CN103334126B - A kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace - Google Patents
A kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace Download PDFInfo
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- CN103334126B CN103334126B CN201310238776.2A CN201310238776A CN103334126B CN 103334126 B CN103334126 B CN 103334126B CN 201310238776 A CN201310238776 A CN 201310238776A CN 103334126 B CN103334126 B CN 103334126B
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Abstract
A kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace, carry out low constant temperature to the calcium chloride fused salt (14) in plumbago crucible (2) to draw water divisional processing, in the vacuum reactor of sealing, argon gas is passed into by inlet pipe (6) after moisture removal, resistance furnace (1) at the uniform velocity rises to 1000 DEG C, by elevating lever (8) automatically decline two battery lead rods (9) titanium dioxide (3) and graphite cake (12) are entered plumbago crucible is interior and electric current is 50A, the carbon monoxide that electrolysis produces and carbonic acid gas and remaining argon gas are discharged in waste gas recovery tank by escape pipe (10), after electrolytic preparation titanium sponge terminates, the vacuum reactor of sealing is hung out, water coolant is passed in annular cyclic water jacket (4) and inner water sleeve (5), to opening the upper cover of falling concavity (11) during room temperature and taking out by the titanium dioxide of electrolysis, the titanium sponge that purity reaches 99.0% can be obtained through cleaning, there is maturing, safe, energy-saving.
Description
Technical field
The invention belongs to technical field of smelting, be related specifically to a kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace.
Background technology
The smelting technology comparative maturity of titanium be Kroll method, Kroll method is discrete, and not only production cost is high, equipment loss is large, and environmental pollution is serious.
For reducing its production cost and expanding the scale of production, also have and adopt FFC fused salt electrolysis process, 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 cleaning → detect
Above-mentioned fused salt electrolysis is the critical process of fused salt electrolysis process, concrete grammar is exactly the titanium dioxide prepared is cathode electrode sheet, with fine and close graphite cake for anode, electrolysis is carried out in the high-temperature molten salt of calcium chloride, electrolysis temperature 950 DEG C, bath voltage 3V, from negative electrode titanium dioxide electrodes sheet, ionize out oxonium ion in electrolytic process and move to anode and carry out electric discharge and generate carbon monoxide and carbonic acid gas and release from electrolyzer, titanium metal in cathode electrode sheet is retained, after electrolysis completes, promote battery lead rod cathode electrode sheet to be placed in resistance furnace and to naturally cool to room temperature with stove under argon shield, open bell take out cathode electrode sheet and can titanium sponge be obtained after cleaning.
The vacuum leakproofness of above-mentioned fused salt electrolysis process is poor, and the corrodibility of high temperature resistant molten salt is also poor.
Patent publication No. CN2778832Y discloses the fused-salt bath that a kind of direct titanium dioxide is raw material production titanium sponge, describe the making method of this electrolyzer and describe 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 in fused salt electrolysis process the problems such as the vacuum leakproofness corrodibility that is poor, high temperature resistant molten salt existed is poor, the invention provides a kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace, titanium sponge can be gone out by electrolytic preparation very well by the method, and electrolysis mass preferably titanium sponge, make the maturing more of FFC fused salt electrolysis process, safe, energy-saving.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace, configuration globars in resistance furnace as heating unit, the top temperature of resistance furnace is not less than 950 DEG C, and fused salt electrolysis process relates to plumbago crucible, and plumbago crucible internal memory is placed with 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 is placed in vacuum reactor, pass into argon gas in vacuum reactor, feature of the present invention is:
The plumbago crucible being placed with calcium chloride fused salt is placed in vacuum reactor, afterwards vacuum reactor is placed in the resistance furnace do not heated up, be configured with annular cyclic water jacket in the upper flanges right angle of vacuum reactor and be configured with lower linking tube at annular cyclic water jacket, at described flange upper end configuration annular seal groove, configuration high-temperature resistant seal ring in described annular seal groove, the upper end of vacuum reactor is buckled with the upper cover of falling concavity, the upper cover of falling concavity is mutually superposed by double-level-metal and is connected with ring flange and forms, inner water sleeve is formed between described superimposed layer, inner water sleeve is configured with upper connecting tube, the upper center both sides of the upper cover of falling concavity are the balanced configuration sealing gap that has diameter identical respectively, difference plug-in electrode bar in two sealing gaps, connect with elevating lever again after two battery lead rods are connected by cross bar, described cathode electrode sheet is wound with by Stainless Steel Wire in the lower end of a battery lead rod, the gross weight of described cathode electrode sheet controls between 300 ~ 500g, described anode strip is plugged with by stainless steel bar in the lower end of another battery lead rod, the gross weight of described stainless steel bar+described anode strip and the gross weight of described cathode electrode sheet match, the diameter matches of the diameter of two battery lead rods and two sealing gaps, the upper end both sides external of the upper cover of falling concavity is the balanced configuration inlet pipe that has diameter identical and escape pipe respectively, the length that inlet pipe puts in vacuum reactor is as the criterion to reach plumbago crucible upper end edge, escape pipe puts in that the length of the upper cover of falling concavity is concordant with described ring flange to be as the criterion, the vacuum-sealing of vacuum reactor and the upper cover of falling concavity can be realized by the butt hole bolt-connection of described flange and described ring flange and described high-temperature resistant seal ring, dw is installed additional in the upper end of the upper cover of falling concavity,
First carry out low constant temperature to the calcium chloride fused salt in plumbago crucible to draw water divisional processing, Control for Kiln Temperature now in resistance furnace is at 30 ~ 70 DEG C, in the vacuum reactor of sealing, argon gas is passed into by inlet pipe again after calcium fused salt moisture removal to be chlorinated, again the furnace temperature of resistance furnace is at the uniform velocity risen to 1000 DEG C when argon gas forms malleation in the vacuum reactor sealed, when in the vacuum reactor can being measured sealing by temperature measurer, temperature reaches more than 950 DEG C, automatically to be declined two battery lead rods by elevating lever again, carry out electrolysis in the calcium chloride fused salt making described cathode electrode sheet and described anode strip enter in plumbago crucible and prepare titanium sponge, the electric current now passed through on described anode strip and described cathode electrode sheet all controls at 50A, and the carbon monoxide that electrolytic process produces and carbonic acid gas and remaining argon gas are discharged in waste gas recovery tank by escape pipe, automatically to be risen two battery lead rods cut off resistance furnace power supply by elevating lever again after electrolytic preparation titanium sponge terminates, cut off electric current and the supply of cut-out argon gas that described anode strip and described cathode electrode sheet pass through, the titanium sponge described cathode electrode sheet being powered on solve departs from calcium chloride fused salt, meanwhile the vacuum reactor of sealing is hung out in resistance furnace, and in annular cyclic water jacket and inner water sleeve, pass into water coolant by described lower linking tube and described upper connecting tube, open when the vacuum reactor cool to room temperature sealed the upper cover of falling concavity again and take out by the described cathode electrode sheet of electrolysis, the titanium sponge that purity reaches 99.0% can be obtained to being carried out cleaning by the described cathode electrode sheet of electrolysis.
Vacuum reactor and the upper cover of falling concavity are made by 304 stainless steels.
Owing to adopting technical scheme described 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 meet low constant temperature and to draw water the requirement of divisional processing; good argon shield coolant seal region built by the titanium sponge gone out for electrolytic preparation again; so vacuum reactor to have stopping property high, also there is high temperature corrosion simultaneously.
2, advantage of the present invention is that vacuum reactor and the upper cover of falling concavity have the features such as structure is simple, easy to operate, practical, environmental pollution and equipment loss is consumed and all reaches lower level.
Accompanying drawing explanation
Fig. 1 is structure of the present invention and method simplified schematic diagram.
In Fig. 1: 1-resistance furnace, 2-plumbago crucible, 3-titanium dioxide, 4-annular cyclic water jacket, 5-inner water sleeve, 6-inlet pipe, 7-sealing gap, 8-elevating lever, 9-battery lead rod, 10-escape pipe, the 11-upper cover of falling concavity, 12-graphite cake, 13-high-temperature resistant seal ring, 14-calcium chloride fused salt, 15-vacuum reactor, 16-globars.
Embodiment
The present invention is a kind of method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace, also be one of extended method of fused salt electrolysis in fused salt electrolysis process, the method can prepare titanium sponge in a small amount, this is because the capacity of plumbago crucible 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 in resistance furnace 1 as heating unit, the top temperature of resistance furnace 1 is not less than 950 DEG C, fused salt electrolysis process relates to plumbago crucible 2, plumbago crucible 2 internal memory is 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 is placed in vacuum reactor 15, passes into argon gas in vacuum reactor 15.
What above-mentioned resistance furnace 1 adopted is conventional, electric-resistance stove and does not need high temperature to carry pressure, although resistance furnace 1 can meet demand of the present invention, resistance furnace 1 energy consumption is larger.
Feature of the present invention is:
The plumbago crucible 2 being placed with calcium chloride fused salt 14 is placed in vacuum reactor 15, afterwards vacuum reactor 15 is placed in the resistance furnace 1 do not heated up, be configured with annular cyclic water jacket 4 in the upper flanges right angle of vacuum reactor 15 and be configured with lower linking tube at annular cyclic water jacket, at described flange upper end configuration annular seal groove, configuration high-temperature resistant seal ring 13 in described annular seal groove, the upper end of vacuum reactor 15 is buckled with the upper cover of falling concavity 11, the upper cover of falling concavity 11 is mutually superposed by double-level-metal and is connected with ring flange and forms, inner water sleeve 5 is formed between described superimposed layer, inner water sleeve 5 is configured with upper connecting tube, the upper center both sides of the upper cover of falling concavity 11 are the balanced configuration sealing gap 7 that has diameter identical respectively, difference plug-in electrode bar 9 in two sealing gaps 7, connect with elevating lever 8 again after two battery lead rods 9 are connected by cross bar, described cathode electrode sheet is wound with by Stainless Steel Wire in the lower end of a battery lead rod, the gross weight of described cathode electrode sheet controls between 300 ~ 500g, described anode strip is plugged with by stainless steel bar in the lower end of another battery lead rod, be plugged on after graphite cake 12 central bore on described stainless steel bar, the gross weight of described stainless steel bar+described anode strip and the gross weight of described cathode electrode sheet match, the diameter matches of the diameter of two battery lead rods 9 and two sealing gaps 7, two sealing gaps 7 can effectively prevent air from entering in the vacuum reactor of sealing, the upper end both sides external of the upper cover of falling concavity 11 is the balanced configuration inlet pipe 6 that has diameter identical and escape pipe 10 respectively, the length that inlet pipe 6 puts in vacuum reactor 15 is as the criterion to reach plumbago crucible 2 upper end edge, escape pipe 10 puts in that the length of the upper cover of falling concavity 11 is concordant with described ring flange to be as the criterion, the vacuum-sealing of vacuum reactor 15 and the upper cover of falling concavity 11 can be realized by the butt hole bolt-connection of described flange and described ring flange and described high-temperature resistant seal ring, state after vacuum reactor 15 and the upper cover of falling concavity 11 vacuum-sealing is referred to as the vacuum reactor sealed, dw is installed additional in the upper end of the upper cover of falling concavity, described dw is to two sealing gaps 7, two battery lead rods 9, dust seal implemented by elevating lever 8 and described cross bar, vacuum reactor 15 and the upper cover of falling concavity 11 are made by 304 stainless steels.
Above-mentioned vacuum reactor 15 and the upper cover of falling concavity 11 have the features such as structure is simple, easy to operate, practical, and the environmental pollution that titanium is smelted and equipment loss consume and all reach lower level.
First carry out low constant temperature to the calcium chloride fused salt 14 in plumbago crucible 2 to draw water divisional processing, Control for Kiln Temperature now in resistance furnace 1 is at 50 ~ 80 DEG C, in the vacuum reactor of sealing, argon gas is passed into by inlet pipe 6 again after calcium fused salt 14 moisture removal to be chlorinated, again the furnace temperature of resistance furnace 1 is at the uniform velocity risen to 1000 DEG C when argon gas forms malleation in the vacuum reactor sealed, when in the vacuum reactor can being measured sealing by temperature measurer, temperature reaches more than 950 DEG C, again by elevating lever 8 decline two battery lead rods 9 automatically, carry out electrolysis in the calcium chloride fused salt 14 making described cathode electrode sheet and described anode strip enter in plumbago crucible 2 and prepare titanium sponge, the electric current now passed through on described anode strip and described cathode electrode sheet all controls at 50A, electric current can reach 50 ~ 70% by efficiency.And the carbon monoxide that electrolytic process produces and carbonic acid gas and remaining argon gas are discharged in waste gas recovery tank by escape pipe 10, automatically to be risen two battery lead rods 9 cut off resistance furnace 1 power supply by elevating lever 8 again after electrolytic preparation titanium sponge terminates, cut off electric current and the supply of cut-out argon gas that described anode strip and described cathode electrode sheet pass through, the titanium sponge described cathode electrode sheet being powered on solve departs from calcium chloride fused salt 14, meanwhile the vacuum reactor of sealing is hung out in resistance furnace 1, and in annular cyclic water jacket 4 and inner water sleeve 5, pass into water coolant by described lower linking tube and described upper connecting tube, open the upper cover of falling concavity 11 again when the vacuum reactor cool to room temperature sealed and take out by the described cathode electrode sheet of electrolysis, the titanium sponge that purity reaches 99.0% can be obtained to being carried out cleaning by the described cathode electrode sheet of electrolysis.
According to the technological principle of fused salt electrolysis deoxidation; vacuum reactor 15 should meet described low constant temperature and to draw water the requirement of divisional processing; good argon shield coolant seal region built by the titanium sponge gone out for electrolytic preparation again; so vacuum reactor 15 must to have stopping property high; namely require that there is higher vacuum tightness, there is high temperature corrosion simultaneously.
By above statement, the present invention can well complete electrolytic preparation titanium sponge, and electrolysis mass preferably titanium sponge, make the maturing more of FFC method, safe, energy-saving.
Claims (1)
1. the method adopting fused salt electrolysis process to prepare titanium sponge in resistance furnace, configuration globars (16) in resistance furnace (1) as heating unit, the top temperature of resistance furnace (1) is not less than 950 DEG C, 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) is placed in vacuum reactor (15), vacuum reactor passes into argon gas in (15), it is characterized in that:
The plumbago crucible (2) being placed with calcium chloride fused salt (14) is placed in vacuum reactor (15), afterwards vacuum reactor (15) is placed in the resistance furnace (1) do not heated up, be configured with annular cyclic water jacket (4) in the upper flanges right angle of vacuum reactor (15) and be configured with lower linking tube at annular cyclic water jacket, at described flange upper end configuration annular seal groove, configuration high-temperature resistant seal ring (13) in described annular seal groove, the upper end of vacuum reactor (15) is buckled with the upper cover of falling concavity (11), the upper cover of falling concavity (11) is mutually superposed by double-level-metal and is connected with ring flange and forms, described double-level-metal superposes formation superimposed layer mutually, inner water sleeve (5) is formed between described superimposed layer, inner water sleeve (5) is configured with upper connecting tube, the upper center both sides of the upper cover of falling concavity (11) are the balanced configuration sealing gap (7) that has diameter identical respectively, difference plug-in electrode bar (9) in two sealing gaps (7), connect with elevating lever (8) again after two battery lead rods (9) are connected by cross bar, described cathode electrode sheet is wound with by Stainless Steel Wire in the lower end of a battery lead rod, the gross weight of described cathode electrode sheet controls at 300 ~ 500g, described anode strip is plugged with by stainless steel bar in the lower end of another battery lead rod, the gross weight of described stainless steel bar+described anode strip and the gross weight of described cathode electrode sheet match, the diameter of two battery lead rods (9) and the diameter matches of two sealing gaps (7), the upper end both sides external of the upper cover of falling concavity (11) is the balanced configuration inlet pipe (6) that has diameter identical and escape pipe (10) respectively, the length that inlet pipe (6) puts in vacuum reactor (15) is as the criterion to reach plumbago crucible (2) upper end edge, escape pipe (10) puts in that the length of the upper cover of falling concavity (11) is concordant with described ring flange to be as the criterion, the vacuum-sealing of vacuum reactor (15) and the upper cover of falling concavity (11) can be realized by the butt hole bolt-connection of described flange and described ring flange and described high-temperature resistant seal ring, dw is installed additional in the upper end of the upper cover of falling concavity (11),
First carry out low constant temperature to the calcium chloride fused salt (14) in plumbago crucible (2) to draw water divisional processing, Control for Kiln Temperature now in resistance furnace (1) is at 50 ~ 80 DEG C, in the vacuum reactor of sealing, argon gas is passed into by inlet pipe (6) again after calcium fused salt (14) moisture removal to be chlorinated, again the furnace temperature of resistance furnace (1) is at the uniform velocity risen to 1000 DEG C when argon gas forms malleation in the vacuum reactor sealed, when in the vacuum reactor can being measured sealing by temperature measurer, temperature reaches more than 950 DEG C, again by elevating lever (8) decline two battery lead rods (9) automatically, carry out electrolysis in the calcium chloride fused salt (14) making described cathode electrode sheet and described anode strip enter in plumbago crucible (2) and prepare titanium sponge, the electric current now passed through on described anode strip and described cathode electrode sheet all controls at 50A, and the carbon monoxide that electrolytic process produces and carbonic acid gas and remaining argon gas are discharged in waste gas recovery tank by escape pipe (10), automatically to be risen two battery lead rods (9) cut off resistance furnace (1) power supply by elevating lever (8) again after electrolytic preparation titanium sponge terminates, cut off electric current and the supply of cut-out argon gas that described anode strip and described cathode electrode sheet pass through, the titanium sponge described cathode electrode sheet being powered on solve departs from calcium chloride fused salt (14), meanwhile the vacuum reactor of sealing is hung out in resistance furnace (1), and in annular cyclic water jacket (4) and inner water sleeve (5), pass into water coolant by described lower linking tube and described upper connecting tube, open the upper cover of falling concavity (11) again when the vacuum reactor cool to room temperature sealed and take out by the described cathode electrode sheet of electrolysis, the titanium sponge that purity reaches 99.0% can be obtained to being carried out cleaning by the described cathode electrode sheet of electrolysis, vacuum reactor (15) and the upper cover of falling concavity (11) are made by 304 stainless steels.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105420762B (en) * | 2015-11-25 | 2018-11-16 | 成都先进金属材料产业技术研究院有限公司 | Cell construction 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 |
| CN111945188B (en) * | 2020-07-20 | 2023-02-10 | 超威电源集团有限公司 | Molten salt primary battery method lead-based master alloy preparation device and preparation method |
| CN112280998B (en) * | 2020-11-19 | 2022-04-29 | 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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