CN103334126A - Method for preparing titanium sponge through resistance furnace by adopting molten salt electrolysis method - Google Patents
Method for preparing titanium sponge through resistance furnace by adopting molten salt electrolysis method Download PDFInfo
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- CN103334126A CN103334126A CN2013102387762A CN201310238776A CN103334126A CN 103334126 A CN103334126 A CN 103334126A CN 2013102387762 A CN2013102387762 A CN 2013102387762A CN 201310238776 A CN201310238776 A CN 201310238776A CN 103334126 A CN103334126 A CN 103334126A
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Abstract
The invention provides a method for preparing a titanium sponge through a resistance furnace by using a molten salt electrolysis method. The method comprises the following steps of: processing a calcium chloride fused salt (14) in a graphite crucible (2) in a low and constant temperature water extracting manner; charging argon into a sealed vacuum reactor through an air inlet pipe (6) after the water is removed; heating the resistance furnace (1) at a constant speed until reaching 1,000 DEG C; automatically lowering two electrode stems (9) through a lifting rod (8) in order to drive titanium dioxide (3) and a graphite plate (12) to enter the graphite crucible, wherein all current is 50A; exhausting carbon monoxide and carbon dioxide generated in electrolysis and the rest argon into a waste gas recycling tank through an air outlet pipe (10); lifting out the sealed vacuum reactor after electrolyzing to prepare the titanium sponge; pouring cooling water into an annular circulating water jacket (4) and an inner water jacket (5) until reaching room temperature; opening a reversed U shaped upper cover (11); taking out electrolyzed titanium dioxide; and then cleaning to obtain the titanium sponge with the purity up to 99.0%. The method has the characteristics of mature performance, safety and energy conservation performance.
Description
Technical field
The invention belongs to technical field of smelting, specially refer to a kind of fused salt electrolysis process that in resistance furnace, adopts and prepare the method for titanium sponge.
Background technology
The smelting technology comparative maturity of titanium be the Kroll method, the Kroll method is discontinuous, not only the loss of production cost height, equipment is big, and environmental pollution is serious.
For reducing its production cost and expanding the scale of production, the FFC of employing fused salt electrolysis process is also arranged, the technological operation of fused salt electrolysis process refining titanium is still under test, and its flow process is roughly as follows:
Titanium dioxide electrodes sheet preparation → fused salt electrolysis → electrode slice cleans → detects
Above-mentioned fused salt electrolysis is the critical process of fused salt electrolysis process; concrete grammar be exactly the titanium dioxide for preparing be cathode electrode sheet; be anode with fine and close graphite cake; in the high-temperature molten salt of calcium chloride, carry out electrolysis; 950 ℃ of electrolysis temperatures; bath voltage 3V; in the electrolytic process from negative electrode titanium dioxide electrodes sheet ionization go out oxonium ion and move to anode to discharge and generate carbon monoxide and carbonic acid gas and from electrolyzer, emit; titanium metal in the cathode electrode sheet is retained; after electrolysis is finished; the lifting battery lead rod is placed on cathode electrode sheet in the resistance furnace and under argon shield and naturally cools to room temperature with stove, opens bell and takes out cathode electrode sheet and can obtain titanium sponge after cleaning.
The vacuum leakproofness of above-mentioned fused salt electrolysis process is relatively poor, and the corrodibility of high temperature resistant molten salt is also relatively poor.
Patent publication No. CN2778832Y disclose a kind of direct be the fused-salt bath of raw material production titanium sponge with titanium dioxide, introduced the making method of this electrolyzer and introduced the making method of anode and negative electrode, the smelting technology of institute's foundation is different from above-mentioned fused salt electrolysis process.
Summary of the invention
For solving problems such as the vacuum leakproofness corrodibility relatively poor, high temperature resistant molten salt that exists in the fused salt electrolysis process is relatively poor, the invention provides a kind of fused salt electrolysis process that in resistance furnace, adopts and prepare the method for titanium sponge, can go out titanium sponge by fine electrolytic preparation by this method, and electrolysis goes out the more excellent titanium sponge of quality, makes the maturing more of FFC fused salt electrolysis process, safe, energy-conservationization.
For achieving the above object, the present invention adopts following technical scheme:
A kind of fused salt electrolysis process that adopts in resistance furnace prepares the method for titanium sponge, configuration globars and as heating unit in the resistance furnace, the top temperature of resistance furnace is not less than 950 ℃, and fused salt electrolysis process relates to plumbago crucible, and the plumbago crucible internal memory is placed with the calcium chloride fused salt, titanium dioxide is as cathode electrode sheet, graphite cake is as anode strip, and electrolytic process produces carbon monoxide and carbonic acid gas, and plumbago crucible places in the vacuum reactor, feed argon gas in the vacuum reactor, feature of the present invention is:
The plumbago crucible that is placed with the calcium chloride fused salt is placed in the vacuum reactor, afterwards vacuum reactor is placed in the resistance furnace that does not heat up, dispose annular cyclic water jacket and dispose lower linking tube at annular cyclic water jacket at the place, upper flanges right angle of vacuum reactor, at described flange upper end configuration annular seal groove, configuration high-temperature resistant seal ring in the described annular seal groove, the upper end of vacuum reactor is buckled with the loam cake of falling the concavity, the loam cake of falling the concavity connects by the double-level-metal mutual superposition and with ring flange and forms, form inner water sleeve between the described superimposed layer, inner water sleeve disposes upper connecting tube, there is the identical sealing gap of diameter the upper center both sides of the loam cake of falling concavity balanced configuration respectively, difference plug-in electrode bar in two sealing gaps, after connecting by cross bar, two battery lead rods connect with elevating lever again, lower end at a battery lead rod is wound with described cathode electrode sheet by Stainless Steel Wire, the gross weight control of described cathode electrode sheet is between 300～500g, lower end at another battery lead rod is plugged with described anode strip by stainless steel bar, the gross weight of described stainless steel bar+described anode strip and the gross weight of described cathode electrode sheet are complementary, the diameter coupling of the diameter of two battery lead rods and two sealing gaps, the upper end both sides external of the loam cake of falling concavity balanced configuration respectively has the identical inlet pipe of diameter and escape pipe, the length that inlet pipe puts in the vacuum reactor is as the criterion to reach the plumbago crucible upper end edge, the length that escape pipe puts in the loam cake of falling the concavity is as the criterion with described ring flange is concordant, by the vacuum-sealing that butt hole Bolt Connection and the described high-temperature resistant seal ring of described flange and described ring flange can be realized vacuum reactor and the loam cake of falling the concavity, install dw additional in the upper end of the loam cake of falling the concavity;
Earlier the calcium chloride fused salt in the plumbago crucible is hanged down the constant temperature divisional processing of drawing water, Control for Kiln Temperature in the resistance furnace is at 30～70 ℃ at this moment, in the vacuum reactor of sealing, feed argon gas by inlet pipe again behind the calcium fused salt moisture removal to be chlorinated, when forming malleation in the vacuum reactor of sealing, argon gas again the furnace temperature of resistance furnace is at the uniform velocity risen to 1000 ℃, can measure by temperature measurer when temperature reaches more than 950 ℃ in the vacuum reactor of sealing, again by automatic two battery lead rods that descend of elevating lever, making described cathode electrode sheet and described anode strip enter in the interior calcium chloride fused salt of plumbago crucible carries out electrolysis and prepares titanium sponge, all control at 50A at the electric current that described anode strip and described cathode electrode sheet pass through this moment, and the carbon monoxide that electrolytic process produces and carbonic acid gas and remaining argon gas are discharged in the waste gas withdrawing can by escape pipe, after the electrolytic preparation titanium sponge finishes again by rise automatically two battery lead rods and cut off the resistance furnace power supply of elevating lever, cut off the electric current that passes through on described anode strip and the described cathode electrode sheet and cut off the argon gas supply, the titanium sponge that makes described cathode electrode sheet power on to solve breaks away from the calcium chloride fused salt, meanwhile the vacuum reactor with sealing hangs out in resistance furnace, and in annular cyclic water jacket and inner water sleeve, feed water coolant by described lower linking tube and described upper connecting tube, when the vacuum reactor cool to room temperature of sealing, open the loam cake of falling the concavity and taking-up again by the described cathode electrode sheet of electrolysis, can obtain purity and reach 99.0% titanium sponge being cleaned by the described cathode electrode sheet of electrolysis.
Vacuum reactor and the loam cake of falling the concavity are made by 304 stainless steels.
Owing to adopt technical scheme as mentioned above, the present invention produces following positively effect:
1, according to the technological principle of fused salt electrolysis deoxidation; vacuum reactor of the present invention should satisfy the draw water requirement of divisional processing of low constant temperature; the titanium sponge that goes out for electrolytic preparation is built good argon shield coolant seal zone again; so vacuum reactor has the stopping property height, also has high-temperature corrosion resistance simultaneously.
2, advantage of the present invention is that vacuum reactor and the loam cake of falling the concavity have characteristics such as simple in structure, easy to operate, practical, makes the loss of environmental pollution and equipment consume the lower level that all reached.
Description of drawings
Fig. 1 is structure of the present invention and method simplified schematic diagram.
Among Fig. 1: 1-resistance furnace, 2-plumbago crucible, 3-titanium dioxide, 4-annular cyclic water jacket, 5-inner water sleeve, 6-inlet pipe, the 7-sealing gap, 8-elevating lever, 9-battery lead rod, the 10-escape pipe, the 11-loam cake of falling the concavity, 12-graphite cake, the 13-high-temperature resistant seal ring, 14-calcium chloride fused salt, 15-vacuum reactor, 16-globars.
Embodiment
The present invention is that a kind of fused salt electrolysis process that adopts in resistance furnace prepares the method for titanium sponge, it also is one of extended method of fused salt electrolysis in the fused salt electrolysis process, this method can prepare titanium sponge in a small amount, this is because the capacity of plumbago crucible is limit, if increase the capacity of plumbago crucible, also can increase the preparation amount of titanium sponge, this is apparent to this area.
Configuration globars 16 and as heating unit in the resistance furnace 1, the top temperature of resistance furnace 1 is not less than 950 ℃, fused salt electrolysis process relates to plumbago crucible 2, plumbago crucible 2 internal memories are placed with calcium chloride fused salt 14, and the amount of storage of calcium chloride fused salt 14 accounts for 2/3 of plumbago crucible 2 capacity and is advisable, and titanium dioxide 3 is as cathode electrode sheet, graphite cake 12 is as anode strip, electrolytic process produces carbon monoxide and carbonic acid gas, and plumbago crucible 2 places in the vacuum reactor 15, feeds argon gas in the vacuum reactor 15.
Above-mentioned resistance furnace 1 adopts is the conventional, electric-resistance stove and does not need high temperature to carry pressure, though resistance furnace 1 can satisfy demand of the present invention, resistance furnace 1 energy consumption is bigger.
Feature of the present invention is:
The plumbago crucible 2 that is placed with calcium chloride fused salt 14 is placed in the vacuum reactor 15, afterwards vacuum reactor 15 is placed in the resistance furnace 1 that does not heat up, dispose annular cyclic water jacket 4 and dispose lower linking tube at annular cyclic water jacket at the place, upper flanges right angle of vacuum reactor 15, at described flange upper end configuration annular seal groove, configuration high-temperature resistant seal ring 13 in the described annular seal groove, the upper end of vacuum reactor 15 is buckled with the loam cake of falling the concavity 11, the loam cake of falling the concavity 11 connects by the double-level-metal mutual superposition and with ring flange and forms, form inner water sleeve 5 between the described superimposed layer, inner water sleeve 5 disposes upper connecting tube, there is the identical sealing gap of diameter 7 the upper center both sides of the loam cake of falling the concavity 11 balanced configuration respectively, difference plug-in electrode bar 9 in two sealing gaps 7, after connecting by cross bar, two battery lead rods 9 connect with elevating lever 8 again, lower end at a battery lead rod is wound with described cathode electrode sheet by Stainless Steel Wire, the gross weight control of described cathode electrode sheet is between 300～500g, lower end at another battery lead rod is plugged with described anode strip by stainless steel bar, be plugged on the described stainless steel bar after the boring in the middle of the graphite cake 12, the gross weight of described stainless steel bar+described anode strip and the gross weight of described cathode electrode sheet are complementary, the diameter coupling of the diameter of two battery lead rods 9 and two sealing gaps 7, two sealing gaps 7 can effectively prevent in the vacuum reactor of air admission sealing, the upper end both sides external of the loam cake of falling the concavity 11 balanced configuration respectively has diameter identical inlet pipe 6 and escape pipe 10, the length that inlet pipe 6 puts in the vacuum reactor 15 is as the criterion to reach plumbago crucible 2 upper end edges, the length that escape pipe 10 puts in the loam cake of falling the concavity 11 is as the criterion with described ring flange is concordant, butt hole Bolt Connection by described flange and described ring flange and described high-temperature resistant seal ring can be realized the vacuum-sealing of vacuum reactor 15 and the loam cake of falling the concavity 11, state after vacuum reactor 15 and the loam cake of falling the concavity 11 vacuum-sealings abbreviates the vacuum reactor of sealing as, upper end at the loam cake of falling the concavity installs dw additional, described dw is to two sealing gaps 7, two battery lead rods 9, elevating lever 8 and described cross bar are implemented dust seal, and vacuum reactor 15 and the loam cake of falling the concavity 11 are made by 304 stainless steels.
Above-mentioned vacuum reactor 15 and the loam cake of falling the concavity 11 have characteristics such as simple in structure, easy to operate, practical, make environmental pollution and equipment loss consumption that titanium is smelted all reach lower level.
Earlier the calcium chloride fused salts 14 in the plumbago crucible 2 are hanged down the constant temperature divisional processing of drawing water, Control for Kiln Temperature in the resistance furnace 1 is at 50～80 ℃ at this moment, in the vacuum reactor of sealing, feed argon gas by inlet pipe 6 again behind calcium fused salt 14 moisture removals to be chlorinated, when forming malleation in the vacuum reactor of sealing, argon gas again the furnace temperature of resistance furnace 1 is at the uniform velocity risen to 1000 ℃, can measure by temperature measurer when temperature reaches more than 950 ℃ in the vacuum reactor of sealing, again by elevating lever 8 automatic two battery lead rods 9 that descend, making described cathode electrode sheet and described anode strip enter in the calcium chloride fused salt 14 in the plumbago crucible 2 carries out electrolysis and prepares titanium sponge, all control at 50A at the electric current that described anode strip and described cathode electrode sheet pass through this moment, and electric current can reach 50～70% by efficient.And the carbon monoxide that electrolytic process produces and carbonic acid gas and remaining argon gas are discharged in the waste gas withdrawing can by escape pipe 10, after the electrolytic preparation titanium sponge finishes again by rise automatically two battery lead rods 9 and cut off resistance furnace 1 power supply of elevating lever 8, cut off the electric current that passes through on described anode strip and the described cathode electrode sheet and cut off the argon gas supply, the titanium sponge that makes described cathode electrode sheet power on to solve breaks away from calcium chloride fused salt 14, meanwhile the vacuum reactor with sealing hangs out in resistance furnace 1, and in annular cyclic water jacket 4 and inner water sleeve 5, feed water coolants by described lower linking tube and described upper connecting tube, when the vacuum reactor cool to room temperature of sealing, open the loam cake of falling the concavity 11 and taking-up again by the described cathode electrode sheet of electrolysis, can obtain purity and reach 99.0% titanium sponge being cleaned by the described cathode electrode sheet of electrolysis.
Technological principle according to the fused salt electrolysis deoxidation; vacuum reactor 15 should satisfy the draw water requirement of divisional processing of described low constant temperature; the titanium sponge that goes out for electrolytic preparation is built good argon shield coolant seal zone again; so vacuum reactor 15 must have the stopping property height; namely require to have higher vacuum tightness, have high-temperature corrosion resistance simultaneously.
By above statement, the present invention can well finish the electrolytic preparation titanium sponge, and electrolysis goes out the more excellent titanium sponge of quality, makes the maturing more of FFC method, safe, energy-conservationization.
Claims (2)
1. one kind is adopted fused salt electrolysis process to prepare the method for titanium sponge in resistance furnace, configuration globars (16) and as heating unit in the resistance furnace (1), the top temperature of resistance furnace (1) is not less than 950 ℃, fused salt electrolysis process relates to plumbago crucible (2), plumbago crucible (2) internal memory is placed with calcium chloride fused salt (14), titanium dioxide (3) is as cathode electrode sheet, graphite cake (12) is as anode strip, electrolytic process produces carbon monoxide and carbonic acid gas, plumbago crucible (2) places in the vacuum reactor (15), feeds argon gas in the vacuum reactor (15); It is characterized in that:
The plumbago crucible (2) that will be placed with calcium chloride fused salt (14) places in the vacuum reactor (15), afterwards vacuum reactor (15) is placed in the resistance furnace (1) that does not heat up, dispose annular cyclic water jacket (4) and dispose lower linking tube at annular cyclic water jacket at the place, upper flanges right angle of vacuum reactor (15), at described flange upper end configuration annular seal groove, configuration high-temperature resistant seal ring (13) in the described annular seal groove, the upper end of vacuum reactor (15) is buckled with the loam cake of falling the concavity (11), the loam cake of falling the concavity (11) connects by the double-level-metal mutual superposition and with ring flange and forms, form inner water sleeve (5) between the described superimposed layer, inner water sleeve (5) disposes upper connecting tube, there is the identical sealing gap of diameter (7) the upper center both sides of the loam cake of falling the concavity (11) balanced configuration respectively, difference plug-in electrode bar (9) in two sealing gaps (7), two battery lead rods (9) connect with elevating lever (8) after connecting by cross bar again, lower end at a battery lead rod is wound with described cathode electrode sheet by Stainless Steel Wire, the gross weight control of described cathode electrode sheet is between 300～500g, lower end at another battery lead rod is plugged with described anode strip by stainless steel bar, the gross weight of described stainless steel bar+described anode strip and the gross weight of described cathode electrode sheet are complementary, the diameter coupling of the diameter of two battery lead rods (9) and two sealing gaps (7), the upper end both sides external of the loam cake of falling the concavity (11) balanced configuration respectively has the identical inlet pipe of diameter (6) and escape pipe (10), the length that inlet pipe (6) puts in the vacuum reactor (15) is as the criterion to reach plumbago crucible (2) upper end edge, the length that escape pipe (10) puts in the loam cake of falling the concavity (11) is as the criterion with described ring flange is concordant, by the vacuum-sealing that butt hole Bolt Connection and the described high-temperature resistant seal ring of described flange and described ring flange can be realized vacuum reactor (15) and the loam cake of falling the concavity (11), install dw additional in the upper end of the loam cake of falling the concavity (11);
Earlier the calcium chloride fused salt (14) in the plumbago crucible (2) is hanged down the constant temperature divisional processing of drawing water, Control for Kiln Temperature in resistance furnace this moment (1) is at 50～80 ℃, in the vacuum reactor of sealing, feed argon gas by inlet pipe (6) again behind calcium fused salt to be chlorinated (14) moisture removal, when forming malleation in the vacuum reactor of sealing, argon gas again the furnace temperature of resistance furnace (1) is at the uniform velocity risen to 1000 ℃, can measure by temperature measurer when temperature reaches more than 950 ℃ in the vacuum reactor of sealing, again by elevating lever (8) two battery lead rods (9) that descend automatically, making described cathode electrode sheet and described anode strip enter in the interior calcium chloride fused salt (14) of plumbago crucible (2) carries out electrolysis and prepares titanium sponge, all control at 50A at the electric current that described anode strip and described cathode electrode sheet pass through this moment, and the carbon monoxide that electrolytic process produces and carbonic acid gas and remaining argon gas are discharged in the waste gas withdrawing can by escape pipe (10), after the electrolytic preparation titanium sponge finishes again by rise automatically two battery lead rods (9) and cut off resistance furnace (1) power supply of elevating lever (8), cut off the electric current that passes through on described anode strip and the described cathode electrode sheet and cut off the argon gas supply, the titanium sponge that makes described cathode electrode sheet power on to solve breaks away from calcium chloride fused salt (14), meanwhile the vacuum reactor with sealing hangs out in resistance furnace (1), and by described lower linking tube and described upper connecting tube feeding water coolant in annular cyclic water jacket (4) and the inner water sleeve (5), when the vacuum reactor cool to room temperature of sealing, open the loam cake of falling the concavity (11) and taking-up again by the described cathode electrode sheet of electrolysis, can obtain purity and reach 99.0% titanium sponge being cleaned by the described cathode electrode sheet of electrolysis.
2. prepare the method for titanium sponge according to the described a kind of fused salt electrolysis process that adopts of claim 1 in resistance furnace, it is characterized in that: vacuum reactor (15) and the loam cake of falling the concavity (11) are made by 304 stainless steels.
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| CN104613760A (en) * | 2014-12-30 | 2015-05-13 | 朱兴发 | Large-diameter circular ring stacked high-purity graphite crucible for electromagnetic induction slag smelter |
| CN105420762A (en) * | 2015-11-25 | 2016-03-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Electrolytic bath structure and molten salt electrolysis method |
| CN105568320A (en) * | 2016-02-24 | 2016-05-11 | 宁夏德运特种冶金有限公司 | Device and method for industrially producing high-purity titanium through fused salt electrolysis process |
| CN109781616A (en) * | 2017-11-13 | 2019-05-21 | 广西大学 | It is a kind of for detecting the experimental rig corroded in molten salt reactor and detection method |
| CN110468434A (en) * | 2019-09-09 | 2019-11-19 | 华北理工大学 | A kind of fused salt electro-deposition prepares titanium corrosion-inhibiting coating technique |
| CN111945188A (en) * | 2020-07-20 | 2020-11-17 | 超威电源集团有限公司 | Molten salt primary battery method lead-based master alloy preparation device and preparation method |
| CN112280998A (en) * | 2020-11-19 | 2021-01-29 | 宝钛华神钛业有限公司 | Closed cycle method titanium sponge production facility of easy operation |
| CN113881975A (en) * | 2021-10-19 | 2022-01-04 | 杭州嘉悦智能设备有限公司 | Fused salt chlorination electrolytic furnace and control method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103728353A (en) * | 2013-12-18 | 2014-04-16 | 中国原子能科学研究院 | Sealed high-temperature electrochemical measuring device |
| CN103728353B (en) * | 2013-12-18 | 2016-03-30 | 中国原子能科学研究院 | A kind of sealing high-temperature electrochemistry measurement mechanism |
| CN104613760A (en) * | 2014-12-30 | 2015-05-13 | 朱兴发 | Large-diameter circular ring stacked high-purity graphite crucible for electromagnetic induction slag smelter |
| CN105420762A (en) * | 2015-11-25 | 2016-03-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Electrolytic bath structure and molten salt electrolysis method |
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| CN105568320A (en) * | 2016-02-24 | 2016-05-11 | 宁夏德运特种冶金有限公司 | Device and method for industrially producing high-purity titanium through fused salt electrolysis process |
| CN109781616A (en) * | 2017-11-13 | 2019-05-21 | 广西大学 | It is a kind of for detecting the experimental rig corroded in molten salt reactor and detection method |
| CN110468434A (en) * | 2019-09-09 | 2019-11-19 | 华北理工大学 | A kind of fused salt electro-deposition prepares titanium corrosion-inhibiting coating technique |
| CN111945188A (en) * | 2020-07-20 | 2020-11-17 | 超威电源集团有限公司 | Molten salt primary battery method lead-based master alloy preparation device and preparation method |
| CN112280998A (en) * | 2020-11-19 | 2021-01-29 | 宝钛华神钛业有限公司 | Closed cycle method titanium sponge production facility of easy operation |
| CN113881975A (en) * | 2021-10-19 | 2022-01-04 | 杭州嘉悦智能设备有限公司 | Fused salt chlorination electrolytic furnace and control method thereof |
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