CN102268697A - Graphite anode for magnesium electrolysis and preparation method thereof - Google Patents
Graphite anode for magnesium electrolysis and preparation method thereof Download PDFInfo
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- CN102268697A CN102268697A CN2011101258657A CN201110125865A CN102268697A CN 102268697 A CN102268697 A CN 102268697A CN 2011101258657 A CN2011101258657 A CN 2011101258657A CN 201110125865 A CN201110125865 A CN 201110125865A CN 102268697 A CN102268697 A CN 102268697A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 34
- 239000010439 graphite Substances 0.000 title claims abstract description 34
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 30
- 239000011777 magnesium Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005868 electrolysis reaction Methods 0.000 title abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 13
- 238000007598 dipping method Methods 0.000 claims abstract description 11
- 238000005087 graphitization Methods 0.000 claims abstract description 8
- 239000002006 petroleum coke Substances 0.000 claims abstract description 8
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 7
- 239000011300 coal pitch Substances 0.000 claims abstract description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008117 stearic acid Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000011230 binding agent Substances 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 28
- 238000012856 packing Methods 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- 239000011295 pitch Substances 0.000 claims description 16
- 238000012545 processing Methods 0.000 claims description 16
- 239000002562 thickening agent Substances 0.000 claims description 16
- 230000000996 additive effect Effects 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 230000037396 body weight Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019786 weight gain Nutrition 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 4
- 238000003754 machining Methods 0.000 claims description 4
- 238000012423 maintenance Methods 0.000 claims description 2
- 238000013461 design Methods 0.000 abstract description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 5
- 239000010936 titanium Substances 0.000 abstract description 5
- 229910052719 titanium Inorganic materials 0.000 abstract description 5
- 238000003723 Smelting Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 230000003111 delayed effect Effects 0.000 abstract 2
- 239000002245 particle Substances 0.000 abstract 2
- 239000000843 powder Substances 0.000 abstract 1
- 238000007689 inspection Methods 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 230000000007 visual effect Effects 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
The invention which relates to a graphite anode for magnesium electrolysis and a preparation method thereof belongs to the technical field of carbon material preparation. The preparation method comprises the following steps: preparing a dry material from delayed roasted petroleum coke particles with different particle grades, delayed petroleum coke powder, and graphite scraps; adding the dry material to a mixing pan, adding additives iron oxide powder and stearic acid, adding a binder medium temperature coal pitch, carrying out moisture mixing to prepare a paste, profiling, calcinating, dipping, and graphitizing. An innovative technological formula, a reasonable calcination system, a large-scale direct-current Acheson graphitization furnace, a graphitization technology and advanced production equipment are utilized in the invention to produce the graphite anode for magnesium electrolysis to replace imported thin-structured graphite anodes for magnesium electrolysis, so technical designs and usage requirements of fields of home and abroad magnesium electrolysis, titanium smelting and the like are satisfied.
Description
Technical field
The invention belongs to the carbon material preparing technical field, particularly a kind of magnesium eletrolysis graphite anode and preparation method thereof.
Background technology
Continuous development along with the magnesium alloy materials technology, and the Application Areas demand growth relevant such as aviation, automobile with the titanium material, domestic magnesium eletrolysis, titanium smelting industry have obtained development rapidly, and electrolytic process is the main method that metal current magnesium is produced, graphite anode requires to have satisfactory electrical conductivity as the core component of closing down magnesium electrolysis bath; High thermal resistance, anti-villaumite, resistance to chlorine corrodibility and oxidation-resistance; Higher withstand voltage, folding strength.Magnesium eletrolysis uses graphite anode as the expendable electro-conductive material, 10～18 months work-ing life, domestic enterprise introduces the modern technique of state's magnesium eletrolysis such as Ukraine, Canada, titanium smelting one after another at present, but the domestic big specification fine structure graphite anode that meets design requirement of still can not producing, seriously restricting the application of magnesium eletrolysis, titanium smelting modern technique, magnesium eletrolysis for a long time relies on from state's imports such as Germany, Japan with big specification fine structure graphite anode, and cost an arm and a leg, increased the production cost of magnesium eletrolysis.
Summary of the invention
It is magnesium eletrolysis fine structure graphite anode agricultural technology problem that the present invention will solve, and the invention provides the preparation method of a kind of magnesium eletrolysis with graphite anode.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of magnesium eletrolysis graphite anode, it is characterized in that to postpone the after-smithing petroleum coke granularity be that 2-1mm accounts for 25-30%, granularity is that 1-0.5mm accounts for 10-15%, granularity is that 0.5-0.075mm accounts for 4-10%, granularity accounts for 45-50% for 0.075-0.002 mm, and the broken 0.5-4mm of graphite accounts for 6%, as siccative, add the additive stearic acid that accounts for thickener gross weight 0.14%, add the additive Fe that accounts for thickener gross weight 0.4%
2O
3, add again mix behind the medium temperature coal pitch of binding agent 20-25% pinch, die mould, roasting, dipping, graphitization technique be prepared from.
1, its processing step is as follows:
(1) preparation of siccative: to postpone the after-smithing petroleum coke granularity is that 2-1mm accounts for 25-30%, and granularity is that 1-0.5mm accounts for 10-15%, and granularity is that 0.5-0.075mm accounts for 4-10%, and granularity accounts for 45-50% for 0.075-0.002 mm, and the broken 0.5-4mm of graphite accounts for 6%, as siccative;
(2) mixed pinching: siccative is directly added the mixed pot of pinching stir, adding accounts for the additive stearic acid of thickener gross weight 0.14%, adds the additive Fe that accounts for thickener gross weight 0.4%
2O
3, add the coal pitch of agglomerant that accounts for siccative gross weight 20-25% again and carry out wet mixing, going out to stick with paste temperature is 140～150 ℃, obtains thickener;
(3) die mould: will mix being lowered to forming mould after the tube stirring is mixed in the thickener adding vibrating forming machine insulation of pinching, blanking temperature 125-135 ℃, shook good time 1-4 minute in advance time 1-4 minute, by vibrating forming machine compacting raw product, the die mould raw product is stand-by after 72 hours through water-cooled, naturally cooling;
(4) bakes to burn the article: with the die mould raw product ring-form calcining furnace of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 96-120 hour, makes the bakes to burn the article product;
(5) single-steeping: with the bakes to burn the article product dipping baskets of packing into, entering impregnating autoclave behind the preheating 7h-9h under the 350-380 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.2-1.4MPa, keep 2-2.5h clamping time, impregnating pitch is returned out carry out water cooling afterwards, go out impregnating autoclave at last, make the single-steeping product, single-steeping rate of body weight gain 13-15%;
(6) re-baking: with the single-steeping product ring-form calcining furnace of packing into, fill and keep down beginning cooling after 23 hours, cool off and come out of the stove after 96-120 hour, make the re-baking product.Material granularity 0.075-6mm.Curve according to the rules heats up, in 1270 ℃ of conditions of top temperature;
(7) double-steeping: with the re-baking product dipping baskets of packing into, entering impregnating autoclave behind the preheating 7h-9h under the 350-380 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.2-1.4MPa, keep 2-2.5h clamping time, impregnating pitch is returned out carry out water cooling afterwards, go out impregnating autoclave at last, make the double-steeping product, double-steeping rate of body weight gain 10-13%;
(8) three roastings: with the double-steeping product ring-form calcining furnace of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 96-120 hour, makes roasting product three times;
(9) greying: three roasting products are packed in the acheson furnace, carry out graphitization processing according to setting power-supply curve, make temperature be heated to 3000～3500 ℃, cooling was safeguarded 288～336 hours, obtained the greying product;
(10) machining: after the inspection of greying product is qualified, can be according to the drawing requirement, multiple working procedure processing on milling machine tool working, after the drawing requirement is satisfied in monolithic processing, assemble examination again, visual appearance and working accuracy check by strictness require to assemble in accordance with regulations.According to every group of graphite anode of design requirements is that a cover is packed, warehouse-in, stand-by.
Roasting heating curve described in the step (4) is:
Roasting heating curve described in step (6), (8) is:
Greying power-supply curve described in the step (9) is:
The invention has the beneficial effects as follows: the magnesium eletrolysis fine structure graphite anode that the present invention produces, product quality indicator and use properties all meet or exceed national standard, have satisfactory electrical conductivity; High thermal resistance, anti-villaumite, resistance to chlorine corrodibility and oxidation-resistance; Higher withstand voltage, folding strength.Alternative import magnesium eletrolysis graphite anode product reduces the magnesium eletrolysis production cost.
Embodiment:
Embodiment 1:
A kind of magnesium eletrolysis preparation method of graphite anode, its processing step is as follows:
(1) preparation of siccative: to postpone the after-smithing petroleum coke granularity is 1mm 440Kg; Granularity is 0.5mm 264Kg; Granularity is 0.075mm 70Kg; Granularity is 0.002 mm 880Kg; The broken 0.5mm 106Kg of graphite; Make siccative, siccative gross weight 1760 Kg.
(2) mixed pinching: siccative is directly added the mixed pot of pinching stir, adding additive stearic acid 3Kg; Add additive Fe
2O
39 Kg; Add coal pitch of agglomerant 440 Kg again and carry out wet mixing, going out to stick with paste temperature is 140 ℃, obtains thickener.
(3) die mould: will mix being lowered to forming mould after the tube stirring is mixed in the thickener adding vibrating forming machine insulation of pinching, 125 ℃ of blanking temperatures shake 1 minute time in advance, 1 minute good time, by vibrating forming machine compacting raw product, the die mould raw product is stand-by after 72 hours through water-cooled, naturally cooling.
(4) bakes to burn the article: with the die mould raw product formula ring-form calcining furnace with cover of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 96 hours, makes the bakes to burn the article product.
(5) single-steeping: with the bakes to burn the article product dipping baskets of packing into, entering impregnating autoclave behind the preheating 7h under 350 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.2MPa, keep 2h clamping time, impregnating pitch is returned out carry out water cooling afterwards, go out impregnating autoclave at last, make the single-steeping product, single-steeping rate of body weight gain 13%.
(6) re-baking: with the single-steeping product formula ring-form calcining furnace with cover of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 96 hours, makes the re-baking product.
(7) double-steeping: with the re-baking product dipping baskets of packing into, entering impregnating autoclave behind the preheating 7h under 350 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.2MPa, keep 2h clamping time, impregnating pitch is returned out carry out water cooling afterwards, go out impregnating autoclave at last, make the double-steeping product, double-steeping rate of body weight gain 10%.
(8) three roastings: with the double-steeping product formula ring-form calcining furnace with cover of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 96 hours, makes roasting product three times.
(9) greying: three roasting products are packed in the acheson furnace, carry out graphitization processing according to setting power-supply curve, make temperature be heated to 3000 ℃, cooling maintenance time 288 hours obtains the greying product.
(10) machining: after the inspection of greying product is qualified, can be according to the drawing requirement, multiple working procedure processing on milling machine tool working, after the drawing requirement is satisfied in monolithic processing, assemble examination again, visual appearance and working accuracy check by strictness require to assemble in accordance with regulations.According to every group of graphite anode of design requirements is that a cover is packed, warehouse-in, stand-by.Product finish size and tolerance:
A, 660 * 200 * 2250mm; 412 * 150 * 2250mm; Specifications such as 330 * 150 * 2250mm.
Assemble behind b, fluting, boring, the processing connecting key, the every group of positive plate specification in assembling back is 824 * 150 * 2250mm; Specifications such as 990 * 150 * 2250mm, working accuracy satisfy user's design or requirement.
The magnesium eletrolysis fine structure graphite anode that the present invention makes, the plain corporate state of the big charcoal of classical prescription is detected in the approval laboratory, meets the top grade product standard of national standard YB/T5053-1997 fully, and main physical and chemical index is as follows:
| Project | Target in kind | National standard (top grade) |
| Ash content | ≤0.2%? | ≯0.2% |
| Volume density | 1.71～1.75g/cm 3 | ≮1.62 g/cm 3 |
| Compressive strength | 30～34 MPa | ≮29MPa |
| Folding strength | ≥16 MPa | ≮16MPa |
| Resistivity | 5.0～7.5μΩ.m | ≯7.5μΩ.m |
Roasting heating curve described in the step (4) is:
Roasting heating curve described in step (6), (8) is:
Greying power-supply curve described in the step (9) is:
Embodiment 2:
A kind of magnesium eletrolysis preparation method of graphite anode, its processing step is as follows:
(1) preparation of siccative: to postpone the after-smithing petroleum coke granularity is 2mm 495Kg; Granularity is 1mm 165Kg; Granularity is that 0.5mm accounts for 9%, 149Kg; Granularity is 0.075 mm 742Kg; The broken 4mm 99Kg of graphite; As siccative, siccative gross weight 1650Kg.
(2) mixed pinching: siccative is directly added the mixed pot of pinching stir, adding additive stearic acid 3Kg; Add additive Fe
2O
39Kg; Add coal pitch of agglomerant 550 Kg again and carry out wet mixing, going out to stick with paste temperature is 150 ℃, obtains thickener.
(3) die mould: will mix being lowered to forming mould after the tube stirring is mixed in the thickener adding vibrating forming machine insulation of pinching, 135 ℃ of blanking temperatures shake 4 minutes time in advance, 4 minutes good time, by vibrating forming machine compacting raw product, the die mould raw product is stand-by after 72 hours through water-cooled, naturally cooling.
(4) bakes to burn the article: with the die mould raw product formula ring-form calcining furnace with cover of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 120 hours, makes the bakes to burn the article product.
(5) single-steeping: with the bakes to burn the article product dipping baskets of packing into, entering impregnating autoclave behind the preheating 9h under 380 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.4MPa, keep 2.5h clamping time, afterwards impregnating pitch is returned out and carry out water cooling, go out impregnating autoclave at last, make the single-steeping product.Single-steeping rate of body weight gain 15%.
(6) re-baking: with the single-steeping product formula ring-form calcining furnace with cover of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 120 hours, makes the re-baking product.
(7) double-steeping: with the re-baking product dipping baskets of packing into, entering impregnating autoclave behind the preheating 9h under 380 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.4MPa, keep 2.5h clamping time, afterwards impregnating pitch is returned out and carry out water cooling, go out impregnating autoclave at last, make the double-steeping product.Double-steeping rate of body weight gain 13%.
(8) three roastings: with the double-steeping product formula ring-form calcining furnace with cover of packing into, stopping composition granularity 0.075-6mm.Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 120 hours, makes roasting product three times.
(9) greying: three roasting products are packed in the acheson furnace, carry out graphitization processing according to setting power-supply curve, make temperature be heated to 3500 ℃, cooling was safeguarded 336 hours, obtained the greying product.
(10) machining: after the inspection of greying product is qualified, can be according to the drawing requirement, multiple working procedure processing on milling machine tool working, after the drawing requirement is satisfied in monolithic processing, assemble examination again, visual appearance and working accuracy check by strictness require to assemble in accordance with regulations.According to every group of graphite anode of design requirements is that a cover is packed, warehouse-in, stand-by.Product finish size and tolerance:
A, 660 * 200 * 2250mm; 412 * 150 * 2250mm; Specifications such as 330 * 150 * 2250mm.
Assemble behind b, fluting, boring, the processing connecting key, the every group of positive plate specification in assembling back is 824 * 150 * 2250mm; Specifications such as 990 * 150 * 2250mm, working accuracy satisfy user's design or requirement.
The magnesium eletrolysis fine structure graphite anode that the present invention makes, the plain corporate state of the big charcoal of classical prescription is detected in the approval laboratory, meets the top grade product standard of national standard YB/T5053-1997 fully, and main physical and chemical index is as follows:
| Project | Target in kind | National standard (top grade) |
| Ash content | ≤0.2%? | ≯0.2% |
| Volume density | 1.72～1.75g/cm 3 | ≮1.62 g/cm 3 |
| Compressive strength | 30～35 MPa | ≮29MPa |
| Folding strength | 16～20 MPa | ≮16MPa |
| Resistivity | 5.0～7.5μΩ.m | ≯7.5μΩ.m |
Roasting heating curve described in the step (4) is:
Roasting heating curve described in step (6), (8) is:
Greying power-supply curve described in the step (9) is:
Claims (5)
1. magnesium eletrolysis graphite anode, it is characterized in that: to postpone the after-smithing petroleum coke granularity is that 2-1mm accounts for 25-30%, granularity is that 1-0.5mm accounts for 10-15%, granularity is that 0.5-0.075mm accounts for 4-10%, granularity accounts for 45-50% for 0.075-0.002 mm, and the broken 0.5-4mm of graphite accounts for 6%, as siccative, add the additive stearic acid that accounts for thickener gross weight 0.14%, add the additive Fe that accounts for thickener gross weight 0.4%
2O
3, add again mix behind the medium temperature coal pitch of binding agent 20-25% pinch, die mould, roasting, dipping, graphitization technique be prepared from.
2. one kind prepares the method for magnesium eletrolysis graphite anode according to claim 1, and its processing step is as follows:
(1) preparation of siccative: to postpone the after-smithing petroleum coke granularity is that 2-1mm accounts for 25-30%, and granularity is that 1-0.5mm accounts for 10-15%, and granularity is that 0.5-0.075mm accounts for 4-10%, and granularity accounts for 45-50% for 0.075-0.002 mm, and the broken 0.5-4mm of graphite accounts for 6%, makes siccative;
(2) mixed pinching: siccative is directly added the mixed pot of pinching stir, adding accounts for the additive stearic acid of thickener gross weight 0.14%, adds the additive Fe that accounts for thickener gross weight 0.4%
2O
3, add the coal pitch of agglomerant that accounts for siccative gross weight 20-25% again and carry out wet mixing, going out to stick with paste temperature is 140～150 ℃, obtains thickener;
(3) die mould: will mix being lowered to forming mould after the tube stirring is mixed in the thickener adding vibrating forming machine insulation of pinching, blanking temperature 125-135 ℃, shook good time 1-4 minute in advance time 1-4 minute, by vibrating forming machine compacting raw product, the die mould raw product is stand-by after 72 hours through water-cooled, naturally cooling;
(4) bakes to burn the article: with the die mould raw product ring-form calcining furnace of packing into, stopping composition granularity 0.075-6mm, curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cool off and come out of the stove after 96-120 hour, make the bakes to burn the article product;
(5) single-steeping: with the bakes to burn the article product dipping baskets of packing into, entering impregnating autoclave behind the preheating 7h-9h under the 350-380 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.2-1.4MPa, keep 2-2.5h clamping time, impregnating pitch is returned out carry out water cooling afterwards, go out impregnating autoclave at last, make the single-steeping product, single-steeping rate of body weight gain 13-15%;
(6) re-baking: with the single-steeping product ring-form calcining furnace of packing into, stopping composition granularity 0.075-6mm, curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cool off and come out of the stove after 96-120 hour, make the re-baking product;
(7) double-steeping: with the re-baking product dipping baskets of packing into, entering impregnating autoclave behind the preheating 7h-9h under the 350-380 ℃ of temperature condition, under-70KPa, keep vacuum 1h, pitch moulding pressure 1.2-1.4MPa, keep 2-2.5h clamping time, impregnating pitch is returned out carry out water cooling afterwards, go out impregnating autoclave at last, make the double-steeping product, double-steeping rate of body weight gain 10-13%;
(8) three roastings: with the double-steeping product ring-form calcining furnace of packing into, stopping composition granularity 0.075-6mm,
Curve according to the rules heats up, and begins cooling after keeping 23 hours under 1270 ℃ of conditions of top temperature, cools off and comes out of the stove after 96-120 hour, makes roasting product three times;
(9) greying: three roasting products are packed in the acheson furnace, carry out graphitization processing according to setting power-supply curve, make temperature be heated to 3000～3500 ℃, cooling maintenance time 288～336 hours obtains the greying product;
(10) machining: the greying product are processed as finished product on the number of combinations controlled machine.
3. a kind of magnesium eletrolysis according to claim 2 preparation method of graphite anode is characterized in that the roasting heating curve described in the step (4) is:
。
4. a kind of magnesium eletrolysis according to claim 2 preparation method of graphite anode is characterized in that the roasting heating curve described in step (6), (8) is:
。
5. a kind of magnesium eletrolysis according to claim 2 preparation method of graphite anode is characterized in that the greying power-supply curve described in the step (9) is:
。
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|---|---|---|---|
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| CN102774830A (en) * | 2012-08-10 | 2012-11-14 | 昆明冶金研究院 | Method for impregnating high-purity graphite by using high-purity coal tar pitch |
| CN103528366A (en) * | 2013-09-25 | 2014-01-22 | 葫芦岛市连山区宏达石化厂 | Method for producing anode butt by adopting energy saving and environment protection technologies |
| CN104129782A (en) * | 2014-07-30 | 2014-11-05 | 焦作市中州炭素有限责任公司 | Graphite electrode with diameter of 348 mm and manufacture method thereof |
| CN105967718A (en) * | 2016-07-08 | 2016-09-28 | 南通扬子碳素股份有限公司 | Graphite anode for heavy current resistant magnesium electrolysis and preparation process thereof |
| CN108541096A (en) * | 2018-05-25 | 2018-09-14 | 山西丹源碳素股份有限公司 | A kind of monoblock type internal thermal tandem graphitization furnace tip electrode and preparation method thereof |
| CN109852081A (en) * | 2018-12-20 | 2019-06-07 | 淄博大陆石墨科技有限公司 | The preparation method that vibration-compression molding special graphite is homogenized with thickener |
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| CN104129782A (en) * | 2014-07-30 | 2014-11-05 | 焦作市中州炭素有限责任公司 | Graphite electrode with diameter of 348 mm and manufacture method thereof |
| CN105967718A (en) * | 2016-07-08 | 2016-09-28 | 南通扬子碳素股份有限公司 | Graphite anode for heavy current resistant magnesium electrolysis and preparation process thereof |
| CN105967718B (en) * | 2016-07-08 | 2019-06-14 | 南通扬子碳素股份有限公司 | The graphite anode for magnesium electrolysis of resistance to high current and its preparation process |
| CN108541096A (en) * | 2018-05-25 | 2018-09-14 | 山西丹源碳素股份有限公司 | A kind of monoblock type internal thermal tandem graphitization furnace tip electrode and preparation method thereof |
| CN109852081A (en) * | 2018-12-20 | 2019-06-07 | 淄博大陆石墨科技有限公司 | The preparation method that vibration-compression molding special graphite is homogenized with thickener |
| CN109852081B (en) * | 2018-12-20 | 2021-07-30 | 淄博大陆石墨科技有限公司 | Preparation method of paste homogenization for special graphite by vibration-compression molding |
| CN110316732A (en) * | 2019-04-30 | 2019-10-11 | 大同市新荣区新大科技有限责任公司 | A kind of process carrying out high temperature purification using acheson furnace |
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