as follows: 1 part of nanoscale silicon powder, 10 parts of natural graphite powder, 30 parts of aggregate petroleum coke, 1 part of ferric oxide powder, 20 parts of binder modified asphalt and 3 parts of stearic acid;
(3) Roasting and molding in an open ring furnace, and then soaking; wherein the temperature rise curve of the roasting furnace is that the temperature rise rate of 30-500 ℃ is 1 ℃/h, the temperature rise rate of 500-800 ℃ is 2 ℃/h, the temperature rise rate of 800-1000 ℃ is 3 ℃/h, the temperature rise rate of 1000-1270 ℃ is 4 ℃/h, the temperature is kept for 40 hours at 1270 ℃, the temperature is naturally reduced to normal temperature, and the temperature is delayed for 48 hours to be discharged;
(4) Graphitizing: isolating air, and graphitizing by using an Acheson graphitizing furnace, wherein the filler of the Acheson graphitizing furnace is metallurgical coke and quartz sand, and the highest temperature is 2200 ℃;
wherein: 3 parts of nanoscale silica powder or boron powder, 10 parts of natural graphite powder, 40 parts of aggregate petroleum coke, 3 parts of ferric oxide powder, 20 parts of binder modified asphalt and 5 parts of stearic acid.
The graphitization degree of the embodiment is improved by 6%, the resistivity of the electrode/joint is reduced by 25%, the elastic modulus is controlled at 15Gpa, and the compressive strength is improved by 100%.
Example 2
The method for improving the graphitization degree of the electrode/joint comprises the following specific steps:
(1) Dispersing nano-grade silicon powder into natural graphite powder at normal temperature to obtain powder;
(2) Kneading, namely sequentially adding aggregate petroleum coke, powder and ferric oxide powder, dry-mixing for 20 minutes, adding binder modified asphalt and stearic acid, and kneading for 40 minutes at 170 ℃; wherein the weight portions of the materials are as follows: 3 parts of nanoscale silicon powder, 20 parts of natural graphite powder, 40 parts of aggregate petroleum coke, 3 parts of ferric oxide powder, 30 parts of binder modified asphalt and 5 parts of stearic acid;
(3) Roasting and molding the mixture in a ring furnace with a cover, and then soaking the mixture; wherein the temperature rise curve of the roasting furnace is that the temperature rise rate of 30-500 ℃ is 1 ℃/h, the temperature rise rate of 500-800 ℃ is 2 ℃/h, the temperature rise rate of 800-1000 ℃ is 3 ℃/h, the temperature rise rate of 1000-1270 ℃ is 4 ℃/h, the temperature is kept for 45 hours at 1270 ℃, the temperature is naturally reduced to normal temperature, and the temperature is delayed for 48 hours to be discharged.
(4) Graphitizing: isolating air, graphitizing by using an Acheson graphitizing furnace, wherein the filler of the graphitizing furnace in the inner string is metallurgical coke, and the highest temperature is 2500 ℃;
wherein: 1 part of nanoscale silica powder or boron powder, 20 parts of natural graphite powder, 30 parts of aggregate petroleum coke, 1 part of ferric oxide powder, 30 parts of binder modified asphalt and 3 parts of stearic acid.
The graphitization degree of the embodiment is improved by 3%, the resistivity of the electrode/joint is reduced by 10%, the elastic modulus is controlled at 10Gpa, and the compressive strength is improved by 120%.
Claims (1)
1. The method for improving the graphitization degree of the electrode/joint is characterized by comprising the following specific steps of:
(1) Dispersing nano-grade silicon powder into natural graphite powder at normal temperature to obtain powder;
(2) Kneading: sequentially adding aggregate petroleum coke, powder and ferric oxide powder, dry-mixing for 15-20 minutes, adding binder modified asphalt and stearic acid, and kneading for 40-45 minutes at 150-170 ℃;
(3) Roasting, forming and soaking;
(4) Graphitizing: isolating air, wherein the highest temperature is 2200-2500 ℃;
wherein the weight portions of the materials are as follows: 1-3 parts of nanoscale silica powder, 10-20 parts of natural graphite powder, 30-40 parts of aggregate petroleum coke, 1-3 parts of ferric oxide powder, 20-30 parts of binder modified asphalt and 3-5 parts of stearic acid;
the temperature rising curve of the roasting furnace in the step (3) is that the temperature rising rate is 1 ℃/h at 30-500 ℃, the temperature rising rate is 2 ℃/h at 500-800 ℃, the temperature rising rate is 3 ℃/h, the temperature rising rate is 1000-1270 ℃, the temperature rising rate is 4 ℃/h, the temperature is kept for 40-45 hours at 1270 ℃, the temperature is naturally reduced to normal temperature, and the temperature is delayed for 48 hours to be discharged from the furnace;
the roasting furnace is a ring furnace with a cover or an open ring furnace;
the graphitization adopts an Acheson furnace or an inner series graphitization furnace, wherein the filler in the Acheson furnace is metallurgical coke and quartz sand, and the filler in the inner series graphitization furnace is metallurgical coke.
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| US3171720A (en) * | 1961-06-23 | 1965-03-02 | Great Lakes Carbon Corp | Carbonaceous bodies useful for thermal insulation and processes for preparing same |
| CN101980583B (en) * | 2010-11-03 | 2012-04-04 | 天津锦美碳材科技发展有限公司 | Method for preparing graphite electrode of quartz crucible |
| CN102158999B (en) * | 2011-05-16 | 2013-03-13 | 方大炭素新材料科技股份有限公司 | Phi 800mm general power graphite electrode and production method thereof |
| CN105350019B (en) * | 2015-12-08 | 2019-04-30 | 贵州师范大学 | A kind of microdilatancy lower shrinkage carbon paste used for aluminium electrolysis of silicon-containing additive and preparation method thereof |
| CN109665845A (en) * | 2019-02-12 | 2019-04-23 | 合肥炭素有限责任公司 | A kind of preparation method of composite graphite electrode |
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| Title |
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| 姜玉敬等.石墨化的基础理论.《现代铝用炭素材料制造技术与产业研究》.冶金工业出版社,2020,第253页. * |
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