CN103060850B - The method of metal titanium is prepared in a kind of continuous fused salt electrolysis - Google Patents
The method of metal titanium is prepared in a kind of continuous fused salt electrolysis Download PDFInfo
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- CN103060850B CN103060850B CN201310039416.XA CN201310039416A CN103060850B CN 103060850 B CN103060850 B CN 103060850B CN 201310039416 A CN201310039416 A CN 201310039416A CN 103060850 B CN103060850 B CN 103060850B
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Abstract
The invention provides a kind of method that metal titanium is prepared in continuous fused salt electrolysis, it is characterized in that: the first step, titanium dioxide is directly carried out granulation with tablets press, obtained titanium dioxide pelletizing; Second step, join in molten bath by the titanium dioxide pelletizing prepared, when the 3rd step, electrolysis, the positive pole of electrolysis power is connected with electrolytic cell anode, and the negative pole of electrolysis power is connected with molten bath, after electrolysis, starts to enter out material process; Heat thrust-augmenting nozzle when the 4th step, discharging, open ball valve, make titanium liquid flow in the reception crucible of cooling room by thrust-augmenting nozzle, after discharging, close ball valve; Product is after cooling room cooling, and the door opening cooling room takes out titanium ingot.By aforesaid method, titanium dioxide electrolysis can be made to realize serialization, therefore, it is possible to significantly reduce the production cost of titanium.
Description
Technical field
The present invention relates to a kind of method of continuous electrolysis titanium, particularly the method for metal titanium is prepared in a kind of continuous fused salt electrolysis.
Background technology
The premium properties such as titanium or titanium alloy has that light specific gravity, specific tenacity are high, creep-resistant property is good, corrosion-resistant under high temperature, extensively structured material is used as in aerospace, metallurgy, automobile and other industries, simultaneously can also as functional materials as hydrogen storage material, shape memory alloy material etc.The production technique of current titanium sponge is Kroll method, also referred to as magnesium reduction process, the method is first by the mineral producing titanium tetrachloride t 5 bx of titaniferous, use magnesium reduction titanium tetrachloride again thus obtained titanium sponge, eventually pass vacuum consumable electricity arc melting and make fine and close titanium ingot, then make the finished product through the mechanical means such as rolling, turning.Although existing magnesium reduction is the industrial process of comparative maturity, but due to production process have that technical process is long, operation is many, energy consumption is high, can not the problem such as continuous seepage, and metallic reducing agent magnesium used is also obtained by electrolysis, therefore production cost is high, environmental pollution is serious, limits 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 most is representational is that to propose a kind of be that the novel process of titanium sponge is produced in raw material negative electrode deoxidation in fused calcium chloride with titanium dioxide to Cambridge University professor Fray etc., 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 does negative electrode deoxidation again, it is slow that oxygen is diffused into anode speed from negative plate, and current efficiency is low.The application number of the present inventor is a kind of method that the earlier application of CN2008101186163 provides preparing metallic titanium with high temperature fused salt electrolysis of titanium dioxide, the method adds water and binding agent when granulation, there is the dry time longer, energy consumption is very high, and the use of binding agent makes to destroy furnace atmosphere when temperature height, increases the problems such as foreign matter content.
Summary of the invention
For the problems referred to above, applicant is on the basis furtherd investigate further it, propose a kind of method by high temperature fused salt electrolysis titanium dioxide continuous production metal titanium, the method can overcome the problems referred to above, thus solve in prior art that the technical process existed is long, operation is many, energy consumption is high, can not the series of problems such as continuous seepage, impurity is many.
Technical scheme of the present invention there is provided a kind of method that metal titanium is prepared in continuous fused salt electrolysis, and described method adopts following steps to implement:
The first step, titanium dioxide is directly carried out granulation with tablets press, obtained granularity is the particle of 2-8mm, is the particle of 2-8mm obtained titanium dioxide pelletizing after drying treatment 20-30min at temperature 150-300 DEG C by granularity;
Second step, join in molten bath by the titanium dioxide pelletizing prepared, added by ionogen in molten bath, described ionogen is the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, and in this fused salt mixt, the weight percent content of lithium fluoride is 5-20%; 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, and maintenance electrolytic 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 is connected with molten bath, and anode electrode adopts graphite material processing; At electric power outputting current 1-30kA, under electrolysis temperature 1800-1900 DEG C condition, carry out electrolysis, after electrolysis 50-900min, start to enter out material process;
Heat thrust-augmenting nozzle when the 4th step, discharging, make the temperature in its exit reach 1800-1900 DEG C, open ball valve, make titanium liquid flow in the reception crucible of cooling room by thrust-augmenting nozzle, after discharging, close ball valve; Product is after cooling room cooling, and the door opening cooling room takes out titanium ingot.
The invention has the beneficial effects as follows: the present invention is by being anode with Graphite Electrodes under high temperature, take titanium dioxide raw material as negative electrode, electrolysis is carried out in the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, titanium dioxide is liquid titanium by electrolytic reduction, due to the difference of density, titanium sinks to the lowest layer, after the titanium of accumulation reaches certain amount, from High Temperature Furnaces Heating Apparatus bottom discharge.Because under high temperature, oxygen anion velocity of diffusion is fast, thus accelerate deoxidation speed, thus the method current efficiency is high, power consumption is low, simultaneously because resultant metal titanium is liquid, titanium dioxide electrolysis can be made to realize serialization, therefore, it is possible to significantly reduce the production cost of titanium, compare with traditional technology and can save energy 50%, current efficiency brings up to more than 90%.
Accompanying drawing explanation
Below with reference to attached Fig. 1 and 2, titanium high-temperature electrolysis stove of the present invention is described in detail, wherein:
Fig. 1 is the schematic 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 schematic 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: 1-molten bath, 2-Heating element, 3-thermoscreen, 4-insulating cotton, 5-is with the furnace shell of water jacket, 6-is with the bell of water jacket, 7-refractory brick, 8-filling tube, 9-electrode, 10-thrust-augmenting nozzle, 11-heating unit, 12-drawing mechanism thermoscreen, 13-drawing mechanism refractory brick, 14-discharge chamber shell, 15-valve seat, 16-spheroid, 17-valve rod, 18-tapping crucible, 19-cooling room, 20-rectifier, 21-transformer, 22-feeder, 23-electrode dop, 24-electrode carrier arm, 25-tank room, 26-discharge chamber, 27-column guide rail, 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 the invention, tank room 25 mainly comprises molten bath 1, Heating element 2, thermoscreen 3, insulating cotton 4, the furnace shell 5 with water jacket and the bell 6 with water jacket, and wherein tank room 25 is rectangular parallelepiped, long 3m, wide 1.5m, high 2m.Refractory brick 7 is laid bottom tank room 25.Molten bath 1 is rectangle, is positioned at the center of tank room 25, is made up of graphite material, is used as the electrolyzer of high temperature fused salt electrolysis, the double negative electrode doing fused salt electrolysis in the process of electrolysis.Be provided with Heating element 2 in the surrounding of distance molten bath 1 outer side 5 ~ 10cm, Heating element 2 is parallel with the sidewall in molten bath 1, and Heating element 2 is made up of graphite material.For improving the homogeneity of temperature field in furnace, burner hearth is divided into four district's temperature controls, and every district forms closed loop loop, carries out temperature control.In order to reduce heat lost by radiation and the accumulation of heat loss of furnace wall further, improve the thermo-efficiency of stove, to be arranged in parallel graphite thermoscreen 3 in the surrounding of Heating element 2, thermoscreen 3 forms rectangle around heating unit 2, and its Main Function is heat insulation, insulation and reduces thermosteresis.Insulating cotton 4 is filled, to reduce the loss of heat between skin at thermoscreen 3 and the furnace shell with water jacket 5.Furnace shell 5 with water jacket is rectangle, is processed by the rolled sheet material with good welds performance, and in order to prevent, heating is uneven causes distortion and protection sealing-ring, is welded with water jacket in the surrounding of furnace shell.Pass through Flange joint with the bell 6 of water jacket and the furnace shell 5 with water jacket of tank room 25, there is high-temperature seal ring centre, can ensure the sealing of tank room 25.In order to prevent thermal radiation cause bell overheated and distortion, and 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 stove from bell over top, and during work, electrode can independently adjust.For ensureing furnace atmosphere and insulation, having between electrode 9 and the bell 6 with water jacket and sealing and seal.In order to ensure carrying out continuously of electrolysis, the bell 6 of tank room 25 with water jacket is uniformly distributed one or more filling tube 8, filling tube 8, with tightness system, has the function preventing heat radiation, prevent gas leakage.The bell 6 of tank room 25 with water jacket arranges liquid titanium drawing mechanism, is realized the opening and closing of liquid titanium drawing mechanism by pneumatics.
The below of tank room 25 is discharge chambers 26, liquid titanium is flow into cooling room 19 from the molten bath 1 of tank room 25 and cools.Discharge chamber 26 forms primarily 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 up of graphite material, is connected, is deep in cooling room 19 always with the valve seat 15 bottom molten bath 1.Solidify to prevent liquid titanium temperature in discharging process from reducing, ensure that the temperature of thrust-augmenting nozzle 10 is more than the fusing point of titanium, makes titanium discharging in a liquid state, is provided with heating unit 11 in the surrounding of thrust-augmenting nozzle 10, for heating thrust-augmenting nozzle 10, heating unit 11 is made up of graphite material.In order to reduce thermal radiation, arrange 3 ~ 5 layers of concentric round shape drawing mechanism thermoscreen 12 in heating unit 11 surrounding, drawing mechanism thermoscreen 12 is made up of graphite material.Drawing mechanism refractory brick 13 is set outside drawing mechanism thermoscreen 12.Be with stainless steel casing 14 outward.Tank room 25 is connected by flange with discharge chamber 26, and discharge chamber 26 is connected by flange with cooling room 19.
Cooling room 19 is positioned at the below of discharge chamber 26, and adopt plain carbon stool to manufacture and form, cooling room 19 Integral sealing, tapping crucible 18 is positioned at cooling room 19.
High Temperature Furnaces Heating Apparatus integral sealing, with the pre-picking device of vacuum pump, discharges furnace air before heating up, is then filled with argon gas, under argon atmosphere, carries out electrolysis.
Rectifier 20 is that rectifier 20 is that alternating-current is become direct current, and by transformation, output voltage is 0-10V, and outward current is 0-30kA for titanium dioxide electrolysis provides power supply needed for electrolysis.The positive pole of rectifier 20 is connected with electrode 9, and the negative pole of rectifier 20 is connected with the negative electrode of high-temperature electrolysis stove.
Transformer 21 is magnetic transformer, range of regulation is 10V-110V, its Main Function is to provide the power supply of high-temperature electrolysis stove heating, and the leading-out end of transformer 21 is connected with the water-cooled copper electrode of high-temperature electrolysis stove, by adjusting voltage thus the temperature of control high-temperature electrolysis stove.
The effect of conductive cross arm holds Graphite Electrodes, drives rise fall of electrodes.Conductive cross arm is primarily of electrode dop 23, electrode carrier arm 24, column guide rail 27, steel platform composition.Electrode carrier arm 24 is connected with electrode dop 23, electrode dop 23 is clamped with Graphite Electrodes 9, by dop, Graphite Electrodes is fixed, column is built with hoist cylinder, by the effect of hoist cylinder, control moving up and down of conductive cross arm, thus electrode can be regulated according to the Expenditure Levels of electrode.The motion of oil cylinder is controlled by Hydraulic Station.
Along with the carrying out of electrolysis, raw material is constantly consuming, and for ensureing carrying out continuously and the stability of electrolysis process of electrolysis, needs constantly to supplement raw material titanium dioxide in electrolytic process.Titanium dioxide is added 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, is fixedly communicated with the lower ending opening of casing by flanged plate, and the other end is circular open, this circular open is fixedly communicated with one end of metallic hose, with leakage, the other end of this metallic hose expects that one end of steel pipe is connected.
Because titanium high-temperature electrolysis stove have employed totally-enclosed design, tail gas discharges from air outlet, and this tail gas mainly comprises the mixed dust of hydrogen fluoride gas and a small amount of solid fluorinated calcium powder dirt or Calcium Fluoride (Fluorspan) and lithium fluoride.Hydrogen fluoride gas has injury to human body, and Calcium Fluoride (Fluorspan) dust also pollutes the environment.The present invention also comprises a set of exhaust gas processing device 28 for titanium high-temperature electrolysis stove provides, and this absorption system is simple to operate, is beneficial to environmental protection, has good assimilation effect to the hydrogen fluoride in tail gas.
Electrolytic process
Titanium dioxide is directly carried out granulation with tablets press, and obtained granularity is the particle of 2-8mm, is that the particle of 2-8mm obtains titanium dioxide pelletizing after drying treatment 20-30min at temperature 150-300 DEG C by granularity.The present invention does not add water and binding agent when this step carries out granulation, and the size range of particle have also been changed, and time of drying shortens, and does not add water like this when granulation, decreases the dry time, reduces energy consumption.If add binding agent when granulation, raw material join in electrolytic furnace carry out electrolysis time, because temperature is high, binding agent can volatilize, and can destroy furnace atmosphere, increases product foreign matter content.In addition binding agent is used also can to increase cost.Therefore, the present invention does not add water and binding agent in this technological process yet, in addition, is controlled by raw material granularity at 2-8mm, and this size range can make raw materials smooth.Drying treatment time shorten is 20-30min, and the water content mainly not adding water therefore particle during granulation is low, and therefore the also corresponding shortening of the time of drying treatment, reduces energy consumption.Join in molten bath 1 by the titanium dioxide pelletizing prepared, added by ionogen in molten bath 1, described ionogen is the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, and in this fused salt mixt, the weight percent content of lithium fluoride is 5 ~ 20%.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, and maintenance electrolytic 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 is connected with molten bath 1.Anode electrode adopts graphite material processing.At electric power outputting current 1 ~ 30kA, carry out electrolysis under electrolysis temperature 1800 ~ 1900 DEG C of conditions, after electrolysis 50 ~ 900min, start to enter out material process.Electrolytic process of the present invention compared with prior art eliminates the process of tapping a blast furnace at the first electrolysis temperature, this is because the raw material used is titanium dioxide, the amount of the impurity iron wherein contained is little, therefore can omit, the impurity contained in product can utilize the design of two discharge holes to discharge, and avoids polluted product.
Heat thrust-augmenting nozzle during discharging, make the temperature in its exit reach 1800 ~ 1900 DEG C.Open pneumatics, union lever drives joint flange, graphite valve rod and ball valve to move upward, make ball valve leave graphite valve seat, now, liquid titanium flow into the reception crucible of cooling room from the opening part of graphite valve seat by thrust-augmenting nozzle, go out after material process completes, open pneumatics, union lever drives joint flange, graphite valve rod and ball valve to move downward, and makes ball valve be pressed on graphite valve seat, now liquid titanium stops discharging, closes heating power supply.Product is after cooling room cooling, and the door opening cooling room takes out titanium ingot.Be 99.9993% by its purity of titanium ingot sampling analysis measuring.
Claims (1)
1. a method for metal titanium is prepared in continuous fused salt electrolysis, it is characterized in that:
The first step, titanium dioxide is directly carried out granulation with tablets press, obtained granularity is the particle of 2-8mm, is the particle of 2-8mm obtained titanium dioxide pelletizing after drying treatment 20-30min at temperature 150-300 DEG C by granularity;
Second step, join in molten bath by the titanium dioxide pelletizing prepared, added by ionogen in molten bath, described ionogen is the fused salt mixt of Calcium Fluoride (Fluorspan) or Calcium Fluoride (Fluorspan) and lithium fluoride, and in this fused salt mixt, the weight percent content of lithium fluoride is 5-20%; 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, and maintenance electrolytic 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 is connected with molten bath, and anode electrode adopts graphite material processing; At electric power outputting current 1-30kA, under electrolysis temperature 1800-1900 DEG C condition, carry out electrolysis, after electrolysis 50-900min, start to enter out material process;
Thrust-augmenting nozzle is heated when the 4th step, discharging, the temperature in its exit is made to reach 1800-1900 DEG C, open pneumatics, union lever drives joint flange, graphite valve rod and ball valve to move upward, make ball valve leave graphite valve seat, liquid titanium flow into the reception crucible of cooling room from the opening part of graphite valve seat by thrust-augmenting nozzle; After discharging, open pneumatics, union lever drives joint flange, graphite valve rod and ball valve to move downward, and makes ball valve be pressed on graphite valve seat, and now liquid titanium stops discharging, closes heating power supply; Product is after cooling room cooling, and the door opening cooling room takes out titanium ingot;
Described thrust-augmenting nozzle is made up of graphite material, is connected with the valve seat bottom molten bath, is deep in cooling room always; The surrounding of thrust-augmenting nozzle is provided with heating unit, and for heating thrust-augmenting nozzle, heating unit is made up of graphite material; Heating unit surrounding arranges 3 ~ 5 layers of concentric round shape drawing mechanism thermoscreen, and drawing mechanism thermoscreen is made up of graphite material; Drawing mechanism refractory brick is set outside drawing mechanism thermoscreen; Be with stainless steel casing outward.
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| CN103484898B (en) * | 2013-10-10 | 2016-04-27 | 宝纳资源控股(集团)有限公司 | A kind of vacuum high-temperature continuous electrolysis furnace system and electrolysis process |
| CN103911631B (en) * | 2014-04-01 | 2016-06-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Collect device and the fused salt electrolysis system of fused salt electrolysis cathode product |
| CN105177635B (en) * | 2015-09-12 | 2017-08-25 | 北京工业大学 | A kind of continuous system and method for 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 |
| CN101343756A (en) * | 2008-08-20 | 2009-01-14 | 北京宝泰丰金属研究所 | Method for preparing metallic titanium with high temperature fused salt electrolysis of titanium dioxide |
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2013
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB963743A (en) * | 1959-11-23 | 1964-07-15 | Shin Ichi Tokumoto | A method of electrodepositing metallic titanium or high titanium alloys |
| CN101343756A (en) * | 2008-08-20 | 2009-01-14 | 北京宝泰丰金属研究所 | Method for preparing metallic titanium with high temperature fused salt electrolysis of titanium dioxide |
| CN102220605A (en) * | 2011-06-29 | 2011-10-19 | 宝纳资源控股(集团)有限公司 | Titanium high-temperature feeding method for use in molten slat electrolysis |
| CN102719857A (en) * | 2012-07-03 | 2012-10-10 | 北京科技大学 | Method and electrolytic tank for producing metal titanium through directive electrolysis of titanium dioxide |
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