CN115198314A - Preparation method of pre-baked anode carbon block trace element for dilutable aluminum electrolysis - Google Patents
Preparation method of pre-baked anode carbon block trace element for dilutable aluminum electrolysis Download PDFInfo
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- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
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Abstract
The invention discloses a preparation method of dilutable prebaked anode carbon block trace elements for aluminum electrolysis, which comprises the following steps: (1) Kneading the calcined coke, asphalt and additive to obtain a green body; (2) Placing the green body in a roasting furnace, cooling the roasted anode and discharging to obtain a prebaked anode; the calcined petroleum coke raw material is screened, and the weight percentage of each grade material in the screened calcined coke is as follows: 9-13% of 5-8mm particle size, 16-25% of 3-5mm particle size, 30-38% of 0.074-3mm particle size and 32-40% of ball milled powder with particle size below 0.074 mm; the additive comprises: graphite powder, rare earth, modified kaolin and clay; the mass ratio of the calcined coke, the asphalt and the additive is 100:40-55:1-10. According to the method, the additive is added into the raw materials, the raw material formula of the prebaked anode is optimized, the contents of trace elements in the prebaked anode carbon block can be diluted through the interaction among the raw materials and the optimized baking process, and the prebaked anode with excellent performance is obtained.
Description
Technical Field
The invention relates to the technical field of aluminum electrolysis, in particular to a preparation method of dilutable trace elements of a prebaked anode carbon block for aluminum electrolysis.
Background
The prebaked anode plays an important role in the production process of the aluminum electrolysis cell, is used as a conductor to guide direct current into the electrolysis cell, and is used as an anode material of the electrolysis cell to participate in the anode reaction process, and the quality and the working condition of the prebaked anode have great relevance to the normality of the aluminum electrolysis production and economic and technical indexes such as current efficiency, electric energy consumption, primary aluminum grade and the like, particularly the resistivity index is an important index for judging whether the anode is high-quality or not.
Previous control of raw materials in the aluminum electrolysis industry was limited to ash, volatiles, true specific gravity and electricityResistivity. However, more and more studies now show that the properties of the raw materials have a great influence on the properties of the baked anode, such as resistance, strength, CO 2 Reactivity, air reactivity, and the like are related to the raw materials. The main raw materials of the prebaked anode for producing the electrolytic aluminum are petroleum coke, coal tar and other raw materials. Although the raw materials contain less trace elements, if the content exceeds a certain range, the use performance of the anode in the electrolytic cell is greatly influenced, the electrolytic efficiency is reduced, the carbon consumption is increased, and the electrolytic production and the cost control are seriously influenced.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon block microelement of a prebaked anode for diluting aluminum electrolysis, thereby overcoming the defects of high microelement content in the prebaked anode and low quality of the prebaked anode.
In order to realize the purpose, the invention provides a preparation method of dilutable trace elements of a prebaked anode carbon block for aluminum electrolysis, which comprises the following steps:
(1) Kneading the calcined coke, asphalt and additive to obtain a kneaded material green body;
(2) Placing the green body in a roasting furnace, heating the roasting furnace to 350-400 ℃ at a heating rate of 12-16 ℃/h, heating the roasting furnace to 600-700 ℃ at a heating rate of 6-8 ℃/h, preserving heat for 2-4h, heating the roasting furnace to 1000-1100 ℃ at a heating rate of 6-8 ℃/h, preserving heat for 45-55h, heating the roasting furnace to 1200-1300 ℃ at a heating rate of 12-16 ℃, preserving heat for 20-30h, cooling the roasted anode, and discharging to obtain a prebaked anode;
the calcined petroleum coke raw material is screened, and the weight percentage of each grade material in the screened calcined coke is as follows: 9-13% of 5-8mm, 16-25% of 3-5mm, 30-38% of 0.074-3mm and 32-40% of ball milled powder with particle size below 0.074 mm;
the additive comprises: graphite powder, rare earth, modified kaolin and clay;
the mass ratio of the calcined coke, the asphalt and the additive is 100:40-55:1-10.
Preferably, in the above technical scheme, the mass ratio of the graphite powder, the rare earth, the modified kaolin and the clay in the additive is 20-30.
Preferably, in the technical scheme, the asphalt is modified asphalt, the modified asphalt has a softening point of 105-110 ℃, the mass content of toluene insoluble substances is 29-32wt%, the mass content of quinoline insoluble substances is 10-11wt%, the mass content of beta-resin is 19.7-21.3wt%, and the coking value is 55-57wt%.
Preferably, in the above technical solution, the rare earth mainly consists of the following elements: samarium, neodymium, yttrium, lanthanum, cerium, and thulium.
Preferably, in the above technical scheme, each element in the rare earth mainly comprises the following raw materials in parts by weight: 10-30% of samarium, 10-30% of neodymium, 10-30% of yttrium, 10-30% of lanthanum, 10-30% of cerium and 10-30% of thulium.
Preferably, in the above technical solution, the clay is: calcining at 700-900 deg.C for 5-10h, and crushing and grinding to obtain clay powder.
Preferably, in the above technical solution, the preparation method of the modified kaolin comprises: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 9-10, filtering and drying, adding water for dissolving, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, uniformly stirring for reacting for a period of time, dehydrating, calcining for 3-10h at the temperature of 500-700 ℃, crushing and grinding to obtain the modified kaolin powder.
Preferably, in the above technical scheme, the total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide in the mixture accounts for 1-5% of the mass of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1-5.
Preferably, in the technical scheme, the kneading in the step (1) is to stir the calcined coke, the asphalt and the additive for 1-3 hours at the temperature of 150-165 ℃, and then to place the mixture in a mould for vibration molding.
Preferably, in the technical scheme, in the step (2), the green body is placed in a roasting furnace, the roasting furnace is heated to 350-380 ℃ at the heating rate of 14-15 ℃/h, the temperature in the roasting furnace is raised to 650-700 ℃ at the heating rate of 6-8 ℃/h, the temperature is kept for 3-4h, the temperature in the roasting furnace is raised to 1050-1100 ℃ at the heating rate of 6-8 ℃/h, the temperature is kept for 50-55h, the temperature in the roasting furnace is raised to 1250-1300 ℃ at the heating rate of 14-15 ℃, the temperature is kept for 24-28h, and the roasted anode is cooled and taken out of the furnace to obtain the prebaked anode.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method of the invention can dilute trace elements of the prebaked anode carbon block for aluminum electrolysis, optimizes the raw material formula of the prebaked anode by adding additives in the raw materials, and can reduce the trace element content of the prebaked anode carbon block by the interaction among the raw materials and the optimized roasting process, thereby obtaining the prebaked anode with excellent performance.
(2) The prebaked anode prepared by the method has the function of CO pairing 2 Low reactivity to air; good thermal shock resistance, no crack, fracture, slag falling and block falling caused by thermal shock; has good conductive performance. Can effectively control the trace elements in the prebaked anode, improve the performance of the prebaked anode, meet the quality requirement of a large-scale prebaked aluminum electrolytic cell on the carbon anode and reduce the consumption of the prebaked anode in the aluminum electrolysis process. Has the advantages of low air permeability and the like.
Detailed Description
The following detailed description of the present invention will be given with reference to specific examples, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Example 1
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes such steps as preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 11% of the powder with the grain diameter of 5-8mm, 21% of the powder with the grain diameter of 3-5mm, 32% of the powder with the grain diameter of 0.074-3mm and 36% of the ball milling powder with the grain diameter of less than 0.074 mm.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 30wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 20.7wt% and a coking value of 56.1wt%.
The mass ratio of the graphite powder, the rare earth, the modified kaolin and the clay in the additive is 23.
The clay is as follows: calcining for 7 hours at the temperature of 800 ℃, and then crushing and grinding to obtain clay powder.
The rare earth mainly comprises the following raw materials in parts by weight: samarium 20%, neodymium 15%, yttrium 22%, lanthanum 18%, cerium 12% and thulium 13%.
The preparation method of the modified kaolin comprises the following steps: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 9.5, filtering and drying, adding water for dissolving, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, stirring uniformly for reacting for 3 hours, dehydrating, calcining for 6 hours at the temperature of 650 ℃, crushing and grinding to obtain the modified kaolin powder.
The total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide in mixing accounts for 3% of the mass of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
(3) Production of a Green body
Stirring the calcined coke, the asphalt and the additive for 2 hours at 160 ℃, and then placing the mixture in a mould for vibration molding.
(4) Roasting
Placing the green body in a roasting furnace, heating the roasting furnace to 380 ℃ at a heating rate of 14 ℃/h, heating the roasting furnace to 650 ℃ at a heating rate of 7 ℃/h, preserving heat for 3h, heating the roasting furnace to 1050 ℃ at a heating rate of 8 ℃/h, preserving heat for 50h, heating the roasting furnace to 1250 ℃ at a heating rate of 13 ℃, preserving heat for 25h, cooling the roasted anode, and discharging to obtain the prebaked anode.
Example 2
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes such steps as preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 13% of powder with particle size of 5-8mm, 16% of powder with particle size of 3-5mm, 38% of powder with particle size of 0.074-3mm, and 33% of ball mill powder with particle size below 0.074 mm.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 29wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 21.3wt% and a coking value of 57wt%.
The mass ratio of the graphite powder, the rare earth, the modified kaolin and the clay in the additive is 30.
The clay is as follows: calcining for 10 hours at the temperature of 700 ℃, and then crushing and grinding to obtain clay powder.
The rare earth mainly comprises the following raw materials in parts by weight: 10% of samarium, 20% of neodymium, 10% of yttrium, 12% of lanthanum, 30% of cerium and 18% of thulium.
The preparation method of the modified kaolin comprises the following steps: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 9, filtering and drying, adding water for dissolving, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, stirring uniformly for reacting for 2 hours, dehydrating, calcining for 3 hours at the temperature of 700 ℃, crushing and grinding to obtain the modified kaolin powder.
The total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide in the mixture accounts for 1% of the mass of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
(3) Production of a Green body
Stirring the calcined coke, the asphalt and the additive for 1h at 165 ℃, and then placing the mixture in a mould for vibration molding.
(4) Roasting
Placing the green body in a roasting furnace, heating the roasting furnace to 400 ℃ at a heating rate of 16 ℃/h, heating the roasting furnace to 600 ℃ at a heating rate of 6 ℃/h, preserving heat for 4h, heating the roasting furnace to 1000 ℃ at a heating rate of 8 ℃/h, preserving heat for 55h, heating the roasting furnace to 1300 ℃ at a heating rate of 16 ℃, preserving heat for 20h, cooling the roasted anode, and discharging to obtain the prebaked anode.
Example 3
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes such steps as preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined petroleum coke is as follows: 9 percent of the powder with the grain diameter of 5-8mm, 25 percent of the powder with the grain diameter of 3-5mm, 30 percent of the powder with the grain diameter of 0.074-3mm and 36 percent of the ball milled powder with the grain diameter of less than 0.074 mm.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 32wt%, a quinoline insoluble matter content of 10wt%, a beta-resin content of 19.7wt% and a coking value of 55wt%.
The mass ratio of the graphite powder, the rare earth, the modified kaolin and the clay in the additive is 20.
The clay is as follows: calcining for 5 hours at the temperature of 900 ℃, and then crushing and grinding to obtain clay powder.
The rare earth mainly comprises the following raw materials in parts by weight: 30% of samarium, 10% of neodymium, 15% of yttrium, 10% of lanthanum, 10% of cerium and 25% of thulium.
The preparation method of the modified kaolin comprises the following steps: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 10, filtering and drying, adding water for dissolving, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, uniformly stirring for reacting for 3 hours, dehydrating, calcining for 10 hours at the temperature of 500 ℃, crushing and grinding to obtain the modified kaolin powder.
The total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide in the mixture accounts for 5% of the mass of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
(3) Production of a Green body
Stirring the calcined coke, the asphalt and the additive for 3 hours at the temperature of 150 ℃, and then placing the mixed material in a mould for vibration molding.
(4) Roasting
Placing the green body in a roasting furnace, heating the roasting furnace to 350 ℃ at the heating rate of 12 ℃/h, heating the roasting furnace to 700 ℃ at the heating rate of 8 ℃/h, preserving heat for 2h, heating the roasting furnace to 1100 ℃ at the heating rate of 8 ℃/h, preserving heat for 45h, heating the roasting furnace to 1200 ℃ at the heating rate of 12 ℃, preserving heat for 30h, cooling the roasted anode and discharging to obtain the prebaked anode.
Example 4
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes such steps as preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 12% of the ball mill powder with the grain diameter of 5-8mm, 23% of the ball mill powder with the grain diameter of 3-5mm, 30% of the ball mill powder with the grain diameter of 0.074-3mm and the content of the ball mill powder with the grain diameter of below 0.074mm are adopted.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, the mass content of toluene insoluble substances is 31wt%, the mass content of quinoline insoluble substances is 10wt%, the mass content of beta-resin is 20.3wt%, and the coking value is 55.8wt%.
The mass ratio of the graphite powder to the rare earth to the modified kaolin to the clay is (26.3).
The clay is as follows: calcining for 7h at the temperature of 770 ℃, and then crushing and grinding to obtain clay powder.
The rare earth mainly comprises the following raw materials in parts by weight: samarium 17%, neodymium 23%, yttrium 12%, lanthanum 27%, cerium 10% and thulium 11%.
The preparation method of the modified kaolin comprises the following steps: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 10, filtering and drying, adding water for dissolving, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, uniformly stirring for reacting for 3 hours, dehydrating, calcining for 7 hours at the temperature of 650 ℃, crushing and grinding to obtain the modified kaolin powder.
The total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide in the mixture accounts for 4% of the mass of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
(3) Production of a Green body
Stirring the calcined coke, the asphalt and the additive for 2 hours at 160 ℃, and then placing the mixture into a mould for vibration molding.
(4) Roasting
Placing the green body in a roasting furnace, heating the roasting furnace to 380 ℃ at a heating rate of 14 ℃/h, heating the roasting furnace to 680 ℃ at a heating rate of 8 ℃/h, preserving heat for 3.5h, heating the roasting furnace to 1100 ℃ at a heating rate of 7 ℃/h, preserving heat for 50h, heating the roasting furnace to 1250 ℃ at a heating rate of 15 ℃, preserving heat for 28h, cooling the roasted anode, and discharging to obtain the prebaked anode.
Comparative example 1
This example is different from example 1 in that the raw material for preparing the prebaked anode is different.
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 11% of the ball mill powder with the particle size of 5-8mm, 21% of the ball mill powder with the particle size of 3-5mm, 32% of the ball mill powder with the particle size of 0.074-3mm and the particle size of below 0.074mm, wherein the ball mill powder with the particle size of 3-5mm is prepared from the raw materials.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 30wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 20.7wt% and a coking value of 56.1wt%.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
Comparative example 2
This example is different from example 1 in that the raw material for preparing the prebaked anode is different.
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined petroleum coke is as follows: 11% of the ball mill powder with the particle size of 5-8mm, 21% of the ball mill powder with the particle size of 3-5mm, 32% of the ball mill powder with the particle size of 0.074-3mm and the particle size of below 0.074mm, wherein the ball mill powder with the particle size of 3-5mm is prepared from the raw materials.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 30wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 20.7wt% and a coking value of 56.1wt%.
The additive is graphite powder.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
Comparative example 3
This example is different from example 1 in that the raw material for preparing the prebaked anode is different.
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes such steps as preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 11% of the ball mill powder with the particle size of 5-8mm, 21% of the ball mill powder with the particle size of 3-5mm, 32% of the ball mill powder with the particle size of 0.074-3mm and the particle size of below 0.074mm, wherein the ball mill powder with the particle size of 3-5mm is prepared from the raw materials.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 30wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 20.7wt% and a coking value of 56.1wt%.
The mass ratio of the graphite powder to the clay mixed in the additive is 23.
The clay is as follows: calcining for 7 hours at the temperature of 800 ℃, and then crushing and grinding to obtain clay powder.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
Comparative example 4
This example is different from example 1 in that the raw material for preparing the prebaked anode is different.
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes such steps as preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 11% of the ball mill powder with the particle size of 5-8mm, 21% of the ball mill powder with the particle size of 3-5mm, 32% of the ball mill powder with the particle size of 0.074-3mm and the particle size of below 0.074mm, wherein the ball mill powder with the particle size of 3-5mm is prepared from the raw materials.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 30wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 20.7wt% and a coking value of 56.1wt%.
The mass ratio of the graphite powder to the modified kaolin to the clay in the additive is 23.
The clay is as follows: calcining for 7 hours at the temperature of 800 ℃, and then crushing and grinding to obtain clay powder.
The preparation method of the modified kaolin comprises the following steps: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 9.5, filtering and drying, adding water to dissolve, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, stirring uniformly to react for 3 hours, dehydrating, calcining for 6 hours at the temperature of 650 ℃, crushing and grinding to obtain the modified kaolin powder.
The total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide which are mixed together accounts for 3% of the mass of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is (100).
Comparative example 5
This example is different from example 1 in that the raw material for preparing the prebaked anode is different.
A process for preparing the diluted trace elements of prebaked anode carbon block for aluminium electrolysis includes preparing raw materials, proportioning, preheating, kneading, shaping, calcining and discharging. The method comprises the following steps:
(1) Stock preparation
Sieving the calcined petroleum coke raw material, wherein the weight percentage of each grade material in the sieved calcined coke is as follows: 11% of the ball mill powder with the particle size of 5-8mm, 21% of the ball mill powder with the particle size of 3-5mm, 32% of the ball mill powder with the particle size of 0.074-3mm and the particle size of below 0.074mm, wherein the ball mill powder with the particle size of 3-5mm is prepared from the raw materials.
The asphalt is modified asphalt, wherein the modified asphalt has a softening point of 108 ℃, a toluene insoluble matter content of 30wt%, a quinoline insoluble matter content of 11wt%, a beta-resin content of 20.7wt% and a coking value of 56.1wt%.
The mass ratio of graphite powder, rare earth, kaolin and clay in the additive is 23.
The clay is as follows: calcining for 7 hours at the temperature of 800 ℃, and then crushing and grinding to obtain clay powder.
The rare earth mainly comprises the following raw materials in parts by weight: samarium 20%, neodymium 15%, yttrium 22%, lanthanum 18%, cerium 12% and thulium 13%.
(2) Ingredients
The mass ratio of the calcined coke, the asphalt and the additive is 100.
Comparative example 6
This example is different from example 1 in the method of preparing a prebaked anode. The firing method is different.
And (3) placing the green body in a roasting furnace, heating the roasting furnace to 650 ℃ at the heating rate of 7 ℃/h, preserving heat for 3h, heating the roasting furnace to 1250 ℃ at the heating rate of 13 ℃, preserving heat for 75h, cooling the roasted anode, and discharging the cooled roasted anode out of the furnace to obtain the prebaked anode.
The performance of the aluminum electrolytic prebaked anodes produced in examples 1 to 4 and comparative examples 1 to 6 was measured and tested according to the specification of YS/T63.9. The results are shown in table 1:
TABLE 1 Performance of aluminum electrolytic prebaked anodes for various examples and comparative examples
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A preparation method of dilutable prebaked anode carbon block trace elements for aluminum electrolysis is characterized by comprising the following steps:
(1) Kneading the calcined coke, asphalt and additive to obtain a kneaded material green body;
(2) Placing the green body in a roasting furnace, heating the roasting furnace to 350-400 ℃ at the heating rate of 12-16 ℃/h, heating the roasting furnace to 600-700 ℃ at the heating rate of 6-8 ℃/h, preserving heat for 2-4h, heating the roasting furnace to 1000-1100 ℃ at the heating rate of 6-8 ℃/h, preserving heat for 45-55h, heating the roasting furnace to 1200-1300 ℃ at the heating rate of 12-16 ℃, preserving heat for 20-30h, cooling the roasted anode and taking out of the furnace to obtain a prebaked anode;
the calcined petroleum coke raw material is screened, and the weight percentage of each grade material in the screened calcined coke is as follows: 9-13% of 5-8mm particle size, 16-25% of 3-5mm particle size, 30-38% of 0.074-3mm particle size and 32-40% of ball milled powder with particle size below 0.074 mm;
the additive comprises: graphite powder, rare earth, modified kaolin and clay;
the mass ratio of the calcined coke, the asphalt and the additive is 100:40-55:1-10.
2. The method for preparing the pre-baked anode carbon block trace elements for dilutable aluminum electrolysis as claimed in claim 1, wherein the mass ratio of the graphite powder, the rare earth, the modified kaolin and the clay in the additive is 20-30.
3. The method for preparing dilutable prebaked anode carbon block trace elements for aluminum electrolysis according to claim 1, wherein the asphalt is modified asphalt having a softening point of 105-110 ℃, a toluene insoluble matter content of 29-32wt%, a quinoline insoluble matter content of 10-11wt%, a β -resin of 19.7-21.3wt%, and a coking value of 55-57wt%.
4. The method for preparing the trace elements of the pre-baked anode carbon block for the dilutable aluminum electrolysis as recited in claim 1, wherein the rare earth mainly comprises the following elements: samarium, neodymium, yttrium, lanthanum, cerium, and thulium.
5. The method for preparing the trace elements in the pre-baked anode carbon block for the aluminum electrolysis as claimed in claim 1, wherein the rare earth mainly comprises the following raw materials in parts by weight: 10-30% of samarium, 10-30% of neodymium, 10-30% of yttrium, 10-30% of lanthanum, 10-30% of cerium and 10-30% of thulium.
6. The method for preparing dilutable prebaked anode carbon block trace elements for aluminum electrolysis according to claim 1, wherein the clay is: calcining at 700-900 deg.C for 5-10h, and crushing and grinding to obtain clay powder.
7. The method for preparing dilutable prebaked anode carbon block trace elements for aluminum electrolysis according to claim 1, wherein the method for preparing the modified kaolin comprises: crushing and grinding kaolin to obtain kaolin powder, fully immersing the kaolin powder in a KOH solution, wherein the pH value of the KOH solution is 9-10, filtering and drying, adding water for dissolving, adding sodium gluconate, ethylene diamine tetraacetic acid and polyacrylamide, uniformly stirring for reacting for a period of time, dehydrating, calcining for 3-10h at the temperature of 500-700 ℃, crushing and grinding to obtain the modified kaolin powder.
8. The method for preparing the trace elements in the pre-baked anode carbon block for the aluminum electrolysis according to claim 7, wherein the total amount of the sodium gluconate, the ethylene diamine tetraacetic acid and the polyacrylamide in the mixture accounts for 1-5% of the kaolin, and the mass ratio of the sodium gluconate to the ethylene diamine tetraacetic acid to the polyacrylamide is 1-5.
9. The method for preparing the trace elements of the pre-baked anode carbon block for the aluminum electrolysis as claimed in claim 1, wherein the step (1) comprises the steps of stirring the calcined coke, the asphalt and the additives for 1-3 hours at 150-165 ℃, and then placing the mixture in a mold for vibration molding.
10. The preparation method of dilutable pre-baked anode carbon block trace elements for aluminum electrolysis according to claim 1, wherein in the step (2), the green body is placed in a baking furnace, the baking furnace is heated to 350-380 ℃ at a heating rate of 14-15 ℃/h, then the baking furnace is heated to 650-700 ℃ at a heating rate of 6-8 ℃/h, the temperature is preserved for 3-4h, then the baking furnace is heated to 1050-1100 ℃ at a heating rate of 6-8 ℃/h, the temperature is preserved for 50-55h, then the baking furnace is heated to 1250-1300 ℃ at a heating rate of 14-15 ℃, the temperature is preserved for 24-28h, and the baked anode is discharged after being cooled to obtain the pre-baked anode.
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