CN205653517U - Device of fused salt electrolysis method industrial production high purity titanium - Google Patents

Device of fused salt electrolysis method industrial production high purity titanium Download PDF

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Publication number
CN205653517U
CN205653517U CN201620137549.XU CN201620137549U CN205653517U CN 205653517 U CN205653517 U CN 205653517U CN 201620137549 U CN201620137549 U CN 201620137549U CN 205653517 U CN205653517 U CN 205653517U
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China
Prior art keywords
reactor
electrolysis
titanium
fused salt
temperature
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CN201620137549.XU
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焦树强
田栋华
王俊香
刘勇
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Ningxia Germany Run Run Titanium Co Ltd
University of Science and Technology Beijing USTB
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Ningxia Germany Run Run Titanium Co Ltd
University of Science and Technology Beijing USTB
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Abstract

The utility model provides a device of fused salt electrolysis method industrial production high purity titanium, the device is including vacuum system (a), fused salt electrolysis device (b) and direct current steady voltage electrolysis power (c), advantages such as the device has low cost, configuration operation is simple and convenient, industrial production is reliable and stable, plant use high efficiency. Adopt this set apparatus can produce the high purity titanium product more than the 4N.

Description

A kind of device of fused salt electrolysis process commercial production high purity titanium
Technical field
This utility model relates to the apparatus of a set of commercial production high purity titanium, and emphasis relates to a set of employing molten-salt electrolysis essence The apparatus of refining method commercial production high purity titanium.Use this equipment can serialization, low energy consumption, low-carbon environment-friendly produce.
Background technology
Titanium has biocompatibility, specific strength height, fusing point height, high temperature corrosion and avirulence because of it, and extensive It is applied to the fields such as Aero-Space.And high purity titanium is mainly used in the sputtering target material of Large Scale integrated circuit in the industry, The industries such as medical apparatus and instruments.At present, the main method producing high purity titanium has: Kroll, iodide process, electron-beam process and molten Salt electrolysis.This utility model content is to produce high purity titanium from the molten salt electrolyte that chloride is main body, but in existing life Production. art is primarily present device structure is complicated, technological operation is inconvenient, high equipment cost and can not serialization industry raw The shortcomings such as product.
Utility model content
This utility model is in order to overcome existing processing disadvantages, it is provided that a set of simple in construction, easy and simple to handle, commercial production is steady Fixed reliable, the equipment set industry of the high efficiency producing high purity titanium by fused salt electrolytic process of production and application and method, the technology used Scheme is as follows:
A kind of device of fused salt electrolysis process commercial production high purity titanium,
Described device includes vacuum system (a), fused salt electrolysis apparatus (b) and DC voltage-stabilizing electrolysis power (c);
Described vacuum system (a) uses oil seal type mechanical pump and Roots vaccum pump, is used for so that fused salt electrolysis apparatus (b) Reactor is in vacuum state;
Described fused salt electrolysis apparatus (b) includes reactor, electrolysis bath, thermocouple, bell, cathode and anode, inlet, outlet, very Do-nothing system connectivity port, temperature lowering water tape loop;Wherein,
Described electrolysis bath is placed in high-temperature reactor device interior low side, uses and separates dividing plate isolation inside reactor high/low temperature Interval, described reactor upper outside is provided with temperature lowering water tape loop, reduces reactor upper interval temperature, reactor low-temperature range If inert gas shielding inlet, outlet, vacuum system connectivity port, described electrolysis bath top is provided with elevated-temperature seal bell, described Having negative and positive electrolysis unit mouth and thermocouple temperature measurement mouth on bell, connecting portion and the reactor flange of cathode and anode are equipped with The O of different model, it is ensured that the sealing in reactor, the anode in described reactor uses different size geomery Useless titanium and titanium sponge compacting form, and its structural area of the anode in described reactor uses formula arrangement symmetrically;
Described DC voltage-stabilizing electrolysis power (c) output constant current electrolysis power, and its positive and negative electrode anode respectively, negative electrode is even Connect.
Described negative electrode, its depositing base is metallic nickel, molybdenum, rustless steel, zinc, titanium, aluminum, copper etc..
Described negative electrode, its depositing base has the shape such as tabular, spherical, pentagon, cylinder.
Described DC voltage-stabilizing electrolysis power (c) is 50A, 500A, 1000A, 3000A, 5000A, 10000A output constant current electricity Solve power supply.
Described reactor uses the materials such as high purity graphite, rustless steel, corundum to process.
The method producing high purity titanium according to the preparation of aforesaid device,
(1) selecting fused electrolyte to load in electrolysis bath, and cathode and anode loaded in electrolysis bath, O seals and is placed in instead Answer in the groove of device flange, cover reactor cap encapsulation process;
(2) open vacuum system, supplement high-purity argon gas when question response device is in vacuum state, rise to predetermined temperature;
(3) cathode and anode being transferred to fused electrolyte, energising certain time is electrolysed;
(4) after electrolysis, yin, yang electrode is carried to reactor low-temperature space, close resistance furnace after static 1-2h, in inertia When question response device low-temperature space temperature is down to less than 200 DEG C in the case of atmosphere, open reactor cap, take out the titanium of cathodic deposition;
(5) product titanium is carried out certain process, seal preservation by processing clean Titanium.
Further, after step (5) completes, reinstall negative electrode and depositing base thereof, then carry out new round electrolysis production The operation of high purity titanium.
The apparatus of a set of fused salt electrolysis process commercial production high purity titanium, applies this device can produce the higher height of purity Pure titanium, and whole production line can operate continuously, simple in construction, easy and simple to handle.Concrete operation is: by the useless titanium in industry or Person's titanium sponge is compressing as anode;Use the cathodic metal matrix of different-shape.Electrolyte be various fluoride (CaF, NaF, LiF) or chloride (CsCl, CaCl2、LiCl、KCl、MgCl2、AlCl3More than the one or two kinds of in) and TiCl3、TiCl2、K2TiF6、Na2TiF6In one or more salt-mixture as molten salt electrolyte.Utilize this complete equipment In vacuum equipment, the air in body of heater is evacuated to vacuum state, topping up argon in body of heater, treat the gas in body of heater During atmosphere balance, utilize resistance furnace to rise to predetermined temperature, and anode and cathode is placed in molten salt electrolyte, be passed through certain electric current (50 ~100000A), control anodic current density (0.001~6A/cm2), cathode-current density is (0.001~6A/cm2), energising Time is 0.5~700h, uses galvanostatic pulse method titanium deposition on cathode base.
When being electrolysed complete, anode and cathode being carried to body of heater low-temperature space, molten salt electrolyte is static in body of heater high-temperature region, treats low When the temperature of warm area is to less than 200 DEG C, opens bell and take out the product of cathodic deposition.Reinstall cathodic deposition matrix, evacuation, Mend argon, carry out new round electrolysis.
It is excellent that a set of equipment device provided by the utility model has good airproof performance, low energy consumption, easy and simple to handle, serialization etc. Point.
Accompanying drawing explanation
Fig. 1 is the apparatus structure chart of the application fused salt electrolysis process industrialized production high purity titanium;
Fig. 2 is fused salt electrolysis apparatus (b) enlargement decomposition;
Vacuum system (a), fused salt electrolysis apparatus (b) and DC voltage-stabilizing electrolysis power (c).
In figure 1 be thermocouple, 2 for reactor cap, 3 for vacuum port, 4 for crucible (electrolysis bath), 5 for reactor, 6 for sun Pole, 7 be negative electrode, 8 be cyclic water jacket, 9 be air inlet, 10 for gas outlet.
Detailed description of the invention
In order to make those skilled in the art be more fully understood that the application scheme, below in conjunction with in the embodiment of the present application Accompanying drawing, is clearly and completely described the technical scheme in the embodiment of the present application, it is clear that described embodiment is only The embodiment of the application part rather than whole embodiments.Based on the embodiment in the application, ordinary skill people The every other embodiment that member is obtained under not making creative work premise, all should belong to the model of the application protection Enclose.
It should be noted that term " first " in the description and claims of this application and above-mentioned accompanying drawing, " Two " it is etc. for distinguishing similar object, without being used for describing specific order or precedence.Should be appreciated that so use Data can exchange in the appropriate case, in order to embodiments herein described herein can with except here diagram or Order beyond those described is implemented.Additionally, term " includes " and " having " and their any deformation, it is intended that cover Cover non-exclusive comprising, such as, contain series of steps or the process of unit, method, system, product or equipment are not necessarily limited to Those steps clearly listed or unit, but can include the most clearly listing or for these processes, method, product Or intrinsic other step of equipment or unit.
Embodiment 1
Select KCl-KF-TiClxFor electrolyte, waste material titanium or titanium sponge are pressed into plate-like type, cathode and anode is loaded electricity In solution groove, O seals in the groove being placed in reactor flange, and covers reactor cap encapsulation process.Open industrial production line Vacuum system, supplements high-purity argon gas when being in vacuum state in question response device, rises to predetermined temperature.Cathode and anode is transferred to molten Melting in electrolyte, energising certain time is electrolysed.After electrolysis, yin, yang electrode is carried to reactor low-temperature space, static 1h Rear cut out resistance furnace, when question response device low-temperature space temperature is down to less than 200 DEG C in the case of inert atmosphere, opens reactor cap, Take out the titanium of cathodic deposition.Product titanium is carried out certain pretreatment, puts into and glove box seals preservation.
Embodiment 2
Select LiCl-KF-TiClxFor electrolyte, waste material titanium or titanium sponge are pressed into stripe shape, by stainless steel cathode, sun Pole loads in electrolysis bath, covers reactor cap and seals with O.Open the vacuum system in industrial production line, question response device In supplement high-purity argon gas when being in vacuum state, opening resistor stove heating schedule also rises to predetermined temperature.According to certain ratio Cathode and anode being transferred to fused electrolyte, energising certain time is electrolysed.After electrolysis, yin, yang electrode is carried to instead Device low-temperature space, static 1.5h is answered to make the electrolyte being mingled with close resistance furnace after flowing back to crucible.Question response in the case of inert atmosphere When device low-temperature space temperature is down to less than 200 DEG C, open reactor cap, take out the high purity titanium of cathodic deposition.Product titanium is carried out acid The pretreatment such as wash, put into vacuum drying oven seals preserve processing clean Titanium.
Embodiment 3
Select a certain proportion of LiCl-NaF-TiClxFor electrolyte, waste material titanium or titanium sponge are pressed into cylinder, will Ti cathode, anode load in electrolysis bath, cover reactor cap and seal with O.Open the vacuum system in industrial production line, Supplement high-purity argon gas when question response device is in vacuum state, open industrial resistance furnace heating schedule and rise to predetermined temperature.Press According to certain size, cathode and anode is transferred to fused electrolyte, be electrolysed.After electrolysis, yin, yang electrode is carried To reactor low-temperature space, static 2h makes the salt being mingled with stop resistance furnace after flowing back to crucible.Question response device in the case of inert atmosphere When low-temperature space temperature is down to less than 200 DEG C, open reactor cap, take out the high purity titanium of cathodic deposition.Product titanium is rinsed, It is dried and waits pretreatment, put into sealing preservation in glove box by processing clean Titanium.
Above-mentioned the embodiment of the present application sequence number, just to describing, does not represent the quality of embodiment, the portion related in embodiment Part title can also be arranged in scope known in the art flexibly.
In above-described embodiment of the application, the description to each embodiment all emphasizes particularly on different fields, and does not has in certain embodiment The part described in detail, may refer to the associated description of other embodiments.
In several embodiments provided herein, it should be understood that disclosed technology contents, can be passed through other Mode realizes.Wherein, device embodiment described above is only schematically, the division of the most described unit, Ke Yiwei A kind of logic function divides, and actual can have other dividing mode when realizing.
The above is only the preferred implementation of the application, it is noted that for the ordinary skill people of the art For Yuan, on the premise of without departing from the application principle, it is also possible to make some improvements and modifications, these improvements and modifications also should It is considered as the protection domain of the application.

Claims (5)

1. the device of a fused salt electrolysis process commercial production high purity titanium, it is characterised in that
Described device includes vacuum system (a), fused salt electrolysis apparatus (b) and DC voltage-stabilizing electrolysis power (c);
Described vacuum system (a) uses oil seal type mechanical pump and Roots vaccum pump, is used for the reaction so that fused salt electrolysis apparatus (b) Device is in vacuum state;
Described fused salt electrolysis apparatus (b) includes reactor, electrolysis bath, thermocouple, bell, cathode and anode, inlet, outlet, vacuum system System connectivity port, temperature lowering water tape loop;Wherein,
Described electrolysis bath is placed in high-temperature reactor device interior low side, uses and separates dividing plate isolation inside reactor height warm area Between, described reactor upper outside is provided with temperature lowering water tape loop, reduces reactor upper interval temperature, and reactor low-temperature range sets Inert gas shielding inlet, outlet, vacuum system connectivity port, described electrolysis bath top is provided with elevated-temperature seal bell, described stove Having covered negative and positive electrolysis unit mouth and thermocouple temperature measurement mouth, connecting portion and the reactor flange of cathode and anode are equipped with not The O of same model, it is ensured that the sealing in reactor, the anode in described reactor uses the useless of different size geomery Titanium and titanium sponge compacting form, and its structural area of the anode in described reactor uses formula arrangement symmetrically;
Described DC voltage-stabilizing electrolysis power (c) output constant current electrolysis power, and its positive and negative electrode anode respectively, negative electrode connects.
Device the most according to claim 1, it is characterised in that: described negative electrode, its depositing base is metallic nickel, molybdenum, stainless Steel, zinc, titanium, aluminum or copper.
Device the most according to claim 1, it is characterised in that: described negative electrode, its depositing base have tabular, spherical, five jiaos Shape or cylinder form.
Device the most according to claim 1, it is characterised in that: described DC voltage-stabilizing electrolysis power (c) is 50A, 500A, 1000A, 3000A, 5000A or 10000A output constant current electrolysis power.
Device the most according to claim 1, it is characterised in that: described reactor uses high purity graphite, rustless steel or corundum Material processes.
CN201620137549.XU 2016-02-24 2016-02-24 Device of fused salt electrolysis method industrial production high purity titanium Active CN205653517U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106868550A (en) * 2017-02-27 2017-06-20 北京科技大学 The method that useless titanium prepares high purity titanium is electrolysed in a kind of fuse salt

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106868550A (en) * 2017-02-27 2017-06-20 北京科技大学 The method that useless titanium prepares high purity titanium is electrolysed in a kind of fuse salt

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