CN103060850A - Method for preparing metallic titanium through continuous fused-salt electrolysis - Google Patents
Method for preparing metallic titanium through continuous fused-salt electrolysis Download PDFInfo
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- CN103060850A CN103060850A CN201310039416XA CN201310039416A CN103060850A CN 103060850 A CN103060850 A CN 103060850A CN 201310039416X A CN201310039416X A CN 201310039416XA CN 201310039416 A CN201310039416 A CN 201310039416A CN 103060850 A CN103060850 A CN 103060850A
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Abstract
The invention provides a method for preparing metallic titanium through continuous fused-salt electrolysis. The method is characterized by comprising the following steps of: 1, pelleting titanium dioxide by directly using a pelleting machine to prepare titanium dioxide pellets; 2, adding the prepared titanium dioxide pellets into a melting bath; 3, during electrolysis, connecting the positive electrode of an electrolysis power supply with the anode of an electrolytic bath, and connecting the cathode of the electrolysis power supply with the melding bath, and after the electrolysis, carrying out a discharging process step; and 4, heating a flow guide tube during discharging, opening a ball valve to ensure that liquid titanium flows into a receiving crucible of a cooling chamber through the flow guide tube, closing the ball valve after discharging, cooling the product in the cooling chamber, and taking titanium ingots out of the cooling chamber by opening a door of the cooling chamber. By adopting the method, the electrolysis of titanium dioxide can be continuously carried out, so that the production cost of titanium can be greatly reduced.
Description
Technical field
The present invention relates to a kind of method of continuous electrolysis titanium, particularly a kind of continuous fused salt electrolysis prepares the method for metal titanium.
Background technology
The premium propertiess such as titanium or titanium alloy has that light specific gravity, specific tenacity are high, creep-resistant property is good, corrosion-resistant under the high temperature, extensively be used as structured material in aerospace, metallurgy, automobile and other industries, simultaneously can also be as functional materials such as hydrogen storage material, shape memory alloy material etc.The production technique of titanium sponge is the Kroll method at present, be also referred to as magnesium reduction process, the method is that elder generation is by the mineral producing titanium tetrachloride t 5 bx of titaniferous, thereby make titanium sponge with the magnesium reduction titanium tetrachloride again, make fine and close titanium ingot finally by crossing vacuum consumable electricity arc melting, then make the finished product through mechanical means such as rolling, turning.Although existing magnesium reduction is the industrial process of comparative maturity, but because there are the problems such as technical process is long, operation is many, energy consumption is high, can not produce continuously in production process, and used metallic reducing agent magnesium also is to be obtained by electrolysis, therefore production cost is high, environmental pollution is serious, has limited the application of titanium.In order to reduce the production cost of titanium, the researchist of countries in the world actively seeks new low cost titanium metallurgical technology, wherein the most representative is that professor Fray of Cambridge University etc. has proposed a kind of novel process that titanium sponge is produced in the negative electrode deoxidation in fused calcium chloride take titanium dioxide as raw material, the cost of the method is lower than Kroll method, therefore oxide electrolysis direct production metal titanium becomes the study hotspot that titanium is smelted, but itself there is intrinsic shortcoming in this technique, be exactly that titanium dioxide is done again deoxidation of negative electrode, it is slow that oxygen is diffused into anode speed from negative plate, and current efficiency is low.The inventor's application number provides a kind of method of preparing metallic titanium with high temperature fused salt electrolysis of titanium dioxide for CN2008101186163's in first to file, the method is added water and binding agent when granulation, exist the dry time longer, energy consumption is very high, and the use of binding agent is so that destroy the problems such as furnace atmosphere, increase foreign matter content when temperature is high.
Summary of the invention
For the problems referred to above, the applicant is on the basis to its further further investigation, a kind of method by high temperature fused salt electrolysis titanium dioxide continuous production metal titanium has been proposed, the method can overcome the problems referred to above, thereby solves the series of problems such as the technical process that exists in the prior art is long, operation is many, energy consumption is high, can not produce continuously, impurity is many.
Technical scheme of the present invention has provided the method that a kind of continuous fused salt electrolysis prepares metal titanium, and described method adopts following steps to implement:
The first step, titanium dioxide directly being carried out granulation with tablets press, make the particle that granularity is 2-8mm, is that the particle of 2-8mm makes the titanium dioxide pelletizing with granularity behind temperature 150-300 ℃ of lower drying treatment 20-30min;
Second step, the titanium dioxide pelletizing for preparing is joined in the molten bath, ionogen is added in the molten bath, described ionogen is the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, and the weight percent content of lithium fluoride is 5-20% in this fused salt mixt; The ionogen add-on is 2/3 of molten bath capacity, titanium high-temperature electrolysis stove evacuation degree to 1 * 10
-1-5 * 10
-3Pa is filled with argon gas in titanium high-temperature electrolysis stove, keeping electrolysis pressure is 10-100Pa;
When the 3rd step, electrolysis, the positive pole of electrolysis power is connected with electrolytic cell anode, and the negative pole of electrolysis power links to each other with the molten bath, and anode electrode adopts graphite material processing; At electric power outputting current 1-30kA, carry out electrolysis under the electrolysis temperature 1800-1900 ℃ condition, behind the electrolysis 50-900min, begin to enter out material process;
The heating thrust-augmenting nozzle makes the temperature in its exit reach 1800-1900 ℃ when the 4th step, discharging, opens ball valve, and titanium liquid is flow in the reception crucible of cooling room by thrust-augmenting nozzle, after discharging is complete, closes ball valve; Product is after the cooling room cooling, and the door of opening cooling room takes out the titanium ingot.
The invention has the beneficial effects as follows: the present invention by under the high temperature take Graphite Electrodes as anode, take the titanium dioxide raw material as negative electrode, in the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, carry out electrolysis, titanium dioxide is liquid titanium by electrolytic reduction, because the difference of density, titanium sinks to the lowest layer, after the titanium of accumulation reaches certain amount, from the High Temperature Furnaces Heating Apparatus bottom discharge.Because the oxygen anion velocity of diffusion is fast under the high temperature, thereby accelerated deoxidation speed, thereby the method current efficiency is high, power consumption is low, simultaneously because the resultant metal titanium is liquid, can make the titanium dioxide electrolysis realize serialization, production cost that therefore can the decrease titanium, relatively can save energy 50% with traditional technology, current efficiency is brought up to more than 90%.
Description of drawings
Below with reference to attached Fig. 1 and 2 titanium high-temperature electrolysis stove of the present invention is elaborated, wherein:
Fig. 1 is the synoptic diagram of the high-temperature electrolysis stove for high temperature fused salt electrolysis titanium dioxide continuous production metal titanium of the present invention;
Fig. 2 is the synoptic diagram of the high-temperature electrolysis furnace system for high temperature fused salt electrolysis titanium dioxide continuous production metal titanium of the present invention.
Wherein: the 1-molten bath, the 2-Heating element, the 3-thermoscreen, the 4-insulating cotton, 5-is with the furnace shell of water jacket, 6-is with the bell of water jacket, 7-refractory brick, the 8-filling tube, the 9-electrode, the 10-thrust-augmenting nozzle, the 11-heating unit, 12-drawing mechanism thermoscreen, 13-drawing mechanism refractory brick, 14-discharge chamber shell, the 15-valve seat, the 16-spheroid, the 17-valve rod, 18-discharging crucible, the 19-cooling room, the 20-rectifier, the 21-transformer, the 22-feeder, 23-electrode dop, 24-electrode holder gripping arm, the 25-tank room, the 26-discharge chamber, the 27-column guide rail, the 28-exhaust gas processing device.
Embodiment
The titanium high-temperature electrolysis furnace system that the present invention relates to mainly comprises high-temperature electrolysis stove, rectifier 20, transformer 21, conductive cross arm, feeder 22, exhaust gas processing device 28.
In this invention, tank room 25 mainly comprises molten bath 1, Heating element 2, thermoscreen 3, insulating cotton 4, with the furnace shell 5 of water jacket with the bell 6 of water jacket, and wherein tank room 25 is rectangular parallelepiped, long 3m, wide 1.5m, high 2m.Refractory brick 7 is laid in tank room 25 bottoms.Molten bath 1 is rectangle, is positioned at the center of tank room 25, is made by graphite material, is used as the electrolyzer that high temperature fused salt electrolysis is used, and doublely in the process of electrolysis does the negative electrode that fused salt electrolysis is used.Around 1 outer side, the 5 ~ 10cm of distance molten bath Heating element 2 is installed, Heating element 2 is parallel with the sidewall in molten bath 1, and Heating element 2 is made by graphite material.For improving the homogeneity of temperature field in furnace, burner hearth is divided into four district's temperature controls, and every district consists of the closed loop loop, carries out temperature control.For heat lost by radiation and the accumulation of heat loss that reduces further the furnace wall, improve the thermo-efficiency of stove, the graphite thermoscreen 3 that be arranged in parallel around Heating element 2, thermoscreen 3 forms rectangles around heating unit 2, and its Main Function is heat insulation, insulation and reduces thermosteresis.Fill insulating cotton 4 at the outer of thermoscreen 3 with between with the furnace shell 5 of water jacket, to reduce the loss of heat.Furnace shell 5 with water jacket is rectangle, is processed by the rolled sheet material with good welds performance, for preventing heating inhomogeneous distortion and the protection sealing-ring of causing, is welded with water jacket around furnace shell.The furnace shell 5 with water jacket with the bell 6 of water jacket and tank room 25 is connected by flange, and there is high-temperature seal ring the centre, can guarantee the sealing of tank room 25.In order to prevent that thermal radiation from causing the overheated and distortion of bell, and the protection sealing element, be welded with watercooling jacket at the upper surface of bell.Tank room 25 has equally distributed one or more electrode ports with the bell 6 of water jacket, and electrode 9 adopts one or more Graphite Electrodes, and electrode diameter is 100 ~ 700mm, and electrode 9 inserts the stove from the bell over top, and electrode can be distinguished independent the adjustment during work.For guaranteeing furnace atmosphere and insulation, sealing and seal are arranged between electrode 9 and the bell 6 with water jacket.In order to guarantee carrying out continuously of electrolysis, at tank room 25 one or more filling tubes 8 that evenly distribute on the bell 6 of water jacket, filling tube 8 is with tightness system, has to prevent from dispelling the heat, prevent the function of leaking gas.With the bell 6 of water jacket liquid titanium drawing mechanism is set at tank room 25, realizes the opening and closing of liquid titanium drawing mechanism by pneumatics.
The below of tank room 25 is discharge chambers 26, the liquid titanium is flow into the cooling room 19 from the molten bath 1 of tank room 25 cool off.Discharge chamber 26 mainly is comprised of thrust-augmenting nozzle 10, heating unit 11, drawing mechanism thermoscreen 12, drawing mechanism refractory brick 13 and discharge chamber shell 14.Thrust-augmenting nozzle 10 is made by graphite material, links to each other with the valve seat 15 of 1 bottom, molten bath, is deep in the cooling room 19 always.Solidify in order to prevent that liquid titanium temperature reduces in the discharging process, guarantee that the temperature of thrust-augmenting nozzle 10 more than the fusing point of titanium, makes titanium in the liquid state bottom discharge, around thrust-augmenting nozzle 10, be provided with heating unit 11, be used for heating thrust-augmenting nozzle 10, heating unit 11 is made by graphite material.In order to reduce thermal radiation, 3 ~ 5 layers of concentric round shape drawing mechanism thermoscreen 12 are set around heating unit 11, drawing mechanism thermoscreen 12 is made by graphite material.At the drawing mechanism thermoscreen 12 outer drawing mechanism refractory brick 13 that arrange.Be with stainless steel casing 14 outward.Tank room 25 and discharge chamber 26 link to each other by flange, and discharge chamber 26 and cooling room 19 link to each other by flange.
The High Temperature Furnaces Heating Apparatus integral sealing with the pre-picking device of vacuum pump, before heating up is discharged furnace air, then is filled with argon gas, carries out electrolysis under argon shield atmosphere.
Transformer 21 is magnetic transformer, range of regulation is 10V-110V, its Main Function provides the power supply of high-temperature electrolysis stove heating usefulness, and the leading-out end of transformer 21 links to each other with the water-cooled copper electrode of high-temperature electrolysis stove, thereby by adjusting the temperature of voltage control high-temperature electrolysis stove.
The effect of conductive cross arm is to control Graphite Electrodes, drives rise fall of electrodes.Conductive cross arm mainly is comprised of electrode dop 23, electrode holder gripping arm 24, column guide rail 27, steel platform.Electrode holder gripping arm 24 links to each other with electrode dop 23,23 clampings of electrode dop have Graphite Electrodes 9, by dop Graphite Electrodes is fixed, hoist cylinder is housed in the column, effect by hoist cylinder, moving up and down of control conductive cross arm, thus electrode can be regulated according to the Expenditure Levels of electrode.The motion of oil cylinder is to control by Hydraulic Station.
Along with the carrying out of electrolysis, raw material consumes constantly, for guaranteeing carrying out continuously and the stability of electrolysis process of electrolysis, needs constantly to replenish raw material titanium dioxide in electrolytic process.Titanium dioxide is to add by feeder 22, feeder 22 comprises casing, feed leakage bucket, metallic hose and leakage material steel pipe, one end of feed leakage bucket is rectangular aperture, fixedly is communicated with the lower ending opening of casing by flanged plate, and the other end is circular open, this circular open fixedly is communicated with an end of metallic hose, and the other end of this metallic hose is connected with an end that leaks the material steel pipe.
Because titanium high-temperature electrolysis stove adopted totally-enclosed design, tail gas discharges from the air outlet, and this tail gas mainly comprises hydrogen fluoride gas and a small amount of solid Calcium Fluoride (Fluorspan) dust or the mixed dust of Calcium Fluoride (Fluorspan) and lithium fluoride.Hydrogen fluoride gas has injury to human body, and the Calcium Fluoride (Fluorspan) dust also pollutes the environment.The present invention also is included as the cover exhaust gas processing device 28 that titanium high-temperature electrolysis stove provides, and this absorption system is simple to operate, is beneficial to environmental protection, and the hydrogen fluoride in the tail gas is had good assimilation effect.
Electrolytic process
Titanium dioxide directly being carried out granulation with tablets press, make the particle that granularity is 2-8mm, is that the particle of 2-8mm makes the titanium dioxide pelletizing with granularity behind temperature 150-300 ℃ of lower drying treatment 20-30min.The present invention does not add water and binding agent when this step is carried out granulation, the size range of particle has also changed, and shorten time of drying, do not add like this water when granulation, reduced the dry time, reduced energy consumption.If when granulation, add binding agent, join when carrying out electrolysis in the electrolytic furnace at raw material, because temperature is high, binding agent can volatilize, and can destroy furnace atmosphere, increases the product foreign matter content.Use in addition binding agent also can increase cost.Therefore, the present invention does not add water and binding agent yet in this technological process, in addition, raw material granularity is controlled at 2-8mm, and this size range can make raw materials smooth.The drying treatment time shorten is 20-30min, and the water content that does not add entry so particle when mainly being granulation is low, so the also corresponding shortening of the time of drying treatment, has reduced energy consumption.The titanium dioxide pelletizing for preparing is joined in the molten bath 1, ionogen is added in the molten bath 1, described ionogen is the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, and the weight percent content of lithium fluoride is 5 ~ 20% in this fused salt mixt.The ionogen add-on is 2/3 of molten bath 1 capacity.Titanium high-temperature electrolysis stove evacuation degree to 1 * 10
-1~ 5 * 10
-3Pa is filled with argon gas in titanium high-temperature electrolysis stove, keeping electrolysis pressure is 10 ~ 100Pa, and the present invention is when electrolysis, and the positive pole of electrolysis power is connected with electrolytic cell anode, and the negative pole of electrolysis power links to each other with molten bath 1.Anode electrode adopts graphite material processing.At electric power outputting current 1 ~ 30kA, carry out electrolysis under 1800 ~ 1900 ℃ of conditions of electrolysis temperature, behind electrolysis 50 ~ 900min, begin to enter out material process.Electrolytic process of the present invention has compared with prior art omitted the process of tapping a blast furnace at the first electrolysis temperature, this is because the raw material that uses is titanium dioxide, the amount of the impurity iron that wherein contains seldom, therefore can omit, the impurity that contains in the product can utilize the design of two discharge holes to discharge, and avoids polluted product.
The heating thrust-augmenting nozzle makes the temperature in its exit reach 1800 ~ 1900 ℃ during discharging.Open pneumatics, union lever drives joint flange, graphite valve rod and ball valve and moves upward, make ball valve leave the graphite valve seat, at this moment, the liquid titanium flow into the reception crucible of cooling room from the opening part of graphite valve seat by thrust-augmenting nozzle, after going out material process and finishing, open pneumatics, union lever drives joint flange, graphite valve rod and ball valve and moves downward, and ball valve is pressed on the graphite valve seat, this moment, the liquid titanium stopped discharging, closed heating power supply.Product is after the cooling room cooling, and the door of opening cooling room takes out the titanium ingot.Be 99.9993% with its purity of titanium ingot sampling analysis measuring.
Claims (1)
1. a continuous fused salt electrolysis prepares the method for metal titanium, it is characterized in that:
The first step, titanium dioxide directly being carried out granulation with tablets press, make the particle that granularity is 2-8mm, is that the particle of 2-8mm makes the titanium dioxide pelletizing with granularity behind temperature 150-300 ℃ of lower drying treatment 20-30min;
Second step, the titanium dioxide pelletizing for preparing is joined in the molten bath, ionogen is added in the molten bath, described ionogen is the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, and the weight percent content of lithium fluoride is 5-20% in this fused salt mixt; The ionogen add-on is 2/3 of molten bath capacity, titanium high-temperature electrolysis stove evacuation degree to 1 * 10
-1-5 * 10
-3Pa is filled with argon gas in titanium high-temperature electrolysis stove, keeping electrolysis pressure is 10-100Pa;
When the 3rd step, electrolysis, the positive pole of electrolysis power is connected with electrolytic cell anode, and the negative pole of electrolysis power links to each other with the molten bath, and anode electrode adopts graphite material processing; At electric power outputting current 1-30kA, carry out electrolysis under the electrolysis temperature 1800-1900 ℃ condition, behind the electrolysis 50-900min, begin to enter out material process;
The heating thrust-augmenting nozzle makes the temperature in its exit reach 1800-1900 ℃ when the 4th step, discharging, opens ball valve, and titanium liquid is flow in the reception crucible of cooling room (19) by thrust-augmenting nozzle, after discharging is complete, closes ball valve; Product is after cooling room (19) cooling, and the door of opening cooling room (19) takes out the titanium ingot.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103484898A (en) * | 2013-10-10 | 2014-01-01 | 宝纳资源控股(集团)有限公司 | Vacuum high-temperature continuous electrolytic furnace system and electrolytic method |
CN103911631A (en) * | 2014-04-01 | 2014-07-09 | 攀钢集团攀枝花钢铁研究院有限公司 | Device for collecting products at cathode during molten salt electrolysis and molten salt electrolysis system |
CN105177635A (en) * | 2015-09-12 | 2015-12-23 | 北京工业大学 | System and method for continuously preparing tungsten powder |
CN108891063A (en) * | 2018-07-10 | 2018-11-27 | 凌鲲 | The manufacture craft of single line single-deck incense coil |
CN109023432A (en) * | 2018-10-09 | 2018-12-18 | 龙蟒佰利联集团股份有限公司 | A kind of electrolyzing fused titanium dioxide prepares the method and electrolysis unit of titanium-aluminium alloy |
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GB963743A (en) * | 1959-11-23 | 1964-07-15 | Shin Ichi Tokumoto | A method of electrodepositing metallic titanium or high titanium alloys |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103484898A (en) * | 2013-10-10 | 2014-01-01 | 宝纳资源控股(集团)有限公司 | Vacuum high-temperature continuous electrolytic furnace system and electrolytic method |
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CN108891063A (en) * | 2018-07-10 | 2018-11-27 | 凌鲲 | The manufacture craft of single line single-deck incense coil |
CN109023432A (en) * | 2018-10-09 | 2018-12-18 | 龙蟒佰利联集团股份有限公司 | A kind of electrolyzing fused titanium dioxide prepares the method and electrolysis unit of titanium-aluminium alloy |
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