CN101250723A - Carbon element anode oxidation resistance layer for aluminium electrolysis, preparation method and coating method thereof - Google Patents
Carbon element anode oxidation resistance layer for aluminium electrolysis, preparation method and coating method thereof Download PDFInfo
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Abstract
The invention discloses an aluminium electrolysis used carbon anode antioxidation layer with good associativity with a carbon anode basal body and excellent antioxidation performance. The invention also discloses a method for preparing the antioxidation layer and a method for coating the antioxidation layer. The aluminium electrolysis used carbon anode antioxidation layer of the invention comprises the antioxidation layer of a bottom layer, the antioxidation layer of a barrier layer and the antioxidation layer of a surface layer from bottom to top. The method for preparing the aluminium electrolysis used carbon anode antioxidation layer comprises: preparing the antioxidation layer of the bottom layer, the antioxidation layer of the barrier layer and the antioxidation layer of the surface layer. The method for coating the aluminium electrolysis used carbon anode antioxidation layer comprises following steps: firstly, spraying slurry coating of the bottom layer twice or three times, wherein spraying time interval is 1 to 3 hours, drying under normal temperature, secondly, spraying the slurry coating of the barrier layer once or twice, wherein the spraying time interval is 1 to 3 hours, drying under the normal temperature, thirdly, spraying the slurry coating of the surface layer once or twice, wherein the spraying time interval is 1 to 3 hours, and drying under the normal temperature.
Description
(1) technical field:
The present invention relates to field of aluminum electrolysis, particularly carbon element anode oxidation resistance layer for aluminium electrolysis; The invention still further relates to the preparation method and the coating method thereof of this anti oxidation layer.
(2) background technology:
In aluminium electrolysis process, carbon annode had both been born electric action, participated in electrochemical reaction again, constantly consumed, and technico-economical comparison and primary aluminum quality are all had very significant effects, therefore was called as " heart " of aluminium cell.The Working environment of electrolysis of aluminum carbon annode is the high temperature aluminum electrolyzer, temperature distribution situation according to aluminium cell, the temperature of anode temperature that makes progress from the bottom reduces gradually, bottom temp is greatly about 900 ℃, head temperature is about 450 ℃, under the hot environment, oxidizing reaction promptly can take place in anode and air contact part, generates CO
2, also have reaction of cloth Dorr and anode to fall slag in addition, these reactions make carbon annode produce extra consumption.In order to reduce owing to CO
2The excess carbon consumption that causes with air combustion, save the production cost of primary aluminum, both economical effective means is at carbon annode surface-coated anti oxidation layer, as application number is 200410022671.4, name is called the " anti-oxidation method of used for aluminium electrolysis carbon annode, anti oxidation layer and coating method thereof " Chinese invention patent, anti-oxidation method at the pre-calcining electrolytic cell carbon annode of prebaked anode surface-coated oxidation resistant coating is disclosed, it also discloses the employed oxidation resistant coating of this method, its prescription comprises in weight part: 5~60 parts of alumina sols in solid content, particle diameter is less than the Al of 165 μ m
2O
316~35 parts in powder, particle diameter is less than 1~3 part in the boron oxide powder of 165 μ m; The coating method of above-mentioned oxidation resistant coating, i.e. spraying method repeatedly.This invention oxidation resistant coating, though reduced certain carbon consumption, there is certain difference in the coefficient of thermal expansion of itself and carbon annode matrix, coating is easy to generate crackle and causes bulk to come off under the high temperature, and its oxidation-resistance is restricted.
(3) summary of the invention:
The present invention will disclose a kind of and carbon element anode oxidation resistance layer for aluminium electrolysis that the carbon annode matrix bond is good, antioxidant property is excellent, with low cost, and the present invention also will disclose the preparation method and the coating method thereof of this anti oxidation layer.
Carbon element anode oxidation resistance layer for aluminium electrolysis of the present invention comprises bottom anti oxidation layer, blocking layer anti oxidation layer and surface layer anti oxidation layer from the bottom to top.
Wherein, described bottom anti oxidation layer comprises the composition of following proportioning in weight part:
Water fluoric resin 15-45 part; Particle diameter is for containing boron substance 25-50 part less than 165 μ m;
Alumina sol 1-20 part; Particle diameter is less than high-temperature anti-oxidant 1-26 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 12-40 part.
Described blocking layer anti oxidation layer comprises the composition of following proportioning in weight part:
Water fluoric resin 4-22 part; Particle diameter is for containing boron substance 1-16 part less than 165 μ m;
Alumina sol 1-25 part; Particle diameter is less than high-temperature anti-oxidant 5-58 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 21-45 part.
Described surface layer anti oxidation layer comprises the composition of following proportioning in weight part:
Water fluoric resin 3-20 part; Particle diameter contains boron substance 1-16 part less than 165 μ m's;
Alumina sol 10-30 part; Particle diameter is less than high-temperature anti-oxidant 6-59 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 22-42 part.
In the above-mentioned prescription, the fluorine content of described water fluoric resin is preferably 12-50%, and number-average molecular weight is 4 * 10
3-10 * 10
4The described boron substance that contains can be boron oxide, or norbide, or boric acid, or any two or more mixture in them; Described high-temperature anti-oxidant can be aluminum oxide, or pseudo-boehmite, or aluminum fluoride, or any two or more mixture in them; Described alumina sol is the alumina sol in solid content>5%; Described defoamer is the water-based non-silicon defoamer, as defoamer DF-558, or defoamer DF-558, or defoamer CLT-371 etc.
Carbon element anode oxidation resistance layer for aluminium electrolysis of the present invention, the composition of bottom prescription is for containing boron substance, water fluoric resin, water, alumina sol and high-temperature anti-oxidant, the effect of this coating is the hole of sealing substrate material surface, reduces the contact area of carbon anode matrix and oxygen under the high temperature; Adherent coating again when containing the wetting carbon annode matrix of being introduced in of boron substance is more or less the same the thermal expansivity of coating and matrix, plays a part relaxation heat stress and improves bonding strength; The composition of blocking layer prescription is high-temperature anti-oxidant, contain boron substance, water fluoric resin, water and alumina sol, the topmost effect of this coating is to isolate matrix and external environment, stop the diffusion of oxygen under the high temperature to be invaded, introducing as aluminum oxide etc., itself plays a part isolation from oxygen, has great antioxidant effect; The composition of surface layer prescription is high-temperature anti-oxidant, contain boron substance, water fluoric resin, water and alumina sol, the boron substance that contains has wherein not only consumed oxygen in the high temperature oxidation atmosphere, and it at high temperature is the glassy phase material, and viscosity is big, has certain fluidity, crackle and hole that coating is at high temperature produced seal, and have reduced extraneous oxygen and have entered passage inner and the matrix direct reaction, play a part to stop oxygen simultaneously; In each anti oxidation layer prescription, add proper quantity of defoaming agent, can eliminate the bubble problem of coating paste in preparation process, avoided coatingsurface to form pore because of foaming.
The present invention also comprises the preparation method of carbon element anode oxidation resistance layer for aluminium electrolysis, it comprises the preparation method of bottom anti oxidation layer, blocking layer anti oxidation layer and surface layer anti oxidation layer, and their preparation method is and adds raw material by following feeding sequence and mix and get final product; The feeding sequence of described raw material is: get a certain amount of water earlier, add alumina sol and defoamer then therein, add and contain boron substance and high-temperature anti-oxidant, add water fluoric resin at last.
The present invention also comprises the coating method of carbon element anode oxidation resistance layer for aluminium electrolysis, and available conventional coating method applies, and preferably adopts coating method provided by the invention, and its step is as follows:
1) spraying primer coating slurry is 2-3 time, and the timed interval of spraying is 1-3 hour, dries under the normal temperature; Described primer coating slurry comprises the composition of following proportioning in weight part:
Water fluoric resin 15-45 part; Particle diameter contains boron substance 25-50 part less than 165 μ m's;
Alumina sol 1-20 part; Particle diameter is less than high-temperature anti-oxidant 1-26 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 12-40 part;
2) spraying barrier coating slurry is 1-2 time, and the timed interval is 1-3 hour, dries under the normal temperature; Described barrier coating slurry comprises the composition of following proportioning in weight part:
Water fluoric resin 4-22 part; Particle diameter contains boron substance 1-16 part less than 165 μ m's;
Alumina sol 1-25 part; Particle diameter is less than high-temperature anti-oxidant 5-58 part of 74 μ m;
Defoamer 0.2-0.5 part; Water 21-45 part;
3) spraying surface layer coating paste is 1-2 time, and the timed interval is 1-3 hour, dries under the normal temperature to get final product; Described surface layer coating paste comprises the composition of following proportioning in weight part:
Water fluoric resin 3-20 part; Particle diameter is for containing boron substance 1-16 part less than 165 μ m;
Alumina sol 10-30 part; Particle diameter is less than high-temperature anti-oxidant 6-59 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 22-42 part.
The fluorine content of described water fluoric resin is preferably 12-50%, and number-average molecular weight is 4 * 10
3-10 * 10
4The described boron substance that contains can be boron oxide, or norbide, or boric acid, or any two or more mixture in them; Described high-temperature anti-oxidant can be aluminum oxide, or pseudo-boehmite, or aluminum fluoride, or any two or more mixture in them; Described alumina sol is the alumina sol of solid content>5%; Described defoamer is the water-based non-silicon defoamer, as defoamer DF-558, or defoamer DF-558, or defoamer CLT-371 etc.; The average coated weight of described whole anti oxidation layer is preferably in 0.05-0.2g/cm
2In.
Carbon element anode oxidation resistance layer for aluminium electrolysis of the present invention, good with the carbon annode matrix bond, antioxidant property is excellent, pollution-free, with low cost to aluminium electrolytic industry.Anti oxidation layer of the present invention comprises bottom, blocking layer and three layers of anti oxidation layer of surface layer from the bottom to top, in three layers of anti oxidation layer, all use water fluoric resin to be organic binder bond, hydrophobic group that it is contained and hydrophilic group make that the organic and inorganic composition is not that " profit " separates but wettability, dispersiveness good organic assembling all, thereby make coating antifouling property excellence, the recoat tack is good; Also used the low-melting boron substance that contains, it had not only wet the carbon annode matrix simultaneously but also adherent coating when fusion, promoted the Chemical bond of oxidation resistant coating and carbon annode matrix under the high temperature, avoided different coating crackings that cause of coating or bulk to come off, improved the adhesiveproperties of coating with carbon annode matrix coefficient of thermal expansion; Contain boron substance on the other hand and be the glass melt shape more than 600 ℃, viscosity is big, has certain fluidity and can make the crackle that produces in the coating up, can be wetting well and cover the carbon element surface, stoped entering of oxidizing gas, made coating have certain self-healing ability; Along with the variation of composition and content in three layers of anti oxidation layer, played good gradient antioxidant property, between three layers of anti oxidation layer, realize action compensating simultaneously.
Anti oxidation layer employing spraying coating process of the present invention forms on the carbon annode matrix has gradient anti-oxidant function three-layer sandwich type structure, not only can overcome the defective of single layer structure coating, relaxation heat stress, strengthen the heat-shock resistance of coating, and can also in temperature-rise period, play and stop and delay the effect of boron oxide evaporable, thereby make coating in long-time, bring into play antioxygenation preferably.
(4) embodiment:
Embodiment 1
(1) preparation coating paste:
1) gets 400 gram water, add the alumina sol and the 1 gram DF-568 defoamer of 10 gram solid content>5% therein; Add again 250 grams less than the norbide of 165 μ m, 95 grams less than the aluminum oxide of 74 μ m, 94 grams pseudo-boehmites less than 74 μ m; Add 150 gram fluorine content at last and be 12% water fluoric resin; It is stand-by to make the primer coating slurry behind the uniform mixing;
2) get 450 gram water, add the alumina sol and the 1 gram DF-568 defoamer of 50 gram solid content>5% therein; Add then 5 grams less than the boron oxide of 165 μ m, 5 grams less than the boric acid of 165 μ m, 449 grams pseudo-boehmites less than 74 μ m; Add 40 gram fluorine content at last and be 12% water fluoric resin; It is stand-by to make the barrier coating slurry behind the uniform mixing;
3) get 400 gram water, add the alumina sol and the 1 gram DF-568 defoamer of 100 gram solid content>5% therein; Adding 5 boron oxides, 5 that restrain less than 165 μ m then restrains less than 165 μ m boric acid, 459 aluminum oxide that restrain less than 74 μ m; Add 200 gram fluorine content at last and be 12% water fluoric resin; It is stand-by to make the surface layer coating paste behind the uniform mixing;
(2) coating method of carbon element anode oxidation resistance layer for aluminium electrolysis:
1) the carbon annode matrix is cut into the 30*30*30mm sample;
2) sample is sprayed the primer coating slurry 3 times, the timed interval of spraying is 1 hour, dries under the normal temperature;
3) sample is sprayed the barrier coating slurry 1 time, dry under the normal temperature;
4) sample is sprayed the surface layer coating paste 1 time, dry under the normal temperature and get final product;
Insulation is 1 hour when 5) sample being placed air be heated to 110 ℃ by room temperature in 70 minutes, temperature rise rate with 1.5 ℃/min is warming up to 900 ℃ then, measure to such an extent that its oxidative mass loss Δ M (%) is 18.1%, coatingsurface is complete, does not see that coatingsurface has obvious crackle; And the naked sample of carbon annode is 78.04% with its oxidative mass loss Δ M (%) under the condition.
Embodiment 2:
(1) preparation coating paste:
1) get 200 gram water, adding 200 gram solid contents therein is 10% alumina sol and 3 gram DF-568 defoamers; Add the boron oxide of 500 grams, 160 μ m, the aluminum oxide of 260 grams, 70 μ m then; Add 187 gram fluorine content at last and be 50% water fluoric resin; It is stand-by to make the primer coating slurry behind the uniform mixing;
2) get 210 gram water, adding 250 gram solid contents therein is 10% alumina sol and 5 gram CLT-371 defoamers; Add the norbide of 80 grams, 100 μ m, the boric acid of 80 grams, 100 μ m, the aluminum oxide of 130 grams, 50 μ m, the pseudo-boehmite of 145 grams, 45 μ m then; Add 100 gram fluorine content at last and be 50% water fluoric resin; It is stand-by to make the barrier coating slurry behind the uniform mixing;
3) get 220 gram water, adding 300 gram solid contents therein is 10% alumina sol and 5 gram DF-568 defoamers; The boron oxide, 40 grams, 100 μ m boric acid, 40 grams, the 50 μ m norbides, 215 that add 80 grams, 50 μ m then restrain the aluminum oxide of 50 μ m; Add 30 gram fluorine content at last and be 50% water fluoric resin; It is stand-by to make the surface layer coating paste behind the uniform mixing;
(2) coating method of carbon element anode oxidation resistance layer for aluminium electrolysis:
1) carbon annode matrix cut mechanically is become the 50*50*50mm sample;
2) sample is sprayed the primer coating slurry 2 times, the timed interval of spraying is 3 hours, dries under the normal temperature;
3) sample is sprayed the barrier coating slurry 1 time, dry under the normal temperature;
4) sample is sprayed the surface layer coating paste 2 times, the timed interval of spraying is 2 hours, dries under the normal temperature to get final product;
Insulation is 1 hour when 5) sample being placed air be heated to 110 ℃ by room temperature in 70 minutes, temperature rise rate with 1.5 ℃/min is warming up to 900 ℃ then, measure to such an extent that its oxidative mass loss/Δ M (%) is 11.3%, coatingsurface is complete, does not see that coatingsurface has obvious crackle.
Claims (10)
1, carbon element anode oxidation resistance layer for aluminium electrolysis is characterized in that: it comprises bottom anti oxidation layer, blocking layer anti oxidation layer and surface layer anti oxidation layer from the bottom to top.
2, anti oxidation layer according to claim 1 is characterized in that described bottom anti oxidation layer comprises the composition of following proportioning in weight part:
Water fluoric resin 15-45 part; Particle diameter contains boron substance 25-50 part less than 165 μ m's;
Alumina sol 1-20 part; Particle diameter is less than high-temperature anti-oxidant 1-26 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 12-40 part.
3, anti oxidation layer according to claim 1 is characterized in that described blocking layer anti oxidation layer comprises the composition of following proportioning in weight part:
Water fluoric resin 4-22 part; Particle diameter contains boron substance 1-16 part less than 165 μ m's;
Alumina sol 1-25 part; Particle diameter is less than high-temperature anti-oxidant 5-58 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 21-45 part.
4, anti oxidation layer according to claim 1 is characterized in that described surface layer anti oxidation layer comprises the composition of following proportioning in weight part:
Water fluoric resin 3-20 part; Particle diameter contains boron substance 1-16 part less than 165 μ m's;
Alumina sol 10-30 part; Particle diameter is less than high-temperature anti-oxidant 6-59 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 22-42 part.
5, according to any one described anti oxidation layer among the claim 2-4, it is characterized in that: the fluorine content of described water fluoric resin is 12-50%, and number-average molecular weight is 4 * 10
3-10 * 10
4
6, according to any one described anti oxidation layer among the claim 2-4, it is characterized in that: the described boron substance that contains is a boron oxide, or norbide, or boric acid, or any two or more mixture in them.
7, according to any one described anti oxidation layer among the claim 2-4, it is characterized in that: described high-temperature anti-oxidant is an aluminum oxide, or pseudo-boehmite, or aluminum fluoride, or any two or more mixture in them.
8, according to any one described anti oxidation layer among the claim 2-4, it is characterized in that: described defoamer is the water-based non-silicon defoamer.
9, the preparation method of carbon element anode oxidation resistance layer for aluminium electrolysis, it is characterized in that it comprises the preparation method of bottom anti oxidation layer, blocking layer anti oxidation layer and surface layer anti oxidation layer, the preparation method of described above each layer anti oxidation layer is: add alumina sol and defoamer in water, add again and contain boron substance and high-temperature anti-oxidant, add water fluoric resin at last, promptly make coating paste after mixing.
10, the coating method of carbon element anode oxidation resistance layer for aluminium electrolysis, its step is as follows:
1) spraying primer coating slurry is 2-3 time, and the timed interval of spraying is 1-3 hour, dries under the normal temperature; Described primer coating slurry comprises the composition of following proportioning in weight part:
Water fluoric resin 15-45 part; Particle diameter contains boron substance 25-50 part less than 165 μ m's;
Alumina sol 1-20 part; Particle diameter is less than high-temperature anti-oxidant 1-26 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 12-40 part;
2) spraying barrier coating slurry is 1-2 time, and the timed interval is 1-3 hour, dries under the normal temperature; Described barrier coating slurry comprises the composition of following proportioning in weight part:
Water fluoric resin 4-22 part; Particle diameter contains boron substance 1-16 part less than 165 μ m's;
Alumina sol 1-25 part; Particle diameter is less than high-temperature anti-oxidant 5-58 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 21-45 part;
3) spraying surface layer coating paste is 1-2 time, and the timed interval is 1-3 hour, dries under the normal temperature to get final product; Described surface layer coating paste comprises the composition of following proportioning in weight part:
Water fluoric resin 3-20 part; Particle diameter is for containing boron substance 1-16 part less than 165 μ m;
Alumina sol 10-30 part; Particle diameter is less than high-temperature anti-oxidant 6-59 part of 74 μ m;
Defoamer 0.1-0.5 part; Water 22-42 part.
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CN104120454A (en) * | 2014-07-01 | 2014-10-29 | 湖南创元铝业有限公司 | Prebaked anode oxidation-resistant ceramic-based coating and coating method thereof |
CN104878411A (en) * | 2015-05-25 | 2015-09-02 | 王二体 | Environment-friendly anode coating as well as preparation method and application thereof |
CN106702431A (en) * | 2015-07-24 | 2017-05-24 | 沈阳铸造研究所 | Anti-oxidation coating for carbon anodes in aluminum electrolysis |
CN106756736A (en) * | 2016-11-21 | 2017-05-31 | 中国科学院大气物理研究所 | There is the microminiature submarine of corrosion-resistant coating |
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CN104120454A (en) * | 2014-07-01 | 2014-10-29 | 湖南创元铝业有限公司 | Prebaked anode oxidation-resistant ceramic-based coating and coating method thereof |
CN104120454B (en) * | 2014-07-01 | 2016-08-17 | 湖南创元铝业有限公司 | Prebaked anode non-oxidizability ceramic base coating and painting method thereof |
CN104878411A (en) * | 2015-05-25 | 2015-09-02 | 王二体 | Environment-friendly anode coating as well as preparation method and application thereof |
CN106702431A (en) * | 2015-07-24 | 2017-05-24 | 沈阳铸造研究所 | Anti-oxidation coating for carbon anodes in aluminum electrolysis |
CN106702431B (en) * | 2015-07-24 | 2018-05-29 | 沈阳铸造研究所 | A kind of electrolytic aluminium carbon anode antioxidizing paint |
CN106756736A (en) * | 2016-11-21 | 2017-05-31 | 中国科学院大气物理研究所 | There is the microminiature submarine of corrosion-resistant coating |
CN113563056A (en) * | 2021-07-15 | 2021-10-29 | 河南和成无机新材料股份有限公司 | Coating material for high-temperature oxidation resistance of carbon anode |
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CN114100895A (en) * | 2021-10-28 | 2022-03-01 | 湖南国发控股有限公司 | Carbon electrode cooling and anti-oxidation treatment integrated control system and method |
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