CN114315356A - Aluminum electrolysis carbon anode oxidation resistant coating and preparation method thereof - Google Patents
Aluminum electrolysis carbon anode oxidation resistant coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminum electrolysis carbon anode oxidation resistant coating and a preparation method thereof, belonging to the field of anode oxidation resistant coatings. The prepared anti-oxidation coating consists of a solid phase, a binder and an auxiliary sintering agent, has stable property, is uniformly coated or sprayed on the surface of an aluminum electrolytic carbon anode at room temperature, is dried to form a protective layer, and is sintered at 400-800 ℃ to form a compact cryolite type structural substance containing Na-Al-Si-O chrysolite, mullite and Na-Al-F so as to improve the oxidation resistance. Through the oxidation resistance test, the weight loss rate of the carbon anode using the coating is reduced by more than 40 percent compared with that of a bare anode under the high-temperature condition, the cost of the used raw materials is low, the coating is compact, and the oxidation resistance effect is good.
Description
Technical Field
The invention belongs to the field of anode oxidation resistant coatings, and particularly relates to an aluminum electrolysis carbon anode oxidation resistant coating and a preparation method thereof.
Background
In the aluminum electrolysis production process, the anode carbon block not only plays a role in conducting electricity in the whole aluminum electrolysis process, but also is an important component participating in the aluminum electrolysis chemical reaction. Therefore, the carbon plays an extremely important role in the whole process flow of aluminum electrolysis, and the quality of the carbon anode influences various technical indexes of the carbon anode in the aluminum electrolysis, and directly influences the stable operation of the electrolytic cell and the like. The consumption of carbon anode is one of the important indicators, and it reacts with O at high temperature2、CO2The oxidation reaction that occurs, i.e., anodic oxidation, results in excessive consumption of the carbon anode. In the economic aspect, a great deal of cost damage is caused to the aluminum electrolysis plant; in environmental aspect, the products are CO and CO2So the pollution to the environment and the warming of the climate are also influenced; in the aspect of social benefit, anode oxidation resistance is one of the important problems required by aluminum electrolysis production and is one of the obstacles for limiting the development of the aluminum electrolysis industry in China.
The consumption of carbon anodes in electrolytic aluminum production can be mainly divided into electrochemical consumption, combustion consumption and mechanical consumption. In the production process of electrolytic aluminum, most of the anode carbon consumption is directly consumed by the electrochemical reaction in the electrolytic process. And in the production process of electrolytic aluminum, O ions are discharged on the surface of the anode and then react with C to generate CO and CO2. The combustion consumption refers to the consumption of the anode carbon block caused by air combustion, a Boolean reaction, a secondary reaction and the like. And the combustion reaction typically occurs both at the top and at the sides of the anode. When the hot anode surface contacts oxygen or CO which is free in the vicinity of the hot anode surface2When the reaction is carried out, the corresponding chemical reaction can be carried out, thereby generating CO2And CO. The mechanical consumption is mainly the consumption of the anode caused by carbon residue. Wherein the carbon residue is a by-product that is detached from the anode due to high temperature agitation, etc. At the root, the mechanism of mechanical wear is: because of the high activity of binder pitch coking, it preferentially undergoes oxidation reactions. Then, the coking substance generated by the reaction of the asphalt protrudes from the surface of the anode carbon block, and under the influence of gravity and the agitation of heat flow and electrolyte, the protruding part falls off from the surface of the anode, so that carbon consumption is caused, and the falling coking substance is carbon residue. According to statistics, the carbon consumption caused by the carbon residue can account for about 5 percent of the total carbon consumption.
The research on the anode oxidation resistance method is mainly divided into three categories: coating methods, additive methods, and solution dipping methods. The coating method is now commonly used as B4C-SiC，SiO2，Si3N4And the like are used as a coating to be painted or sprayed on the anode carbon block to enable the anode carbon block to generate antioxidant capacity. But the disadvantages are that: the effect is not lasting and is easy to fall off, and the grade of the final product is influenced. The basic principle of the additive method, namely the pre-anode method, is to add some elements capable of changing the oxidation resistance of the anode, such as metals like Cu or a few aluminum salts, in the pre-preparation and manufacturing processes of the carbon anode. However, the additive method has some obvious disadvantages, the main disadvantages are that the preparation process of the special material prepared anode is very complicated, and the antioxidant capacity of the prepared anode is seriously influenced due to uneven dispersion of the added additive in the anode carbon block. The solution dipping method is to use AlCl firstly3The solution is used for dipping the carbon anode, then ammonia water is used for dipping, and finally roasting treatment is carried out, so that the pre-prepared anode with the oxidation resistance is obtained. The solution impregnation method also has certain disadvantages, mainly manifested by non-durable oxidation resistance and complex operation.
Disclosure of Invention
The technical task of the invention is to provide an aluminum electrolysis carbon anode oxidation resistant coating and a preparation method thereof aiming at the defects of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: an aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 39-51% of aluminum hydroxyfluoride, 9-41% of a binder and 19-41% of an auxiliary sintering agent, wherein the sum of the mass percentages of the components is 100%.
Further, the binder is prepared by mixing one or more of polyvinyl alcohol, sodium carboxymethylcellulose, water glass, polyacrylamide and a silane coupling agent with water according to a mass ratio of (1-5) to 1.
Further, the auxiliary sintering agent is one or more of sodium fluoride, magnesium fluoride, potassium fluoride, lithium fluoride, sodium carbonate, magnesium carbonate and potassium carbonate.
Further, the aluminum hydroxyfluoride (AlF)x(OH)3-xAnd x < 3) and the auxiliary sintering agent are both below 200 meshes.
The preparation method of the aluminum electrolysis carbon anode oxidation resistant coating based on the components comprises the following steps:
(1) weighing raw materials of each component; (2) uniformly mixing aluminum hydroxyfluoride and an auxiliary sintering agent to obtain a solid-phase mixture; (3) preparing a liquid phase binder; (4) uniformly dispersing the solid-phase mixture in a liquid-phase binder to obtain the antioxidant coating; (5) and (3) uniformly coating the antioxidant coating on the surface of the carbon anode, and then placing the carbon anode in a shade place for air drying.
Further, the stirring time in the configuration process of the step (3) is not less than 30 min.
Further, the air drying time in the step (5) is 6-24 h.
Further, the preparation method further comprises the following steps: and (3) roasting the air-dried carbon anode with the coating, and then cooling.
Further, the roasting temperature is 400-800 ℃, and the time is not less than 2 hours.
Compared with the prior art, the invention has the beneficial effects that:
the prepared anti-oxidation coating consists of a solid phase, a binder and an auxiliary sintering agent, and can be attached to the surface of an anode to form a protective layer after being coated or sprayed and dried. The protective layer is sintered at 400-800 ℃ to form a compact cryolite-type structural substance containing Na-Al-Si-O chrysolite, mullite and Na-Al-F, so that the oxidation resistance is improved. Compared with the prior art, the anti-oxidation coating prepared by the invention has stable property, can be used for brushing or spraying the anode at room temperature, and is simple to operate. In the process flow, no volatile raw materials such as ammonia water and the like exist, so that manual operation is greatly facilitated. Compared with a method of adding a metal element additive, the method has the advantages that the used raw materials are low in price, the economic conditions are more excellent, and the prepared coating is good in oxidation resistance effect.
Drawings
FIG. 1 is a flow chart of a preparation method of the present invention;
FIG. 2 is an optical representation of the carbon anode of example 1 with a coating applied to the surface thereof;
FIG. 3 is an optical representation of the baked coating of example 1;
FIG. 4 is a phase representation of the baked coating of example 1;
FIG. 5 is a phase diagram of the baked coating of example 2.
FIG. 6 is a phase diagram of the baked coating of example 6.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The aluminum hydroxyfluoride used in each example has the formula AlF1.5(OH)1.5The particle size of the auxiliary sintering agent is 200 meshes or less. The preparation flow of the anode oxidation resistant coating of the aluminum electrolytic carbon is shown in figure 1.
Example 1
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 40% of aluminum hydroxyfluoride, 40% of a binder and 20% of an auxiliary sintering agent; wherein the binder is formed by mixing water glass and water according to the mass ratio of 3: 1; the auxiliary sintering agent is sodium fluoride (NaF) and magnesium fluoride (MgF) with the mass ratio of 3:12) A mixture of (a); the water glass contains 40 wt% of Na2O·nSiO2The modulus was 3.3.
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) crushing of aluminum hydroxyfluoride: the blocky aluminum hydroxyfluoride is crushed by a crusher, and in the crushing process, the crushed particles pass through a 200-mesh sieve every time. The passed is ready for use, and the residual particles are crushed again with the next batch of crushed materials. The operation is circulated until all the materials are crushed to be below 200 meshes;
(2) weighing the raw materials of the components according to the proportion, putting the hydroxyl aluminum fluoride and the sodium fluoride into a mixer, and uniformly mixing to obtain a solid-phase mixture for later use;
(3) preparing a binder, namely adding water into water glass in batches, continuously stirring, sealing by using a preservative film, and stirring for 40min in a shade place;
(4) mixing a solid-liquid material, namely mixing the solid-phase mixture obtained in the step with a liquid-phase binder, and adding the binder for multiple times while stirring in the mixing process so as to better uniformly mix the solid-liquid material and the liquid-phase binder;
(5) painting the coating, namely uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 12 hours, as shown in figures 2-3, wherein figure 2 (left) is a representation diagram in the coating process; FIG. 2 (right) is a representation of the coating after air drying;
(6) and (3) roasting, namely heating the air-dried anode to 700 ℃ and preserving heat for 2 hours, wherein the phase of the roasted coating is shown in figure 4.
Na2SiO3The aqueous solution is subjected to a sintering reaction at a high temperature of 600-950 ℃ to generate a Na-Al-Si-O special phase structure substance with a rutile structure, and the oxidation resistance is guaranteed by means of a compact surface structure.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 48.9 percent compared with that of the graphite carbon block without the coating.
Example 2
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 50% of aluminum hydroxyfluoride, 25% of binder and 25% of auxiliary sintering agent; wherein the binder is formed by mixing polyvinyl alcohol and water according to the mass ratio of 2: 1; the auxiliary sintering agent is sodium fluoride (NaF), and the molecular weight of the polyvinyl alcohol used is 44.05.
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) examples (1) to (4) were the same except for the binder;
(5) uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 16 hours;
(6) and (3) roasting, namely heating the air-dried anode to 800 ℃ and preserving heat for 2.5 hours, wherein the phase of a roasted coating is shown in figure 5.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 46.7 percent compared with that of the graphite carbon block without the coating.
Example 3
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 45% of aluminum hydroxyfluoride, 15% of binder and 40% of auxiliary sintering agent; the adhesive is formed by mixing polyvinyl alcohol and water according to the mass ratio of 3:1, the auxiliary sintering agent is a mixture of sodium fluoride (NaF) and lithium fluoride (LiF) according to the mass ratio of 3:1, and the molecular weight of the polyvinyl alcohol is 44.05.
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) examples (1) to (4) were the same except for the binder;
(5) uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 12 hours;
(6) and (4) roasting, namely heating the air-dried anode to 750 ℃ and preserving heat for 2 hours.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 46.2 percent compared with that of the graphite carbon block without the coating.
Example 4
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 48% of aluminum hydroxyfluoride, 12% of a binder and 40% of an auxiliary sintering agent; the binder is prepared by mixing sodium carboxymethylcellulose and water according to a mass ratio of 4:1, the auxiliary sintering agent is sodium fluoride (NaF), and the viscosity of the used sodium carboxymethylcellulose is 800-1200 mpa.s.
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) examples (1) to (4) were the same except for the binder;
(5) uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 12 hours;
(6) and (4) roasting, namely heating the air-dried anode to 650 ℃ and keeping the temperature for 2 hours.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 45.1 percent compared with that of the graphite carbon block without the coating.
Example 5
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 50% of aluminum hydroxyfluoride, 10% of binder and 40% of auxiliary sintering agent; wherein the adhesive is formed by mixing a silane coupling agent and water according to the mass ratio of 1:1, and the auxiliary sintering agent is sodium carbonate (Na)2CO3)。
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) the steps (1) to (4) are the same as the step (3) except that the binder is different, and the stirring time is 60 min;
(5) uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 12 hours;
(6) and (4) roasting, namely heating the air-dried anode to 780 ℃ and preserving heat for 2 hours.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 47.8 percent compared with that of the graphite carbon block without the coating.
Example 6
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 46% of aluminum hydroxyfluoride, 25% of binder and 29% of auxiliary sintering agent; the adhesive is formed by mixing a silane coupling agent and water according to the mass ratio of 2:1, the auxiliary sintering agent is sodium fluoride (NaF), the used silane coupling agent is vinyl tris (2-methoxyethoxy) silane, and the purity: 96.0% (GC).
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) examples (1) to (6) are the same as example 5 except that the binder is different; the phase of the coating after firing of this example is shown in FIG. 6.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 42.9 percent compared with that of the graphite carbon block without the coating.
Example 7
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 48% of aluminum hydroxyfluoride, 32% of binder and 20% of auxiliary sintering agent; the binder is prepared by mixing sodium carboxymethylcellulose and water according to the mass ratio of 2:1, the auxiliary sintering agent is sodium fluoride (NaF), and the viscosity of the used sodium carboxymethylcellulose is 800-1200 mpa.s.
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) the steps (1) to (4) are the same as the step (3) except that the binder is different, and the stirring time is 55 min;
(5) uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 12 hours;
(6) and (4) roasting, namely heating the air-dried anode to 800 ℃ and keeping the temperature for 2 hours.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 44.8 percent compared with that of the graphite carbon block without the coating.
Example 8
An aluminum electrolysis carbon anode oxidation resistant coating comprises the following raw materials in percentage by mass: 40% of aluminum hydroxyfluoride, 20% of binder and 40% of auxiliary sintering agent; the binder is prepared by mixing sodium carboxymethylcellulose and water according to a mass ratio of 5:1, the auxiliary sintering agent is sodium fluoride (NaF), and the viscosity of the used sodium carboxymethylcellulose is 800-1200 mpa.s.
The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon comprises the following steps:
(1) the steps (1) to (4) are the same as the step (3) except that the binder is different, and the stirring time is 50 min;
(5) uniformly coating the uniformly mixed coating obtained by the operation on the surface of the carbon anode, and then placing the carbon anode in a ventilated and cool place for air drying for 12 hours;
(6) and (4) roasting, namely heating the air-dried anode to 600 ℃ and preserving heat for 2 hours.
And (3) testing the oxidation resistance:
and (3) measuring the weight loss rate at high temperature by a high-temperature weight loss rate tester for the obtained anode with the antioxidant coating and the anode without the antioxidant coating, and comparing.
Measurement conditions were as follows: keeping the temperature from room temperature to 550 ℃ for 1h, then heating to 960 ℃ and keeping the temperature for 1h, wherein the heating rate is 10 ℃/min.
Through detection, the final weight loss rate is calculated, and the oxidation effect of the graphite carbon block with the coating is reduced by 45.6 percent compared with that of the graphite carbon block without the coating.
The technical idea of the present invention is described in the above technical solutions, and the protection scope of the present invention is not limited thereto, and any changes and modifications made to the above technical solutions according to the technical essence of the present invention belong to the protection scope of the technical solutions of the present invention.
Claims (9)
1. The aluminum electrolysis carbon anode oxidation resistant coating is characterized by comprising the following raw materials in percentage by mass: 39-51% of aluminum hydroxyfluoride, 9-41% of a binder and 19-41% of an auxiliary sintering agent, wherein the sum of the mass percentages of the components is 100%.
2. The aluminum electrolytic carbon anode oxidation resistant coating as claimed in claim 1, wherein the binder is formed by mixing one or more of polyvinyl alcohol, sodium carboxymethylcellulose, water glass, polyacrylamide and silane coupling agent with water according to a mass ratio of (1-5) to 1.
3. The aluminum electrolytic carbon anode antioxidant coating as claimed in claim 1, wherein the auxiliary sintering agent is one or more of sodium fluoride, magnesium fluoride, potassium fluoride, lithium fluoride, sodium carbonate, magnesium carbonate and potassium carbonate.
4. The aluminum electrolytic carbon anode oxidation resistant coating as claimed in claim 1, wherein the particle size of the aluminum hydroxyfluoride and the particle size of the auxiliary sintering agent are both below 200 meshes.
5. The preparation method of the aluminum electrolysis carbon anode oxidation resistant coating as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
(1) weighing raw materials of each component; (2) uniformly mixing aluminum hydroxyfluoride and an auxiliary sintering agent to obtain a solid-phase mixture; (3) preparing a liquid phase binder; (4) uniformly dispersing the solid-phase mixture in a liquid-phase binder to obtain the antioxidant coating; (5) and (3) uniformly coating the antioxidant coating on the surface of the carbon anode, and then placing the carbon anode in a shade place for air drying.
6. The method for preparing the anode oxidation resistant coating of the aluminum electrolytic carbon according to claim 5, wherein the stirring time in the preparation process of the step (3) is not less than 30 min.
7. The preparation method of the anode oxidation resistant coating of the aluminum electrolytic carbon according to claim 5, wherein the air drying time in the step (5) is 6-24 h.
8. The method for preparing the anode oxidation resistant coating of the aluminum electrolytic carbon according to claim 5, further comprising: and (3) roasting the air-dried carbon anode with the coating, and then cooling.
9. The method for preparing the anode oxidation resistant coating of the aluminum electrolytic carbon according to claim 8, wherein the roasting temperature in the step (6) is 400-800 ℃ and the time is not less than 2 h.
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Cited By (2)
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| CN116606561A (en) * | 2023-06-12 | 2023-08-18 | 云南点援微晶科技有限公司 | Electrolytic aluminum carbon anode antioxidation anticorrosive paint |
| CN116813386A (en) * | 2023-06-30 | 2023-09-29 | 广西大学 | Self-healing high-oxygen-resistance high-temperature-oxidation-prevention composite coating for aluminum electrolysis carbon anode and preparation method thereof |
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