CN100366800C - Preparation method of TiB2 composite layer cathode carbon block - Google Patents
Preparation method of TiB2 composite layer cathode carbon block Download PDFInfo
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- CN100366800C CN100366800C CNB2004101009777A CN200410100977A CN100366800C CN 100366800 C CN100366800 C CN 100366800C CN B2004101009777 A CNB2004101009777 A CN B2004101009777A CN 200410100977 A CN200410100977 A CN 200410100977A CN 100366800 C CN100366800 C CN 100366800C
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- tib
- cathode carbon
- carbon block
- graphite
- composite
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 14
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 title abstract 5
- 229910033181 TiB2 Inorganic materials 0.000 title abstract 5
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000010439 graphite Substances 0.000 claims abstract description 21
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims description 18
- 239000011159 matrix material Substances 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000002562 thickening agent Substances 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 8
- 239000011294 coal tar pitch Substances 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005087 graphitization Methods 0.000 claims description 3
- 239000011295 pitch Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229920006332 epoxy adhesive Polymers 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 15
- 239000004411 aluminium Substances 0.000 abstract description 12
- 229910052708 sodium Inorganic materials 0.000 abstract description 5
- 239000011734 sodium Substances 0.000 abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 4
- 239000010406 cathode material Substances 0.000 abstract description 4
- 239000003792 electrolyte Substances 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000007767 bonding agent Substances 0.000 abstract 1
- 239000010424 alunite Substances 0.000 description 9
- 229910052934 alunite Inorganic materials 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 239000007788 liquid Substances 0.000 description 8
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 description 8
- 239000003610 charcoal Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 241000761003 Rastellus Species 0.000 description 2
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 description 2
- 239000003830 anthracite Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 208000002599 Smear Layer Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 alunite compound Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Electrolytic Production Of Metals (AREA)
Abstract
The present invention relates to a method for preparing a cathode carbon block with a TiB2 composite layer, which relates to a method for preparing a cathode material carbon block for large-sized aluminium cells, particularly to a method for preparing a TiB2-graphite composite cathode carbon block. The method of the present invention is characterized in that 20 to 70% of TiB2 powder, 15 to 17% of bonding agent and graphite scraps as the rest are mixed according to mass ratio to be prepared into TiB2 composite layer paste, the composite paste is added on a base block of the prepared cathode carbon block until the forming work is finished, the base block and the composite paste are integrally calcined, and a TiB [2]-graphite scrap composite cathode carbon block is prepared. The cathode carbon block with a TiB2 composite layer, which is prepared by the method of the present invention, has the advantage that the sodium aspiration quantity of cathodes is obviously reduced during the high sodium aspiration period when an electrolytic tank is primarily started. The lowering speed of the molecular ratio of electrolytes is only 30% of that of a contrast tank. The electrolytic tank has the advantages of stabile operation, clean tank bottom and no precipitation. Compared with the contrast tank, the electrolytic tank has the advantages that the cathode drop is reduced by 60 mv to 80 mv, the DC power consumption of primary aluminium is reduced by 100 Kwh/t. A to 200 Kwh/t. A, and the service life of the tank is predicted to be improved by 400 days to 600 days.
Description
Technical field
A kind of TiB
2The composite layer cathode carbon block preparation method relates to a kind of preparation, particularly TiB that is used for the cathode material charcoal piece of large-scale aluminum electrolytic cell
2The preparation method of-graphite composite cathode carbon piece.
Background technology
In the Aluminium Electrolysis process, because the sodium that electrochemical reaction generates in the reaction of aluminium liquid and negative electrode carbon and the ionogen is to the osmosis of charcoal lattice, cause phenomenons such as charcoal cathode expansion, protuberance, spalling, make ionogen liquation seepage, pot shell distortion, the electrolyzer early damage appears, shorten the life-span of electrolyzer, be forced to overhaul.TiB
2It is the good wettable material of metallic aluminium, forming the layer of aluminum liquid film behind the aluminium liquid covered cathode can effectively isolate ionogen and contact with the direct of bottom charcoal, stoped the anticathode erosion of ionogen, this composite bed and have anti-sodium perviousness and good electroconductibility is an ideal aluminium electrolytic cell cathode material.But TiB
2The cost costliness, too high and be difficult to bear with the charcoal negative electrode cost that replaces electrolyzer, so people just attempt the way with coating, by smearing TiB at cathode surface
2The way of coating makes TiB
2Coating charcoal piece.Last century, 80-90 age people once tested for this reason.But this smear layer since with the qualitative difference of carbon matrix piece, too thick being difficult to forms stable one, easily comes off; Too thin difficult antiscour or inoperative so all do not get an expected result, has no resolution and end in succession.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides that a kind of compound material and base bonding property wash away by force, firm, anti-, long service life and production method is simple, suitability is strong, can effectively guarantee the TiB of the effect of wettable negative electrode
2The composite layer cathode carbon block preparation method.
The objective of the invention is to be achieved through the following technical solutions.
A kind of TiB
2The composite layer cathode carbon block preparation method is characterized in that preparation process comprises:
A. prepare TiB
2The composite bed thickener
By mass ratio is the TiB of 20%--70%
2Powder, mass ratio are that 15%～17% coal-tar pitch or mass ratio are that 13% epoxy adhesive, surplus are that the broken ratio of graphite is prepared burden, earlier with TiB
2With broken dried the doing time 10～20 minutes of graphite, add that rewetting mixed 35--50 minute behind the pitch, mixed Nie Wendu is higher than 40 ℃～60 ℃ of binding agent softening temperatures, prepares compound material and sticks with paste;
B.TiB
2Composite layer cathode carbon block
Prepare conventional cathode carbon pieces and make matrix, vibrate and add compound thickener after 30～60 seconds, evenly shakeout the back and continue moulding and finish, obtain the TiB of various different sizes by one roasting, processing until moulding
2The broken composite cathode carbon piece of-graphite product.
Method of the present invention is characterized in that binding agent is the coal-tar pitch that SP equals 85.5 ℃.
Method of the present invention is characterized in that TiB
2The chemical purity of powder is greater than 85%.
Method of the present invention is characterized in that the broken degree of graphitization of graphite is 80%～98%, powder resistivity 120-300 μ Ω m, granularity be less than 2mm.
A kind of TiB
2The composite layer cathode carbon block preparation method is characterized in that TiB
2Be compound thickener evenly is layered on moulding box bottom during composite layer cathode carbon block, add the matrix material moulding then.
A kind of TiB
2The composite layer cathode carbon block preparation method is characterized in that keeping working face and not processing adding man-hour goods, only processes all the other five faces, unprocessed working face when brickwork as the furnace bottom upper surface.
Method of the present invention adopts TiB
2The broken matrix material of-graphite, compound material mix in special use with rational binding agent and mix alunite in the alunite pot separately, and be one-body molded in moulding process, TiB
2Content is arbitrarily adjusted in 20%～70% scope as required.Because graphite and binding agent and the carbon matrix piece selected for use have same or analogous performance, and are one-body molded, roastings, compound bed thickness 10～25mm is so compound material and base bonding property wash away by force, firm, anti-, long service life.The negative electrode composite block of Sheng Chaning like this, method is simple, suitability is strong, reaches the effect of wettable negative electrode.Furnace bottom loss of voltage, bottom land do not have aliquation, do not have protuberance, and trough operates steadily.
Make cathode of aluminium electrolytic bath with the inventive method, the characteristic of negative electrode working face is greatly improved, and aluminium liquid is good to its wettability, and the surfaces of aluminum liquid film of formation has played the erosion that the protection cathode material exempts from fused electrolyte, has improved negative electrode work-ing life.Method is simple, except that carrying out separately not increasing any miscellaneous equipment the small-sized mixed alunite with material to compound, production process also strong, the good operability of no change, suitability, easily apply.Employing composite bed-matrix block is one-body molded, the method for roasting, good, the unsuitable delamination of plyability, long service life, and trough is stable.TiB
2Content can change in 20%～70% scope, is applicable to the requirement of various conditions, and can suitably control manufacturing cost under the satisfactory prerequisite of product performance.Adopt the TiB of method preparation of the present invention
2Composite layer cathode carbon block is received the absorption phase at electrobath start height just, and the negative electrode sodium absorbing capacity obviously reduces, and electrolyte molecule only is 30% of a comparison groove than underspeeding.Electrolyzer is stable, bottom land is clean, do not have precipitation compares with comparison groove, and cathode drop reduces by 60～80mv, and the primary aluminum direct current consumption reduces by 100～200Kwh/t.A, estimates that cell life can improve 400～600 days.
Embodiment
A kind of TiB
2The composite layer cathode carbon block preparation method is the TiB of 20%--70% with chemical purity greater than 85% mass ratio at first
2Powder, ratio are 13%～17% a kind of binding agent in coal-tar pitch or the Resins, epoxy of being selected from, and all the other are that degree of graphitization 80%～98%, powder resistivity 120--300 μ Ω m, granularity are broken less than the powder graphite of 2mm; In mixed alunite pot compound material list is solely mixed alunite, mixed Nie Wendu is higher than 40 ℃～60 ℃ of binding agent softening temperatures, dried doing time 10-20 minute, add cakingagent after 35--50 minute wet mixing time make TiB
2Compound thickener; The conventional cathode carbon pieces of refabrication is made matrix, vibrates to add compound thickener after 30～60 seconds, evenly shakeouts back continuation moulding and finishes until moulding, obtains the TiB of various different sizes by one roasting, processing
2The broken composite cathode carbon piece of-graphite product.
Embodiment 1
Mixing the alunite pot with the 50L electrically heated, is 20% TiB with mass ratio
2Powder, mass ratio are that 63% graphite is broken, mass ratio is that 17% SP equals 85.5 ℃ coal-tar pitch and carries out mix, earlier with TiB
2With the broken dried 20min that does time of graphite, add that rewetting mixes 50min behind the pitch, mix 145 ℃ of Nie Wendu, prepare compound material.
The matrix material is aggregate with the electric calcined anthracite, and adopting powder resistivity is the cathode carbon pieces production thickener of 540 μ Ω m.Take by weighing negative electrode matrix thickener 1450Kg, in the moulding box of the wide 560mm of long 3620mm weight-adding hammer vibration 45see, mention weight, with the upper surface plucking, evenly spread compound material 40kg, the demoulding after relaying lower heavy punch and vibrating 2min, cooling with special-purpose rastellus.After 230h adds thermal bake-out, come out of the stove, process, check, TiB
2Composite bed and matrix closely combine together, no sharp interface, and its thick 12mm that is about does not have cracking, no aliquation, but through test and metal aluminium liquid complete wetting.
Embodiment 2
Mixing the alunite pot with the 50L electrically heated, is 50% TiB with mass ratio
2Powder, mass ratio are that 37% graphite is broken, mass ratio is that 13% Resins, epoxy carries out mix, earlier with TiB
2With the broken dried 10min that does time of graphite, add that rewetting mixes 35min behind the Resins, epoxy, mix 165 ℃ of Nie Wendu, prepare compound material.
The matrix material is aggregate with the electric calcined anthracite, and adopting powder resistivity is the cathode carbon pieces production thickener of 540 μ Ω m.Take by weighing negative electrode matrix thickener 1450Kg, in the moulding box of the wide 560mm of long 3620mm weight-adding hammer vibration 45sec, mention weight, with the upper surface plucking, evenly spread compound material 40kg, the demoulding after relaying lower heavy punch and vibrating 2min, cooling with special-purpose rastellus.After 230h adds thermal bake-out, come out of the stove, process, check, TiB
2Composite bed and matrix closely combine together, no sharp interface, and its thick 12mm that is about does not have cracking, no aliquation, but through test and metal aluminium liquid complete wetting.
Embodiment 3
Mix the alunite pot with the 50L electrically heated and mix alunite compound, TiB
2Mass ratio be 70%, mass ratio is that 15% graphite is broken, mass ratio is that 15% SP equals that 85.5 ℃ coal-tar pitch carries out other parameter of mix and step is identical with example 1.Made-up article, through cooling, roasting, processing, inspection, composite bed and matrix form one, no sharp interface, working face is smooth, and the about 10mm of compound bed thickness with metal aluminium liquid test, 10～12 ° of angle of wettings, can be used as the wettability cathode block of electrolyzer.Keep working face and do not process adding man-hour goods, only process all the other five faces, unprocessed working face when brickwork as the furnace bottom upper surface.
Claims (6)
1. TiB
2The composite layer cathode carbon block preparation method is characterized in that preparation process comprises:
A. prepare TiB
2The composite bed thickener
By mass ratio is the TiB of 20%--70%
2Powder, mass ratio are that 15%～17% coal-tar pitch or mass ratio are that 13% epoxy adhesive, surplus are that the broken ratio of graphite is prepared burden, earlier with TiB
2With broken dried the doing time 10～20 minutes of graphite, add that rewetting mixed 35--50 minute behind the pitch, mixed Nie Wendu is higher than 40 ℃～60 ℃ of binding agent softening temperatures, prepares compound material and sticks with paste;
B.TiB
2Composite layer cathode carbon block
Prepare conventional cathode carbon pieces and make matrix, vibrate and add compound thickener after 30～60 seconds, evenly shakeout the back and continue moulding and finish, obtain the TiB of various different sizes by one roasting, processing until moulding
2The broken composite cathode carbon piece of-graphite product.
2. method according to claim 1 is characterized in that binding agent is the coal-tar pitch that SP equals 85.5 ℃.
3. method according to claim 1 is characterized in that TiB
2The chemical purity of powder is greater than 85%.
4. method according to claim 1 is characterized in that the broken degree of graphitization of graphite is 80%～98%, powder resistivity 120-300 μ Ω m, granularity be less than 2mm.
5. method according to claim 1 is characterized in that TiB
2Be compound thickener evenly is layered on moulding box bottom during composite layer cathode carbon block, add the matrix material moulding then.
6. method according to claim 1 is characterized in that keeping working face and not processing adding man-hour goods, only processes all the other five faces, unprocessed working face when brickwork as the furnace bottom upper surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101009777A CN100366800C (en) | 2004-12-28 | 2004-12-28 | Preparation method of TiB2 composite layer cathode carbon block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004101009777A CN100366800C (en) | 2004-12-28 | 2004-12-28 | Preparation method of TiB2 composite layer cathode carbon block |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1651612A CN1651612A (en) | 2005-08-10 |
| CN100366800C true CN100366800C (en) | 2008-02-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004101009777A Active CN100366800C (en) | 2004-12-28 | 2004-12-28 | Preparation method of TiB2 composite layer cathode carbon block |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102011004014A1 (en) * | 2011-02-11 | 2012-08-16 | Sgl Carbon Se | Cathode block with a covering layer containing hard material |
| DE102011004012A1 (en) * | 2011-02-11 | 2012-08-16 | Sgl Carbon Se | Surface profiled graphite cathode block with an abrasion resistant surface |
| DE102011004001A1 (en) * | 2011-02-11 | 2012-08-16 | Sgl Carbon Se | Hard material-containing surface profiled cathode block |
| CN102212845B (en) * | 2011-05-24 | 2012-10-31 | 昆明冶金研究院 | Method for preparing TiB2 cathode coating for aluminium electrolysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85205776U (en) * | 1985-12-31 | 1986-10-22 | 东北工学院 | Tib2 composite layers-type cathode for ai electrolysis |
| CN87214638U (en) * | 1987-10-22 | 1988-11-02 | 河北省马头铝厂 | Cathod structure of half-lead electrolytic cell with high electric conductivity |
| CN1091471C (en) * | 2000-05-08 | 2002-09-25 | 新化县碳素厂 | Carbon block as cathode with compound titanium boride-carbon layer and its preparing process |
-
2004
- 2004-12-28 CN CNB2004101009777A patent/CN100366800C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85205776U (en) * | 1985-12-31 | 1986-10-22 | 东北工学院 | Tib2 composite layers-type cathode for ai electrolysis |
| CN87214638U (en) * | 1987-10-22 | 1988-11-02 | 河北省马头铝厂 | Cathod structure of half-lead electrolytic cell with high electric conductivity |
| CN1091471C (en) * | 2000-05-08 | 2002-09-25 | 新化县碳素厂 | Carbon block as cathode with compound titanium boride-carbon layer and its preparing process |
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| Publication number | Publication date |
|---|---|
| CN1651612A (en) | 2005-08-10 |
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