CN103194101A - Titanium boride-based coating composite material for aluminum electrolysis, preparation method and coating method thereof - Google Patents
Titanium boride-based coating composite material for aluminum electrolysis, preparation method and coating method thereof Download PDFInfo
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Abstract
The invention discloses a titanium boride-based coating composite material for aluminum electrolysis, a preparation method and a coating method thereof. The composite material consists of the following raw materials in percentage by weight: 55%-70% of titanium boride-oxide composite particles, 8%-15% of a carbon additive, 15%-30% of an organic resin adhesive and 0.5%-2% of a reinforcing agent. The coating method comprises the following steps: (1) putting a graphite base material into a coating mould, and then, pouring the obtained slurry into a mould; (2) curing the base material coated with the slurry at 15 DEG C-35 DEG C for 24h-48h, and then, curing the base material at 80 DEG C-150 DEG C for 12h-24h; and (3) putting the base material coated with the slurry into a graphite crucible, filling graphite carbon powder into the graphite crucible, and carbonizing and sintering the graphite crucible in an inert gas atmosphere or in vacuum, wherein the carbonizing and sintering temperature is 850-1050 DEG C, and the carbonizing and sintering time is 80-120 hours. The titanium boride-based coating composite material for aluminum electrolysis has high combination degree with a base and good tensile strength high up to 8-10MPa; and a coating structure is dense and has strong anti-scouring property.
Description
Technical fieldThe present invention relates to electrochemical field, be specifically related to a kind of noble electrode used for aluminium electrolysis negative electrode titanium boride based composites and technology of preparing thereof of being applicable to.
Background technology
Cathode material in the aluminum electrolyzation technology not only will carry electric action, also to bear the chemical erosion of high temperature cryolite melts and the physics erosion of aluminium liquid, aluminium cell of the prior art generally all adopts the carbonaceous cathodes material, because its relatively poor electrolyte-resistant penetrating quality and not good with aluminum-liquid wetting has had a strong impact on the efficient stable operation of electrolyzer.Titanium boride is owing to the conductivity with excellence, easily wetting by molten metals such as aluminium, and good corrosion-resistant and high-temperature oxidation resistance, therefore becomes the preferred material of making used for aluminium electrolysis wettability inert cathode.The component that patent CN1537975 introduces titanium boride/aluminum oxide cathode and constitutes coating wherein adopts TiB in this coating
2/ Al
2O
3Matrix material replaces pure TiB
2Component has influenced conductivity and its stability.Patent CN101914786 has introduced a kind of technology of preparing and paint-on technique of coating paste, and this technology can realize coating in the even distribution on carbon base body surface, but coat-thickness is thinner, is difficult to tolerate for a long time aluminium liquid and washes away.At present, the wettable cathode material of using in Aluminium Electrolysis is mainly obtained by coating paint-on technique, vibratory compaction and heat pressing process.And it is the most commonly used in Aluminium Electrolysis based on the coating paint-on technique of manual application mode.Patent US5651874, CN1448542, CN1405358 and CN1537974 have introduced the preparation method of a kind of electrolysis of aluminum titanium boride-C cathode material coating, this method is that thermosetting resin etc. is mixed with into high thick thickener with powders of titanium boride, is painted on aluminium cell carbon cathode surface by hand.Patent US6436250B1, US5728466 have introduced sol-gel processing and have prepared titanium boride-MO coating technology (MO represents metal oxide), have improved the bonding force of electroconductibility and coating and matrix greatly.There is certain deficiency but adopt the manual brushing method to construct, as: (1) productivity is low, labour intensity is big; (2) coat-thickness heterogeneity, surface irregularity, unfairness; (3) brush applied coating is thicker, makes at the electrolyzer electrical roasting, is subjected to thermal shock effect big when starting, and coefficient of thermal expansion mismatch causes the thermal stresses inequality, finally causes early stage the coming off of coating.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at prior art, provide a kind of can solve and carbon basal body between possess good thermal expansion matching, anti-sodium potassium expands,, refractory wetting with aluminium liquid height melts ionogen and ooze erosion and the erosion of aluminium liquid, high conduction and low-cost, easy working used for aluminium electrolysis titanium boride base coating composite material, and the present invention will provide the preparation method of this matrix material and simultaneously with the coating method of this material.
The objective of the invention is to be achieved through the following technical solutions:
A kind of used for aluminium electrolysis titanium boride base coating composite material, formed by following raw material by weight percentage:
Titanium boride-oxide composite particle: 55% ~ 70%; Carbonaceous additive: 8% ~ 15%; Organic resin glue: 15% ~ 30%; Toughener: 0.5% ~ 2%.
Described titanium boride-oxide composite particle is mixed by 60% ~ 90% titanium boride and 10% ~ 40% oxide sol by weight percentage, and described oxide sol solid content is 5% ~ 30%.
Described oxide sol is at least a in alumina sol, magnesium oxide colloidal sol, titanium oxide sol, zinc oxide colloidal sol or the silica sol.
The carbonaceous additive is at least a in graphite, refinery coke or the electric calcined anthracite.
Described organic resin glue is made up of binding agent, dispersion agent, solidifying agent; The quality percentage composition of each component is respectively binding agent 35% ~ 58%, dispersion agent 40% ~ 64%, solidifying agent 1% ~ 5%.
Described binding agent is at least a in pitch, furane resin, resol, Resins, epoxy or the furfuryl resin; Dispersion agent is at least a in acetone, butanone, ethanol or the butylacetate; Solidifying agent is at least a in tosic acid, polyamide resin, m-xylene diamine, hexamethylenetetramine, trimethylhexamethylenediamine, diethyl amino propylamine, quadrol or the diethylenetriamine.
Described toughener is at least a in carbon fiber, silicon carbide fiber, sapphire whisker, Zirconium oxide fibre or the titanium carbide.
Prepare the method for above-mentioned titanium boride base coating composite material, may further comprise the steps:
At first prepare titanium boride-oxide composite particle, the proportioning by above-mentioned titanium boride and oxide sol stirs titanium boride and oxide sol, obtains through the broken 100-150 mesh sieve of crossing after 700 ~ 1000 ℃ of calcinings;
Press the proportioning raw materials of above-mentioned titanium boride base coating composite material, titanium boride-oxide composite particle, carbonaceous additive, organic resin glue, toughener are mixed pinch stirring, obtain applying slurry; Kneading temperature is 15 ℃ ~ 35 ℃, and relative humidity is 30% ~ 90% in the air, and mixing the time of pinching is 2 ~ 6h.
Coating method with above-mentioned titanium boride base coating composite material may further comprise the steps:
(1) applies, graphite substrate material is put into the coating mould, the distance at graphite substrate material upper surface and mould edge suitable for reading, and the graphite substrate material surrounded surface is consistent with the gap size between the mold wall, then the above-mentioned slurry that obtains is poured in the mould;
(2) solidify, with the body material that is coated with slurry at 15 ℃ ~ 35 ℃ solidification treatment 24h ~ 48h, and then at 80 ℃ ~ 150 ℃ solidification treatment 12h ~ 24h;
(3) charing sintering, the body material that step (2) is coated with slurry places plumbago crucible, and landfill graphite carbon dust carries out the charing sintering then in inert gas atmosphere or in the vacuum; Described charing sintering temperature is 850 ~ 1050 ℃, and the charing sintering time is 80h ~ 120h.
The described rare gas element of step (3) is that Ar is or/and N
2O in the described inert gas atmosphere or in the vacuum
2Content is controlled to be 10ppm ~ 50ppm; Described vacuum is 10
-1Pa.
The present invention compared with prior art has following obvious advantage:
A kind of used for aluminium electrolysis titanium boride base coating composite material of the present invention, the titanium boride composition profiles is reasonable, void content is low, has effectively stoped electrolytical infiltration, and can form uniform aluminium liquid film on the surface; Coated material and matrix bond degree height, tensile strength can reach 8-10MPa; Coating structure densification, erosion resistibility are strong.Owing to the sintering aid that adds, effectively reduced the sintering temperature of matrix material, manufacturing cost is far below heat pressing process.
Adopt mould control brushing process among the present invention, make coating processes can realize automatization, controlled, the homogeneous of coat-thickness is controlled planeness, the smooth finish of coatingsurface effectively.
Embodiment
Embodiment 1
At first prepare solid content and be 5% titanium oxide sol (also can directly buy from market), then 70% titanium boride (median size 5 ~ 10 μ m) and 30% titanium oxide sol are mixed, under 700 ℃, carry out calcination processing again, then will calcine the broken 100-150 of the mistake sieve of back material, obtain titanium boride-titanium oxide composite particles powder.With 55% titanium boride-titanium oxide composite particles, 8% Graphite Powder 99 (particle diameter is 10-150), 5% refinery coke (40-50 μ m), 7% furane resin, 3.5% Resins, epoxy, 10% ethanol, 5.2% butanone, 4% butylacetate, 0.3% polyamide resin, 1% sapphire whisker, 1% titanium carbide place to mix to pinch in the pot and stir, kneading temperature is 15 ℃, relative humidity is 30% in the air, mixing the time of pinching is 5h, obtains applying slurry.The slurry that mixes after pinching is coated on the graphite substrate material surface, applies operation according to the following steps: in the coating mould of will coated body material packing into, one of body material facing to mould openings, is provided with the gap between remaining four face and the mould.Body material is facing to this one side of mould openings and the distance at mould mouth edge, and the gap width between remaining four face and the mould, is coat-thickness.In mould, pour the above-mentioned slurry that obtains into, concordant with mould mouth edge until slurry.After slurry was poured into, available flat board was scraped along mould mouth edge, and is concordant with mould mouth edge to guarantee slurry, gets final product the demoulding in 2-5 minute.Graphite substrate material after the demoulding is at 20 ℃ of following isothermal curing 24h, then at 80 ℃ of following isothermal curing 12h, be placed on again and put into electric furnace in the plumbago crucible, landfill graphite carbon dust, in rare gas element Ar atmosphere, carry out the charing sintering then, the charing sintering temperature is 900 ℃, and the charing sintering time is 80h, and the oxygen level in the inert gas atmosphere is 50ppm.
Obtaining resistivity is the sample of 29 μ Ω m.
Embodiment 2
At first prepare solid content and be 15% alumina sol, then 60% titanium boride and 40% alumina sol are mixed, under 1000 ℃, carry out calcination processing at last, then will calcine the broken 100-150 of mistake of back material mesh sieve and obtain titanium boride-aluminum oxide composite particles powder.With 70% titanium boride-aluminum oxide composite particles, 5% Graphite Powder 99 (particle diameter is 10-150 μ m), 3% electric calcined anthracite (particle diameter is 100-150 μ m), 6% pitch (150-200 μ m), 4% resol, 1.6% furfuryl resin, 4% ethanol, 3% acetone, 1% butylacetate, 0.4% tosic acid, 2% carbon fiber places to mix to pinch in the pot and stirs, kneading temperature is 25 ℃, relative humidity is 50% in the air, mixing the time of pinching is 6h, obtains applying slurry.The slurry that mixes after pinching is coated on the graphite substrate material surface, at 25 ℃ of following isothermal curing 48h, then at 150 ℃ of following isothermal curing 24h, be placed on again and put into electric furnace in the plumbago crucible, landfill graphite carbon dust carries out the charing sintering then in rare gas element Ar atmosphere, the charing sintering temperature is 950 ℃, the charing sintering time is 100h, and the oxygen level in the inert gas atmosphere is 10ppm.
Obtaining resistivity is the sample of 38 μ Ω m.
All the other are implemented as embodiment 1.
Embodiment 3
At first prepare solid content and be 30% silica sol, then 90% titanium boride and 10% silica sol are mixed, under 900 ℃, carry out calcination processing at last, then will calcine the broken 100-150 of mistake of back material mesh sieve and obtain titanium boride-silicon oxide composite particles powder.With 65% titanium boride-silicon oxide composite particles, 9.5% electric calcined anthracite (particle diameter is 100-150 μ m), 5% pitch (particle diameter is 150-200 μ m), 3% resol, 2% Resins, epoxy, 5.5% ethanol, 9% acetone, 0.5% quadrol, 0.5% silicon carbide fiber places to mix to pinch in the pot and stirs, kneading temperature is 35 ℃, relative humidity is 70% in the air, mixing the time of pinching is 2h, obtains applying slurry; The slurry that mixes after pinching is coated on the graphite substrate material surface, at 35 ℃ of following isothermal curing 30h, at 90 ℃ of following isothermal curing 12h, is placed on and puts into electric furnace in the plumbago crucible then, landfill graphite carbon dust is then at rare gas element N
2Can be arbitrary proportion with Ar(, both mix with 1:1 in the present embodiment) carry out the charing sintering in the atmosphere, the charing sintering temperature is 1050 ℃, and the charing sintering time is 90h, and the oxygen level in the inert gas atmosphere is 30ppm.
Obtain the sample that resistivity is 48 Ω cm.
All the other are implemented as embodiment 1.
Embodiment 4
At first prepare solid content and be 20% magnesium oxide colloidal sol, then 80% titanium boride and 20% magnesium oxide colloidal sol are mixed, under 880 ℃, carry out calcination processing at last, then will calcine the broken 100-150 of mistake of back material mesh sieve and obtain titanium boride-magnesium oxide composite particles powder.With 58.5% titanium boride-magnesium oxide composite particles, 8.5% graphite (particle diameter is 10-150 μ m), 6.5% refinery coke (particle diameter is 40-50 μ m), 8% pitch (particle diameter is 10-150 μ m), 4.5% resol, 6.5% ethanol, 3% butanone, 2.6% butylacetate, 0.4% diethylenetriamine, 1.5% Zirconium oxide fibre places to mix to pinch in the pot and stirs, and kneading temperature is 30 ℃, and relative humidity is 70% in the air, mixing the time of pinching is 2h, obtains applying slurry; The slurry that mixes after pinching is coated on the graphite substrate material surface, at 35 ℃ of following isothermal curing 30h, at 90 ℃ of following isothermal curing 12h, is placed on and puts into electric furnace in the plumbago crucible then, landfill graphite carbon dust is then at rare gas element N
2Carry out the charing sintering in the atmosphere, the charing sintering temperature is 980 ℃, and the charing sintering time is 90h, and the oxygen level in the inert gas atmosphere is 20ppm.
Obtaining resistivity is the sample of 26 μ Ω m.
All the other are implemented as embodiment 1.
Embodiment 5
At first prepare solid content and be 18% zinc oxide colloidal sol, then 75% titanium boride and 25% zinc oxide colloidal sol are mixed, under 900 ℃, carry out calcination processing again, then will calcine the broken 100-150 of mistake of back material mesh sieve and obtain titanium boride-zinc oxide composite particles powder.With 66.8% titanium boride-zinc oxide composite particles, 8% graphite (particle diameter 10-150 μ m), 3% refinery coke (40-50 μ m), 3% electric calcined anthracite (100-150 μ m), 5% Resins, epoxy, 4% resol, 4.5% ethanol, 2.5% butanone, 1.1% butylacetate, 5% m-xylene diamine, 1.2% sapphire whisker place to mix to pinch in the pot and stir, kneading temperature is 30 ℃, relative humidity is 50% in the air, and mixing the time of pinching is 4h, obtains applying slurry; The slurry that mixes after pinching is coated on the graphite substrate material surface, at 30 ℃ of following isothermal curing 30h, at 90 ℃ of following isothermal curing 12h, is placed on again and puts into electric furnace in the plumbago crucible then, landfill graphite carbon dust, (vacuum tightness is 10 in vacuum then
-1Pa) carry out the charing sintering in the atmosphere, the charing sintering temperature is 850 ℃, and the charing sintering time is 90h.
Obtaining resistivity is the sample of 35 μ Ω m.
All the other are implemented as embodiment 1.
Claims (10)
1. used for aluminium electrolysis titanium boride base coating composite material is characterized in that being made up of following raw material by weight percentage:
Titanium boride-oxide composite particle: 55% ~ 70%; Carbonaceous additive: 8% ~ 15%; Organic resin glue: 15% ~ 30%; Toughener: 0.5% ~ 2%.
2. a kind of used for aluminium electrolysis titanium boride base coating composite material according to claim 1, it is characterized in that: described titanium boride-oxide composite particle, mixed by 60% ~ 90% titanium boride and 10% ~ 40% oxide sol by weight percentage, described oxide sol solid content is 5% ~ 30%.
3. a kind of used for aluminium electrolysis titanium boride base coating composite material according to claim 2 is characterized in that: described oxide sol is at least a in alumina sol, magnesium oxide colloidal sol, titanium oxide sol, zinc oxide colloidal sol or the silica sol.
4. a kind of used for aluminium electrolysis titanium boride base coating composite material according to claim 1 is characterized in that: the carbonaceous additive is at least a in graphite, refinery coke or the electric calcined anthracite.
5. a kind of used for aluminium electrolysis titanium boride base coating composite material according to claim 1, it is characterized in that: described organic resin glue is made up of binding agent, dispersion agent, solidifying agent; The quality percentage composition of each component is respectively binding agent 35% ~ 58%, dispersion agent 40% ~ 64%, solidifying agent 1% ~ 5%.
6. a kind of used for aluminium electrolysis titanium boride base coating composite material according to claim 5 is characterized in that: described binding agent is at least a in pitch, furane resin, resol, Resins, epoxy or the furfuryl resin;
Dispersion agent is at least a in acetone, butanone, ethanol or the butylacetate;
Solidifying agent is at least a in tosic acid, polyamide resin, m-xylene diamine, hexamethylenetetramine, trimethylhexamethylenediamine, diethyl amino propylamine, quadrol or the diethylenetriamine.
7. a kind of used for aluminium electrolysis titanium boride base coating composite material according to claim 1 is characterized in that: toughener is at least a in carbon fiber, silicon carbide fiber, sapphire whisker, Zirconium oxide fibre or the titanium carbide.
8. prepare the method for the described titanium boride base of claim 1 coating composite material, it is characterized in that may further comprise the steps:
At first prepare titanium boride-oxide composite particle, by the described proportioning of claim 2, titanium boride and oxide sol are stirred, obtain through the broken 100-150 mesh sieve of crossing after 700 ~ 1000 ℃ of calcinings;
Press the described proportion of raw materials of claim 1, titanium boride-oxide composite particle, carbonaceous additive, organic resin glue, toughener are mixed pinch stirring, obtain applying slurry; Kneading temperature is 15 ℃ ~ 35 ℃, and relative humidity is 30% ~ 90% in the air, and mixing the time of pinching is 2 ~ 6h.
9. prepare the method for coating with the described titanium boride based composites of claim 8, it is characterized in that may further comprise the steps:
(1) applies, graphite substrate material is put into the coating mould, the distance at graphite substrate material upper surface and mould edge suitable for reading, and the graphite substrate material surrounded surface is consistent with the gap size between the mold wall, the slurry that claim 8 is obtained is poured in the mould then;
(2) solidify, with the graphite substrate material that is coated with pulp layer at 15 ℃ ~ 35 ℃ solidification treatment 24h ~ 48h, and then at 80 ℃ ~ 150 ℃ solidification treatment 12h ~ 24h;
(3) charing sintering, the graphite substrate material that step (2) is coated with pulp layer places plumbago crucible, and landfill graphite carbon dust carries out the charing sintering then in inert gas atmosphere or in the vacuum; Described charing sintering temperature is 850 ~ 1050 ℃, and the charing sintering time is 80h ~ 120h.
10. titanium boride based composites according to claim 9 prepares the method for coating, it is characterized in that: the described rare gas element of step (3) is that Ar is or/and N
2O in the described inert gas atmosphere or in the vacuum
2Content is controlled to be 10ppm ~ 50ppm; Described vacuum≤10
-1Pa.
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| CN103468134A (en) * | 2013-08-14 | 2013-12-25 | 苏州康华净化系统工程有限公司 | Gum rosin-containing waterproof antistatic aluminium alloy coating |
| CN103668331A (en) * | 2013-11-29 | 2014-03-26 | 云南云铝润鑫铝业有限公司 | Method for effectively prolonging service life of aluminum electrolytic tank |
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| CN106435644A (en) * | 2016-12-05 | 2017-02-22 | 中南大学 | Tamping paste for aluminum electrolytic cell and use method of tamping paste |
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| CN113185856B (en) * | 2021-04-25 | 2024-04-09 | 仲恺农业工程学院 | Preparation method and application of coating material for oil sludge cracking treatment |
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| CN114134539B (en) * | 2021-11-05 | 2024-09-27 | 新疆农六师碳素有限公司 | Special coating material for aluminum carbon production line and preparation method thereof |
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Effective date of registration: 20170105 Address after: 100082 Beijing, Xizhimen, North Street, No. 62, No. Patentee after: Aluminum Corporation of China Limited Address before: 223005 Haikou Road, Huaian Economic Development Zone, Jiangsu, No. 9 Patentee before: Jiangsu United Ceralloy Materials Technologies Co., Ltd. |