CN101250722A - Carbon element anode oxidation resistance layer for aluminium electrolysis and coating method thereof - Google Patents
Carbon element anode oxidation resistance layer for aluminium electrolysis and coating method thereof Download PDFInfo
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- CN101250722A CN101250722A CNA2007100505504A CN200710050550A CN101250722A CN 101250722 A CN101250722 A CN 101250722A CN A2007100505504 A CNA2007100505504 A CN A2007100505504A CN 200710050550 A CN200710050550 A CN 200710050550A CN 101250722 A CN101250722 A CN 101250722A
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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, excellent antioxidation performance and low cost. The invention also discloses 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 coating the aluminium electrolysis used carbon anode antioxidation layer comprises following steps: firstly, spraying slurry coating of the bottom layer once or twice, wherein spraying time interval is 2 to 3 hours, drying under normal temperature, secondly, spraying the slurry coating of the barrier layer twice or three times, wherein the spraying time interval is 2 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 2 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 coating method 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 primary aluminum production cost, 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, the coefficient of thermal expansion of its coating and matrix carbon also has certain difference, and the application of its high-temperature 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 coating method of this anti oxidation layer.
A kind of 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:
Aqueous epoxy resins 30-50 part; Particle diameter be 1-5 μ m contain boron substance 15-25 part;
Alumina sol 5-20 part; Particle diameter is less than aluminum oxide 10-35 part of 75 μ m;
Defoamer 0.1-0.3 part; Water 30-50 part;
Described blocking layer anti oxidation layer comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 15-25 part; Particle diameter be 1-5 μ m contain boron substance 2-15 part;
Alumina sol 25-35 part; Particle diameter is less than aluminum oxide 30-50 part of 75 μ m;
Defoamer 0.1-0.3 part; Particle diameter is less than pseudo-boehmite 5-10 part of 20 μ m;
Water 30-50 part;
Described surface layer anti oxidation layer comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 5-15 part; Particle diameter be 1-5 μ m contain boron substance 2-20 part;
Alumina sol 10-25 part; Particle diameter is less than aluminum oxide 60-75 part of 75 μ m;
Defoamer 0.1-0.3 part; Water 30-50 part.
In the above-mentioned prescription, described aqueous epoxy resins is 0.42-0.46 in the oxirane value of 100% solid part, preferably selects the bisphenol A-type aqueous epoxy resins for use; The described boron substance that contains can be boron nitride, or boron oxide, or norbide, or boric acid, or any two or more mixture in them; Described defoamer can be the water-based non-silicon defoamer, as defoamer DF-558, or defoamer DF-568, or defoamer CLT-371 etc.; Described alumina sol is the alumina sol of solid content＞5%.
Carbon element anode oxidation resistance layer for aluminium electrolysis of the present invention, in the bottom prescription, adopt aqueous epoxy resins and contained boron substance, and add a certain amount of high temperature adhesive alumina sol and high-temperature anti-oxidant aluminum oxide, under hot environment coating can with matrix carbon generation chemical reaction, make coating produce combining of chemical bond with the matrix carbon annode, form " pricking nail " structure, thereby avoided coming off of coating and matrix effectively; And can also with CO
2Deng the micro-molecular gas reaction, reduce the discharging of greenhouse gases, increased the carbon content of coating, reduced the carbon consumption from another point of view; Adopting with the aluminum oxide in the prescription of blocking layer is main stuffing, add pseudo-boehmite, contain additive such as boron substance, effectively in the blocks air oxygen to the diffusion of matrix carbon, under the hot environment, alumina sol can form imporosity, has further stopped the diffusion of oxidizing gas; Adopting alumina sol in the surface layer prescription is main external phase, add a certain amount of boron substance that contains, contain boron substance and in hot environment, can form glass state material, be easy to flow, thereby well packing the tiny crack in the coating, further reduce the oxidizing gas internal divergence; 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 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 1-2 time, and the timed interval of spraying is 2-3 hour, dries under the normal temperature; Described primer coating slurry comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 30-50 part; Particle diameter be 1-5 μ m contain boron substance 15-25 part;
Alumina sol 5-20 part; Particle diameter is less than 75 μ m aluminum oxide 10-35 parts;
Defoamer 0.1-0.3 part; Water 30-50 part;
2) spraying barrier coating slurry is 2-3 time, and the timed interval is 2-3 hour, dries under the normal temperature; Described barrier coating slurry comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 15-25 part; Particle diameter be 1-5 μ m contain boron substance 2-15 part;
Alumina sol 25-35 part; Particle diameter is less than 75 μ m aluminum oxide 30-50 parts;
Defoamer 0.1-0.3 part; Particle diameter is less than 20 μ m pseudo-boehmite 5-10 parts;
Water 30-50 part;
3) spraying surface layer coating paste is 1-2 time, and the timed interval is 2-3 hour, dries under the normal temperature to get final product; Described surface layer coating paste comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 5-15 part; Particle diameter be 1-5 μ m contain boron substance 2-20 part;
Alumina sol 10-25 part; Particle diameter is less than 75 μ m aluminum oxide 60-75 parts;
Defoamer 0.1-0.3 part; Water 30-50 part.
In the aforesaid method, the preparation of described coating paste is that the raw material that will take by weighing by prescription mixes at normal temperatures and gets final product; Described aqueous epoxy resins is 0.42-0.46 in the oxirane value of 100% solid part, preferably selects bisphenol A type epoxy resin for use; The described boron substance that contains can be boron nitride, or boron oxide, or norbide, or boric acid, or any two or more mixture in them; Described defoamer can be the water-based non-silicon defoamer, as defoamer DF-558, or defoamer DF-568, or defoamer CLT-371 etc.; Described alumina sol is the alumina sol of solid content＞5%; The average coated weight of described whole anti oxidation layer is preferably in 0.03-0.10g/cm
2In.
Carbon element anode oxidation resistance layer for aluminium electrolysis of the present invention is good with the carbon annode matrix bond, have a good gradient antioxidant property, 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 used and contained boron substance and combine with aqueous epoxy resins, improved the bonding strength of coating and carbon annode matrix, made coating more firm with combining of matrix; Wherein, the low-melting boron substance that contains, when fusion, not only wet the carbon annode matrix simultaneously but also adherent coating, 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, have certain fluidity, but the crackle that produces in the packing coating is wetting well and cover the carbon annode surface, make coating have certain self-healing ability, better stop the invasion of oxygen; 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 of the present invention adopts spraying coating process to form the three-layer sandwich type structure with gradient anti-oxidant function on the carbon annode matrix, not only can overcome the defective of single layer structure coating, relaxation heat stress, can also strengthen the heat-shock resistance of coating, thereby make coating in long-time, bring into play antioxygenation preferably.
(4) embodiment:
Embodiment 1
(1) preparation coating paste:
1) aluminum oxide, 150 gram solid contents that takes by weighing norbides, 350 grams, the 70 μ m of 400 gram water, 300 gram bisphenol A-type aqueous epoxy resins, 200 grams, 3 μ m be greater than 5% alumina sol and 1.5 gram DF-568 defoamers, mixes under the normal temperature that to be prepared into the primer coating slurry stand-by;
2) pseudo-boehmite, 250 gram solid contents that takes by weighing aluminum oxide, 100 grams, the 10 μ m of boric acid, 450 grams, the 70 μ m of boron oxides, 30 grams, the 3 μ m of 500 gram water, 150 gram bisphenol A-type aqueous epoxy resins, 20 grams, 3 μ m be greater than 5% alumina sol and 2 gram DF-568 defoamers, mixes under the normal temperature that to be prepared into the barrier coating slurry stand-by;
3) aluminum oxide, 240 gram solid contents that takes by weighing norbide, 650 grams, the 70 μ m of boron oxides, 20 grams, the 3 μ m of 300 gram water, 50 gram bisphenol A-type aqueous epoxy resins, 40 grams, 3 μ m be greater than 5% alumina sol and 2 gram DF-568 defoamers, mixes under the normal temperature that to be prepared into the surface layer coating paste stand-by;
(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 2 hours, dries under the normal temperature;
3) sample is sprayed the barrier coating slurry 3 times, the timed interval of spraying is 2 hours, dries under the normal temperature;
4) sample is sprayed the surface layer coating paste 1 time, dry under the normal temperature and get final product;
5) the average coated weight of this sample is 0.05g/cm
2, being placed on that the temperature rise rate with 1 ℃/min rises to 940 ℃ by 25 ℃ in the air, its oxidative mass loss Δ M (%) is 6.1%; And be 75% with its oxidative mass loss Δ M (%) under the condition with the naked sample of carbon annode.
Embodiment 2:
(1) preparation coating paste:
1) norbides, the boron oxide of 100 grams, 1 μ m, the aluminum oxide of 300 grams, 20 μ m, the 50 gram solid contents that take by weighing 500 gram water, 500 gram bisphenol A-type aqueous epoxy resins, 50 grams, 5 μ m are 10% alumina sol and 1.5 gram DF-558 defoamers, mix under the normal temperature that to be prepared into the primer coating slurry stand-by;
2) boron oxides, the aluminum oxide of 350 grams, 50 μ m, the pseudo-boehmite of 100 grams, 15 μ m, the 250 gram solid contents that take by weighing 500 gram water, 200 gram bisphenol A-type aqueous epoxy resins, 100 grams, 2 μ m are 10% alumina sol and 2 gram DF-558 defoamers, mix under the normal temperature that to be prepared into the barrier coating slurry stand-by;
3) boric acid, the aluminum oxide of 750 grams, 10 μ m, the 180 gram solid contents that take by weighing 300 gram water, 50 gram bisphenol A-type aqueous epoxy resins, 20 grams, 1 μ m are 10% alumina sol and 3 gram DF-568 defoamers, mix under the normal temperature that to be prepared into the surface layer coating paste stand-by;
(2) coating method of carbon element anode oxidation resistance layer for aluminium electrolysis:
1) carbon annode matrix cut mechanically is become the 60*60*60mm sample;
2) sample is sprayed the primer coating slurry 1 time, dry under the normal temperature;
3) sample is sprayed the barrier coating slurry 2 times, the timed interval of spraying is 2 hours, dries under the normal temperature;
4) sample is sprayed the surface layer coating paste 2 times, the timed interval of spraying is 3 hours, dries under the normal temperature to get final product;
5) the average coated weight of this sample is 0.08g/cm
2, dried this sample is directly put into 900 ℃ High Temperature Furnaces Heating Apparatus, being incubated and recording its oxidative mass loss Δ M (%) after 10 hours is 20.1%, coatingsurface is complete, does not see that coatingsurface has obvious crackle.
Embodiment 3
(1) preparation coating paste:
1) norbides, the boron oxide of 50 grams, 3 μ m, 100 grams, 5 μ m boric acid, the aluminum oxide of 150 grams, 25 μ m, the 20 gram solid contents that take by weighing 400 gram water, 400 gram bisphenol A-type aqueous epoxy resins, 100 grams, 3 μ m are 6% alumina sol and 1 gram CLT-371 defoamer, mix under the normal temperature that to be prepared into the primer coating slurry stand-by;
2) norbides, the aluminum oxide of 500 grams, 30 μ m, the pseudo-boehmite of 50 grams, 8 μ m, the 250 gram solid contents that take by weighing 300 gram water, 170 gram bisphenol A-type aqueous epoxy resins, 30 grams, 4 μ m are 6% alumina sol and 2 gram DF-558 defoamers, mix under the normal temperature that to be prepared into the barrier coating slurry stand-by;
3) boron oxides, the aluminum oxide of 650 grams, 10 μ m, the 150 gram solid contents that take by weighing 300 gram water, 150 gram bisphenol A-type aqueous epoxy resins, 50 grams, 5 μ m are 6% alumina sol and 2 gram CLT-371 defoamers, mix under the normal temperature that to be prepared into the surface layer coating paste stand-by;
(2) coating method of carbon element anode oxidation resistance layer for aluminium electrolysis:
1) carbon annode matrix cut mechanically is become the 75*75*75mm sample;
2) sample is sprayed the primer coating slurry 1 time, dry under the normal temperature;
3) sample is sprayed the barrier coating slurry 3 times, the timed interval of spraying is 2 hours, dries under the normal temperature;
4) sample is sprayed the surface layer coating paste 1 time, dry under the normal temperature and get final product;
5) the average coated weight of this sample is 0.12g/cm
2, it is carried out 8 oxidative mass loss Δ M (%) after the thermal shock resistance experiment is 2.7%;
Described thermal shock experiment is for to be rapidly heated 900 ℃ with sample by 30 ℃ of beginnings in 20min, and is incubated 20min in 900 ℃, again fast cooling to 30 ℃.
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:
Aqueous epoxy resins 30-50 part; Particle diameter be 1-5 μ m contain boron substance 15-25 part;
Alumina sol 5-20 part; Particle diameter is less than aluminum oxide 10-35 part of 75 μ m;
Defoamer 0.1-0.3 part; Water 30-50 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:
Aqueous epoxy resins 15-25 part; Particle diameter be 1-5 μ m contain boron substance 2-15 part;
Alumina sol 25-35 part; Particle diameter is less than aluminum oxide 30-50 part of 75 μ m;
Defoamer 0.1-0.3 part; Particle diameter is less than pseudo-boehmite 5-10 part of 20 μ m;
Water 30-50 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:
Aqueous epoxy resins 5-15 part; Particle diameter be 1-5 μ m contain boron substance 2-20 part;
Alumina sol 10-25 part; Particle diameter is less than aluminum oxide 60-75 part of 75 μ m;
Defoamer 0.1-0.3 part; Water 30-50 part.
5, according to any one described anti oxidation layer among the claim 2-4, it is characterized in that: described aqueous epoxy resins is 0.42-0.46 in the oxirane value of 100% solid part.
6, anti oxidation layer according to claim 5 is characterized in that: described aqueous epoxy resins is the bisphenol A-type aqueous epoxy resins.
7, 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 nitride, or boron oxide, or norbide, or boric acid, 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, according to any one described anti oxidation layer among the claim 2-4, it is characterized in that: described alumina sol is the alumina sol of solid content＞5%.
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 1-2 time, and the timed interval of spraying is 2-3 hour, dries under the normal temperature; Described primer coating slurry comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 30-50 part; Particle diameter be 1-5 μ m contain boron substance 15-25 part;
Alumina sol 5-20 part; Particle diameter is less than 75 μ m aluminum oxide 10-35 parts;
Defoamer 0.1-0.3 part; Water 30-50 part;
2) spraying barrier coating slurry is 2-3 time, and the timed interval is 2-3 hour, dries under the normal temperature; Described barrier coating slurry comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 15-25 part; Particle diameter be 1-5 μ m contain boron substance 2-15 part;
Alumina sol 25-35 part; Particle diameter is less than 75 μ m aluminum oxide 30-50 parts;
Defoamer 0.1-0.3 part; Particle diameter is less than 20 μ m pseudo-boehmite 5-10 parts;
Water 30-50 part;
3) spraying surface layer coating paste is 1-2 time, and the timed interval is 2-3 hour, dries under the normal temperature to get final product; Described surface layer coating paste comprises the composition of following proportioning in weight part:
Aqueous epoxy resins 5-15 part; Particle diameter be 1-5 μ m contain boron substance 2-20 part;
Alumina sol 10-25 part; Particle diameter is less than 75 μ m aluminum oxide 60-75 parts;
Defoamer 0.1-0.3 part; Water 30-50 part.
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| CN200710050550A CN100580144C (en) | 2007-11-16 | 2007-11-16 | Carbon element anode oxidation resistance layer for aluminium electrolysis and coating method thereof |
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| CN100580144C CN100580144C (en) | 2010-01-13 |
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Cited By (6)
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| CN103132104A (en) * | 2013-03-07 | 2013-06-05 | 沈阳化工大学 | Method for protecting electrolytic aluminum by using carbon anode |
| CN103741167A (en) * | 2013-12-25 | 2014-04-23 | 中国矿业大学 | Method for improving oxidization resistance of carbon anode for electrolyzing aluminum |
| CN104047031A (en) * | 2014-07-03 | 2014-09-17 | 四川华索自动化信息工程有限公司 | Water-cooling coil pipe type integral cast aluminum anode for aluminum electrolysis |
| 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 |
| CN106189600A (en) * | 2016-08-15 | 2016-12-07 | 昌吉州准东经济技术开发区唯新能源科技有限公司 | Electrolytic aluminium carbon anode surface high temperature resistance antioxidant coating and preparation method thereof |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE543739A (en) * | 1954-12-31 |
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2007
- 2007-11-16 CN CN200710050550A patent/CN100580144C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103132104A (en) * | 2013-03-07 | 2013-06-05 | 沈阳化工大学 | Method for protecting electrolytic aluminum by using carbon anode |
| CN103132104B (en) * | 2013-03-07 | 2016-08-03 | 沈阳化工大学 | Method with carbon anode protection electrolytic aluminium |
| CN103741167A (en) * | 2013-12-25 | 2014-04-23 | 中国矿业大学 | Method for improving oxidization resistance of carbon anode for electrolyzing aluminum |
| 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 |
| CN104047031A (en) * | 2014-07-03 | 2014-09-17 | 四川华索自动化信息工程有限公司 | Water-cooling coil pipe type integral cast aluminum anode for aluminum electrolysis |
| CN106189600A (en) * | 2016-08-15 | 2016-12-07 | 昌吉州准东经济技术开发区唯新能源科技有限公司 | Electrolytic aluminium carbon anode surface high temperature resistance antioxidant coating and preparation method thereof |
| 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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