CN102212843A - Start-up method for preparing metal and alloys through molten salt electrolysis - Google Patents
Start-up method for preparing metal and alloys through molten salt electrolysis Download PDFInfo
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- CN102212843A CN102212843A CN2011101407793A CN201110140779A CN102212843A CN 102212843 A CN102212843 A CN 102212843A CN 2011101407793 A CN2011101407793 A CN 2011101407793A CN 201110140779 A CN201110140779 A CN 201110140779A CN 102212843 A CN102212843 A CN 102212843A
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Abstract
The invention relates to a start-up method for preparing metal and alloys through molten salt electrolysis. The method comprises the following steps: (1) ensuring the tip of a sharply pointed graphite block in a start-up device for preparing the metal and alloys through molten salt electrolysis to contact with the bottom of a graphite crucible in an electrolytic cell and be separated from the top edge of the graphite crucible by a gap, and then adding a solid electrolyte into the graphite crucible; (2) switching on an alternating current regulated power supply to heat the solid electrolyte until the solid electrolyte completely becomes liquid to obtain molten electrolyte; (3) adjusting a lifting insulation rack to ensure the tip of the sharply pointed graphite block connected with the lifting insulation rack to break away from the bottom of the graphite crucible; (4) after the molten electrolyte is fully molten into liquid molten salt, switching off the alternating current regulated power supply; (5) putting an electrolysis product metal or alloy receiver at the central bottom of the graphite crucible and simultaneously installing a tungsten rod; and (6) using the graphite crucible as an anode and the tungsten rod as a cathode to carry out electrolysis operation. The start-up method has the advantages of flexible and convenient conversion from start-up operation to electrolysis operation and stability in operation.
Description
Technical field
The present invention relates to metallurgical technology field, relate in particular to the stove method that opens that fused salt electrolysis process prepares metal and alloy.
Background technology
At present, when preparing metal simple-substance or metal alloy, need ionogen is heated to thawing before the electrolysis, just can carry out formal electrolytic process then with fused salt electrolysis process.The heating of adopting is at present opened the stove method and is mainly contained three kinds: (1) outer heating method, i.e. heating unit and equipment outside the fused-salt bath exterior arrangement, this mode makes that to comprise outer heating unit bigger at interior whole electrolyzer volume, and outer heating efficiency is not high yet, and power loss is bigger; (2) built-in electrode heating method promptly is specifically designed to the electrode of heating in the electrolyzer internal configuration, heating electrode and electrolysis electrode generally can not be general, and this causes the structure more complicated of electrolyzer, has brought extra burden for the design preparation of electrolyzer; (3) starting the arc heating method though this method is more flexible, needs to be equipped with special equipment, and heat-processed is also steady inadequately.Therefore, easy and simple to handle, energy-conservation be suitable for, operate steadily open the active demand that the stove method has become this area.
Summary of the invention
Technical problem to be solved by this invention provides the stove method that opens that a kind of fused salt electrolysis process easy and simple to handle, that operate steadily prepares metal and alloy.
For addressing the above problem, fused salt electrolysis process of the present invention prepares the stove method that opens of metal and alloy, may further comprise the steps:
(1) fused salt electrolysis process is prepared the tip of the tip graphite block in the start-up device of metal and alloy and the plumbago crucible bottom connection in the electrolyzer and touch, and be provided with the gap with described plumbago crucible top; Once or one by one in described plumbago crucible, add single or hybrid solid electrolyte then;
(2) open alternating current steady voltage plug in the start-up device that described fused salt electrolysis process prepares metal and alloy, described solid electrolyte is heated to becomes liquid fully, obtain fused electrolyte;
(3) regulate liftable insulating support in the start-up device that described fused salt electrolysis process prepares metal and alloy, the tip of coupled described tip graphite block is disengaged bottom described plumbago crucible; At this moment, utilize described fused electrolyte to conduct electricity and make fused electrolyte self-heating, fusing;
(4) treat that described fused electrolyte fully is fused into the liquid fused salt after, close described alternating current steady voltage plug, remove or remove the lead that is connected between lead, described plumbago crucible and the described alternating current steady voltage plug of being connected between described tip graphite block, liftable insulating support and described tip graphite block and the described alternating current steady voltage plug simultaneously;
(5) put into electrolysate metal or alloy receptor in described plumbago crucible centre bottom, on described liftable insulating support, tungsten bar is installed simultaneously, and this tungsten bar is put into described liquid fused salt;
(6) with described plumbago crucible as anode, link to each other with the positive terminal of electrolysis power with positive wire or busbar; Described tungsten bar as negative electrode, is linked to each other with the negative pole end of described electrolysis power with cathode wire or busbar; Open described electrolysis power, carry out electrolysis procedure and get final product.
Tip graphite block in the described step (1) is wedge shape or taper, and its underpart is most advanced and sophisticated.
The present invention compared with prior art has the following advantages:
1, the present invention adopts readily removable tip graphite block that removes and plumbago crucible to constitute heating circuit, compare with starting the arc heating method with the outer heating of present employing, built-in electrode heating, have cell construction simple, open furnace operating and change advantage flexible, that save energy and reduce the cost, operate steadily with electrolysis procedure.
2, method of the present invention is in opening the process of furnace operating, easily the element of loss has only the tip graphite block, can reduce its height after the loss of tip graphite block, guarantee that its most advanced and sophisticated contact with the plumbago crucible bottom gets final product, only under tip graphite block loss serious situation, just need to change monoblock tip graphite block, thus easy to operate, and running cost is low.
3, use range is wide, the application scenario is wide, not being subject to concrete molten salt electrolyte forms, when opening stove with any single or multi-component ionogen, can adopt present method, therefore, can be widely used in metal and alloy electrolysis, open stove when being particularly useful for preparing rare earth metal and rare earth alloy with fused salt electrolysis process.
Embodiment
Embodiment 1 carries out the stove method that opens that fused salt electrolysis process prepares metal and alloy with Repone K as ionogen, may further comprise the steps:
(1) fused salt electrolysis process is prepared the tip of the tip graphite block in the start-up device (Qinghai Yanhu Inst., Chinese Academy of Sciences's development) of metal and alloy and the plumbago crucible bottom connection in the electrolyzer and touch, and be provided with the gap with described plumbago crucible top; In plumbago crucible, add Repone K 2kg then.
(2) open alternating current steady voltage plug in the start-up device that fused salt electrolysis process prepares metal and alloy, make power switch be positioned at the constant current shelves, this moment, electric current was 800A, voltage 5V.Energising 15min post chlorization potassium becomes liquid fully, continues to append Repone K 1kg again, become liquid state fully after, obtain fusion Repone K.
(3) regulate liftable insulating support in the start-up device that fused salt electrolysis process prepares metal and alloy, the tip graphite block is raised 1.5cm, the tip of coupled tip graphite block is disengaged bottom plumbago crucible; At this moment, utilize fusion Repone K to conduct electricity and make Repone K self-heating, fusing, electric current diminishes, and voltage raises, and electric current becomes 400～600A, and voltage becomes 10～15V; Append pure Repone K 1kg again, make it be converted into liquid state fully.
(4) treat that fusion Repone K fully is fused into the liquid fused salt after, close alternating current steady voltage plug, remove or remove the lead that is connected between lead, plumbago crucible and the alternating current steady voltage plug of being connected between tip graphite block, liftable insulating support and tip graphite block and the alternating current steady voltage plug simultaneously.
(5) put into electrolysate metal or alloy receptor in the plumbago crucible centre bottom, on the liftable insulating support, tungsten bar is installed simultaneously, and this tungsten bar is put into the liquid fused salt.
(6) with plumbago crucible as anode, link to each other with the positive terminal of electrolysis power with positive wire or busbar; Tungsten bar as negative electrode, is linked to each other with the negative pole end of electrolysis power with cathode wire or busbar; Open electrolysis power, carry out electrolysis procedure and get final product.
Embodiment 2 carries out the stove method that opens that fused salt electrolysis process prepares metal and alloy with the mixture (mass ratio 1: 1) of Repone K and Magnesium Chloride Anhydrous as ionogen, may further comprise the steps:
(1) fused salt electrolysis process is prepared the tip of the tip graphite block in the start-up device of metal and alloy and the plumbago crucible bottom connection in the electrolyzer and touch, and be provided with the gap with described plumbago crucible top; In plumbago crucible, add blended solid salt 2kg then.
(2) open alternating current steady voltage plug in the start-up device that fused salt electrolysis process prepares metal and alloy, make power switch be positioned at the constant current shelves, this moment, electric current was 800A, voltage 5V.The energising 8min after mixing salt become liquid fully, continue to append mixing salt 1.5kg again, become liquid state fully after, obtain melting salt.
(3) regulate liftable insulating support in the start-up device that fused salt electrolysis process prepares metal and alloy, the tip graphite block is raised 1.5cm, the tip of coupled tip graphite block is disengaged bottom plumbago crucible; At this moment, utilize melting salt to conduct electricity and make melting salt self-heating, fusing, electric current diminishes, and voltage raises, and electric current becomes 400～600A, and voltage becomes 10～15V; Append mixing salt 1.5kg again, make it be converted into liquid state fully.
(4) treat that melting salt fully is fused into the liquid fused salt after, close alternating current steady voltage plug, remove or remove the lead that is connected between lead, plumbago crucible and the alternating current steady voltage plug of being connected between tip graphite block, liftable insulating support and tip graphite block and the alternating current steady voltage plug simultaneously.
(5) put into electrolysate metal or alloy receptor in the plumbago crucible centre bottom, on the liftable insulating support, tungsten bar is installed simultaneously, and this tungsten bar is put into the liquid fused salt.
(6) with plumbago crucible as anode, link to each other with the positive terminal of electrolysis power with positive wire or busbar; Tungsten bar as negative electrode, is linked to each other with the negative pole end of electrolysis power with cathode wire or busbar; Open electrolysis power, carry out electrolysis procedure and get final product.
Embodiment 3 carries out the stove method that opens that fused salt electrolysis process prepares metal and alloy with the mixture (mass ratio 2: 1) of Repone K and Magnesium Chloride Anhydrous as ionogen, may further comprise the steps:
(1) fused salt electrolysis process is prepared the tip of the tip graphite block in the start-up device of metal and alloy and the plumbago crucible bottom connection in the electrolyzer and touch, and be provided with the gap with described plumbago crucible top; In plumbago crucible, add blended solid salt 1.5kg then.
(2) open alternating current steady voltage plug in the start-up device that fused salt electrolysis process prepares metal and alloy, make power switch be positioned at the constant current shelves, this moment, electric current was 800A, voltage 5V.The energising 10min after mixing salt become liquid fully, continue to append mixing salt 1.5kg again, become liquid state fully after, obtain melting salt.
(3) regulate liftable insulating support in the start-up device that fused salt electrolysis process prepares metal and alloy, the tip graphite block is raised 1.5cm, the tip of coupled tip graphite block is disengaged bottom plumbago crucible; At this moment, utilize melting salt to conduct electricity and make melting salt self-heating, fusing, electric current diminishes, and voltage raises, and electric current becomes 400～600A, and voltage becomes 10～15V; Append mixing salt 1.5kg again, make it be converted into liquid state fully.
(4) treat that melting salt fully is fused into the liquid fused salt after, close alternating current steady voltage plug, remove or remove the lead that is connected between lead, plumbago crucible and the alternating current steady voltage plug of being connected between tip graphite block, liftable insulating support and tip graphite block and the alternating current steady voltage plug simultaneously.
(5) put into electrolysate metal or alloy receptor in the plumbago crucible centre bottom, on the liftable insulating support, tungsten bar is installed simultaneously, and this tungsten bar is put into the liquid fused salt.
(6) with plumbago crucible as anode, link to each other with the positive terminal of electrolysis power with positive wire or busbar; Tungsten bar as negative electrode, is linked to each other with the negative pole end of electrolysis power with cathode wire or busbar; Open electrolysis power, carry out electrolysis procedure and get final product.
Tip graphite block in the foregoing description 1～3 is wedge shape or taper, and its underpart is most advanced and sophisticated.
Content involved in the present invention is not subject to concrete molten salt electrolyte to be formed, and when opening stove with any single or multi-component ionogen, can adopt the inventive method.
Claims (2)
1. fused salt electrolysis process prepares the stove method that opens of metal and alloy, may further comprise the steps:
(1) fused salt electrolysis process is prepared the tip of the tip graphite block in the start-up device of metal and alloy and the plumbago crucible bottom connection in the electrolyzer and touch, and be provided with the gap with described plumbago crucible top; Once or one by one in described plumbago crucible, add single or hybrid solid electrolyte then;
(2) open alternating current steady voltage plug in the start-up device that described fused salt electrolysis process prepares metal and alloy, described solid electrolyte is heated to becomes liquid fully, obtain fused electrolyte;
(3) regulate liftable insulating support in the start-up device that described fused salt electrolysis process prepares metal and alloy, the tip of coupled described tip graphite block is disengaged bottom described plumbago crucible; At this moment, utilize described fused electrolyte to conduct electricity and make fused electrolyte self-heating, fusing;
(4) treat that described fused electrolyte fully is fused into the liquid fused salt after, close described alternating current steady voltage plug, remove or remove the lead that is connected between lead, described plumbago crucible and the described alternating current steady voltage plug of being connected between described tip graphite block, liftable insulating support and described tip graphite block and the described alternating current steady voltage plug simultaneously;
(5) put into electrolysate metal or alloy receptor in described plumbago crucible centre bottom, on described liftable insulating support, tungsten bar is installed simultaneously, and this tungsten bar is put into described liquid fused salt;
(6) with described plumbago crucible as anode, link to each other with the positive terminal of electrolysis power with positive wire or busbar; Described tungsten bar as negative electrode, is linked to each other with the negative pole end of described electrolysis power with cathode wire or busbar; Open described electrolysis power, carry out electrolysis procedure and get final product.
2. fused salt electrolysis process as claimed in claim 1 prepares the stove method that opens of metal and alloy, it is characterized in that: the tip graphite block in the described step (1) is wedge shape or taper, and its underpart is most advanced and sophisticated.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101407793A CN102212843A (en) | 2011-05-25 | 2011-05-25 | Start-up method for preparing metal and alloys through molten salt electrolysis |
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| CN2011101407793A CN102212843A (en) | 2011-05-25 | 2011-05-25 | Start-up method for preparing metal and alloys through molten salt electrolysis |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105441988A (en) * | 2015-11-19 | 2016-03-30 | 中国科学院青海盐湖研究所 | Furnace starting method for preparing simple substance metal or alloy in molten salt electrolysis mode |
| CN106801234A (en) * | 2017-01-17 | 2017-06-06 | 中国科学院青海盐湖研究所 | The preparation method of aluminium lithium intermediate alloy |
| CN110592617A (en) * | 2019-08-29 | 2019-12-20 | 青海物产工业投资有限公司 | Secondary starting method for full-series power failure of aluminum electrolysis cell |
-
2011
- 2011-05-25 CN CN2011101407793A patent/CN102212843A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105441988A (en) * | 2015-11-19 | 2016-03-30 | 中国科学院青海盐湖研究所 | Furnace starting method for preparing simple substance metal or alloy in molten salt electrolysis mode |
| CN106801234A (en) * | 2017-01-17 | 2017-06-06 | 中国科学院青海盐湖研究所 | The preparation method of aluminium lithium intermediate alloy |
| CN110592617A (en) * | 2019-08-29 | 2019-12-20 | 青海物产工业投资有限公司 | Secondary starting method for full-series power failure of aluminum electrolysis cell |
| CN110592617B (en) * | 2019-08-29 | 2021-06-15 | 青海物产工业投资有限公司 | Secondary starting method for full-series power failure of aluminum electrolysis cell |
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Application publication date: 20111012 |