CN103436920A - High-temperature molten salt electrolysis rare earth metal bath discharge device and method - Google Patents

High-temperature molten salt electrolysis rare earth metal bath discharge device and method Download PDF

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Publication number
CN103436920A
CN103436920A CN201310352311XA CN201310352311A CN103436920A CN 103436920 A CN103436920 A CN 103436920A CN 201310352311X A CN201310352311X A CN 201310352311XA CN 201310352311 A CN201310352311 A CN 201310352311A CN 103436920 A CN103436920 A CN 103436920A
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rare earth
liquid storage
storage bag
earth metal
vacuum
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CN103436920B (en
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薛娟琴
刘志飞
唐长斌
毕强
赵四军
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Xian University of Architecture and Technology
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Xian University of Architecture and Technology
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Abstract

A high-temperature molten salt electrolysis rare earth metal bath discharge device comprises a vacuum liquid storage bag with a metal liquid outlet, wherein the vacuum liquid storage bag is tightly fixed on a turn type lifting platform car, one end of the vacuum liquid storage bag is communicated with a siphon inserted into a molten salt electrolysis bath, the other end of the vacuum liquid storage bag is communicated with a vacuum buffer tank through a metal corrugated pipe, the vacuum buffer tank is connected with a vacuum pump, the invention further provides a method using the high-temperature molten salt electrolysis rare earth metal bath discharge device, the siphon principle is used in the invention, the molten metal liquid is sucked into the vacuum liquid storage bag, then a plurality of moulds are cast, so that the bath discharge time is shortened, the loss of heat of a bath body is reduced, the fluctuation of the condition of the bath is avoided, the defects of high labor strength and poor operating environment and the like are overcome, the production cost is lowered, the product quality is improved, the stability is good, the metal liquid is guaranteed to go smoothly from the electrolysis bath to casting to moulding, and the problem of the hardly acceptable difficulties in taking out the rare earth metal and sealing a casting chamber after the casting on the site is also avoided.

Description

The high temperature fused salt electrolysis rare earth metal goes out slot device and method
Technical field
The invention belongs to the rare earth metal metallurgical technology field, particularly a kind of high temperature fused salt electrolysis rare earth metal goes out slot device and method, for the large-scale groove industrial production of fluoride smelt salt oxide compound Rare Earth Electrolysis.
Background technology
Because rare earth element has unique performance, China's rare earth is naturally abundant in addition, and China has developed into rare earth metal production, consumption and export State the biggest in the world.Fused salt electrolysis is the topmost commercial run of producing single light rare earth metal, norium and rare earth alloy.Along with development and the growth of China's rare earth metal industry, fluoride smelt salt oxide electrolysis technique (being called for short oxide electrolysis technique) has become the main flow production technique, and current electrolyzer specification mostly is 3000~8000A.But; with regard to its production capacity, scale, stability and long-range development prospect; large scale electrolytic cell demonstrates incomparable advantage than middle or small electrolyzer; and large scale electrolytic cell is convenient to realize that level of automation is higher; equip more perfect improvement upgrading, be suitable for intensively, large-scale production, this is to stably manufactured technique and quality product; reduce production costs, the important in inhibiting of enhancing productivity.Therefore, the grooved that scale is Wan An training some enterprises at home starts the operation of going into operation in succession.But going out groove automatically, liquid rare earth metal/alloy becomes the important key that restriction production is carried out smoothly.Because, still adopting and manually go out the end pot or scoop out and wait the mode of simply coming out of the stove, labour intensity will be very large, and high, the auxiliary material consumption of energy consumption is greatly, the groove condition more highlights by the drawback such as man's activity.
During domestic current electrolyzer industrialization is produced, the rare earth metal liquid of electrolysis in the groove mode of coming out of the stove mainly still adopts the titanium spoon manually scoop out or go out mode with the Stainless Steel Crucible clamp.The lifetime of manually coming out of the stove is long, the cell body calorific loss is more, the fluctuation of groove condition is large, the shortcomings such as labor strength is large, radiations heat energy is large, severe operational environment, causes that electrolysis is discontinuous, production cost is higher, the poor stability of quality product.For this reason, in the rare earth molten-salt electrolysis field, go out metal device and be widely studied and applied (as Chinese patent 01209185.5, the patent No. 200520127615.7 etc.).But the problem existed has: rare earth metal very easily occurs and is condensate in siphon pipe and advances the stove port and stop up in (1), extremely difficult cleaning, this and siphon-shaped, length and relevant without Insulation.(2) molten metal enters vacuum come out of the stove when bag and can't determine when that siphon is complete and stop the siphon operation.(3) in the whole process of coming out of the stove, the vacuum bag heat diffusion of coming out of the stove is fast, also needs repeatedly to open, seals and cause operational difficulty, labour intensity large.(4) after the pre-buried molybdenum fairlead electrically heated that the Shedd E S of the U.S. and Goldsmith J R propose, flow out and boron nitride siphon pipe siphon method; but need to be in sealing system while having out groove, under the argon shield state, be only applicable to the rare earth metal of low melting point and siphonal complex manufacturing technology, cost is higher; and metal blocking pipe or suction pipe suddenly cold and hot easily occur; therefore; these the two kinds modes of coming out of the stove also are difficult to be promoted and apply in actual production, more are not suitable for the actual production of maximization Rare Earth Electrolysis under the uncovered system of China.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of high temperature fused salt electrolysis rare earth metal to go out slot device and method, guaranteed that molten metal can be successfully from electrolyzer to being cast to mold, avoid the sealing difficulty of the rear rare earth metal taking-up of casting and casting chamber, be suitable for site work.
To achieve these goals, the technical solution used in the present invention is:
A kind of high temperature fused salt electrolysis rare earth metal goes out slot device, comprise the vacuum liquid storage bag 3 with molten metal outlet 31, vacuum liquid storage bag 3 is anchored on convertible lifting platform truck 2, one end of vacuum liquid storage bag 3 is communicated with the siphon pipe 1 in inserting fused-salt bath, the other end is communicated with vacuum buffer tank 5 by metallic bellows 4, and vacuum buffer tank 5 is connected to vacuum pump 7.
The hollow rectangular structure that described vacuum liquid storage bag 3 is the external belt thermal insulation layer, its inside is provided with gradient baffle plate 32, and the top of gradient baffle plate 32 is provided with the height baffle plate 33 of level.
Described siphon pipe 1 and metallic bellows 4 are connected with two relative horizontal ends on vacuum liquid storage bag 3 respectively, and described molten metal outlet 31 is arranged on the scarp of gradient baffle plate 32 on extension line, and blind nut is disposed in molten metal outlet 31.
Described height baffle plate 33 is for being arranged at the fluid limit position of vacuum liquid storage bag 3.
Described vacuum liquid storage bag 3 tops are provided with quartz glass window 34 with respect to height baffle plate 33.
The flip angle of described convertible lifting platform truck 2 is more than or equal to the angle of inclination of gradient baffle plate 32.
Described siphon pipe 1 is straight line fillet siphon pipe, by titanium base material, is made.
Described siphon pipe 1 pipeline is outside equipped with boosting or the attemperator that carries out temperature control.
Described convertible lifting platform truck 2 moves between fused-salt bath and casting die.
The present invention also provides and has utilized described high temperature fused salt electrolysis rare earth metal to go out the method for slot device, comprises the steps:
By convertible lifting platform truck 2, vacuum liquid storage bag 3 is moved near fused-salt bath, keep molten metal outlet 31 sealings;
Block the mouth of pipe of siphon pipe 1, open vacuum pump 7, vacuumized;
After treating fused salt electrolyzer Raw electrolysis fully, regulate the stroke of siphon pipe 1 to fused-salt bath bottom land top 10~20mm, and go deep into preheating 1min~2min in groove;
Open the valve of 3 of siphon pipe 1 and vacuum liquid storage bags, start to extract molten metal, cut off vacuum pump 7 after extraction, siphon pipe 1 is lifted from out to fused-salt bath;
Open molten metal on vacuum liquid storage bag 3 outlet 31, control convertible lifting platform truck 2 rollovers, make the steady outflow of molten metal each mould of casting one by one.
Compared with prior art, the present invention utilizes siphon principle, makes the molten metal of molten state suck vacuum liquid storage bag, a plurality of molds is cast thereupon.By this go out groove method operation can realize electrolysis continuously, reduced the time of coming out of the stove, cell body calorific loss, the fluctuation of groove condition, radiations heat energy etc., the shortcomings such as labor strength is large, severe operational environment have been overcome, reduce production cost, improved quality product, and good stability.And, guaranteed that molten metal is smoothly from electrolyzer to being cast to mold, avoided again the sealing difficulty of the rear rare earth metal taking-up of casting and casting chamber, be not easy to the problem of accepting for scene.
The accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is vacuum liquid storage bag schematic diagram of the present invention.
Embodiment
Describe embodiments of the present invention in detail below in conjunction with drawings and Examples.
As shown in Figure 1, a kind of high temperature fused salt electrolysis rare earth metal goes out slot device, comprise the vacuum liquid storage bag 3 with molten metal outlet 31, vacuum liquid storage bag 3 is anchored on convertible lifting platform truck 2, one end of vacuum liquid storage bag 3 is communicated with siphon pipe 1, the other end is communicated with vacuum buffer tank 5 by metallic bellows 4, and vacuum buffer tank 5 connects vacuum pump 7 by vacuum connection tube 6.Siphon pipe 1 is straight line fillet siphon pipe, and by high-temperature heat-resistance, anticorrosive, thermal conductivity is little, be easy to make, and the titanium base material that does not affect quality product makes, and the degree of depth that siphon pipe 1 inserts in the electrolyzer fused salt can freely be adjusted according to demand.Outside siphon pipe 1 pipeline, boosting or the lagging facility that need install certain-length additional carry out temperature control.Metallic bellows 4 for having than high mechanical property, good punching performance, high-temperature heat-resistance, anticorrosive, thermal conductivity is little, be easy to make, and the titanium or the titanium alloy material that do not affect quality product are made.
As shown in Figure 2, the hollow rectangular structure that vacuum liquid storage bag 3 is the external belt thermal insulation layer, its inside is provided with gradient baffle plate 32, and the top of gradient baffle plate 32 is provided with the height baffle plate 33 of level.Siphon pipe 1 and metallic bellows 4 are connected with two relative horizontal ends on vacuum liquid storage bag 3 respectively, and molten metal outlet 31 is arranged on the scarp of gradient baffle plate 32 on extension line, is positioned at the fluid limit position of vacuum liquid storage bag 3.Molten metal outlet 31 is disposed blind nut for by its sealing.Vacuum liquid storage bag 3 tops are provided with quartz glass window 34 with respect to height baffle plate 33, are convenient to observe control out liquid limit.Install boosting additional or lagging facility carries out temperature control in vacuum liquid storage bag external demand.
Convertible lifting platform truck 2 moves between fused-salt bath and casting die, realizes casting.Its flip angle is should be at least mutually concordant with the angle of gradient baffle plate 32 in vacuum liquid storage bag 3, and the angle of inclination of gradient baffle plate 32 is got 25 ° in the present embodiment.
After equipment connection is complete, determine that the supply lead connection is normal, can open vacuum pump 7 and vacuum buffer tank 5.Then block siphon pipe 1 mouth of pipe with ready stopper, and, with blind nut sealing metal liquid outlet 31, seal venting port simultaneously.Open vacuum buffer tank 5 and vacuum liquid storage bag 3 coupling cocks, check that interface, vacuum pump 7 and each mouth of pipe connecting portion of siphon pipe 1 guarantees without gas leak phenomenon.
Before formal siphon, can simulate examination takes out, regulate siphon pipe 1 stroke after the good electrolyzer height of Measurement accuracy to bottom land top 10~20mm, the whole process of simulated operation, determine without abnormal (after operation repeatedly, reach skill level, just can be without simulated operation), can start the beamhouse operation siphon and go out groove.
When the electrolytic process molten metal goes out groove, only stop normal feeding in raw material, can not stop electrolysis procedure.Before going out metal, at the bottom of agitator bath, judge the whether complete electrolysis of raw material (if electrolysis is fully treated carrying out relating operation after electrolysis fully).After determining electrolysis fully, convertible lifting platform truck 2 is opened to the trough rim appropriate location, opened convertible lifting gantry, adjusting siphon pipe 1 makes and enters in the cell body fused salt, highly be controlled at furnace bottom top 10~20mm, allow siphon pipe 1 go deep into preheating 1min~2min in groove.Then open siphon pipe 1 and 3 valves of vacuum liquid storage bag, start to extract molten metal.Should note observing the inflow situation of rare earth metal (alloy) and molten salt electrolyte in drawing liquid, when rising to height baffle plate 33 position, vacuum liquid storage bag 3 interior liquid (by quartz glass window 34, judge) that metal is taken out in expression complete, cut off immediately vacuum pump 7, disconnected power down source, then make siphon pipe 1 slowly lift from out electrolyzer.
Open subsequently molten metal and export 31 seal caps, then handle 2 rollovers of convertible lifting platform truck, by pouring gate, steadily flow out rare earth metal liquid each mould of casting one by one.
Close all switches after having cast, enter and go out the groove preparation next time.

Claims (10)

1. a high temperature fused salt electrolysis rare earth metal goes out slot device, the vacuum liquid storage bag (3) that comprises band molten metal outlet (31), it is characterized in that, vacuum liquid storage bag (3) is anchored on convertible lifting platform truck (2), one end of vacuum liquid storage bag (3) is communicated with the siphon pipe (1) in inserting fused-salt bath, the other end is communicated with vacuum buffer tank (5) by metallic bellows (4), and vacuum buffer tank (5) is connected to vacuum pump (7).
2. high temperature fused salt electrolysis rare earth metal according to claim 1 goes out slot device, it is characterized in that, the hollow rectangular structure that described vacuum liquid storage bag (3) is the external belt thermal insulation layer, its inside is provided with gradient baffle plate (32), and the top of gradient baffle plate (32) is provided with the height baffle plate (33) of level.
3. high temperature fused salt electrolysis rare earth metal according to claim 2 goes out slot device, it is characterized in that, described siphon pipe (1) and metallic bellows (4) are connected with upper two the relative horizontal ends of vacuum liquid storage bag (3) respectively, described molten metal outlet (31) is arranged on the scarp of gradient baffle plate (32) on extension line, and blind nut is disposed in molten metal outlet (31).
4. high temperature fused salt electrolysis rare earth metal according to claim 2 goes out slot device, it is characterized in that, described height baffle plate (33) is for being arranged at the fluid limit position of vacuum liquid storage bag (3).
5. high temperature fused salt electrolysis rare earth metal according to claim 2 goes out slot device, it is characterized in that, described vacuum liquid storage bag (3) top is provided with quartz glass window (34) with respect to height baffle plate (33).
6. high temperature fused salt electrolysis rare earth metal according to claim 2 goes out slot device, it is characterized in that, the flip angle of described convertible lifting platform truck (2) is more than or equal to the angle of inclination of gradient baffle plate (32).
7. high temperature fused salt electrolysis rare earth metal according to claim 1 goes out slot device, it is characterized in that, described siphon pipe (1) is straight line fillet siphon pipe, by titanium base material, is made.
8. go out slot device according to the described high temperature fused salt electrolysis rare earth metal of claim 1 or 7, it is characterized in that, described siphon pipe (1) pipeline is outside equipped with boosting or the attemperator that carries out temperature control.
9. high temperature fused salt electrolysis rare earth metal according to claim 1 goes out slot device, it is characterized in that, described convertible lifting platform truck (2) moves between fused-salt bath and casting die.
10. utilize the described high temperature fused salt electrolysis rare earth metal of claim 1 to go out the method for slot device, comprise the steps:
By convertible lifting platform truck (2), vacuum liquid storage bag (3) is moved near fused-salt bath, keep molten metal outlet (31) sealing;
Block the mouth of pipe of siphon pipe (1), the sealing venting port, open vacuum pump (7), vacuumized;
After treating fused salt electrolyzer Raw electrolysis fully, regulate the stroke of siphon pipe (1) to fused-salt bath bottom land top 10~20mm, and go deep into preheating 1min~2min in groove;
Open the valve between siphon pipe (1) and vacuum liquid storage bag (3), start to extract molten metal, cut off vacuum pump (7) after extraction, siphon pipe (1) is lifted from out to fused-salt bath;
Open molten metal on vacuum liquid storage bag (3) outlet (31), control convertible lifting platform truck (2) rollover, make the steady outflow of molten metal each mould of casting one by one.
CN201310352311.XA 2013-08-13 2013-08-13 High temperature fused salt electrolysis rare earth metal goes out slot device and method Expired - Fee Related CN103436920B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105369293A (en) * 2015-09-01 2016-03-02 包头市玺骏稀土有限责任公司 Rare earth electrolysis cell tapping device and method
CN105696027A (en) * 2014-11-27 2016-06-22 江苏永昌新能源科技有限公司 Lithium electrolytic tank lifting structure
CN107012486A (en) * 2017-03-27 2017-08-04 包头稀土研究院 Large-scale rare earth molten salt electrolytic goes out metal equipment
CN109680302A (en) * 2019-03-01 2019-04-26 赣州有色冶金研究所 A kind of lithium electrolysis vacuum pumping lithium system and method
CN110528030A (en) * 2019-09-17 2019-12-03 益阳鸿源稀土有限责任公司 A kind of Rare Earth Electrolysis device
CN111621815A (en) * 2020-05-27 2020-09-04 赣州市华新金属材料有限公司 Short-process method for preparing low-oxygen high-purity rare earth metal
CN111962102A (en) * 2020-08-21 2020-11-20 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院) Preparation method of low-oxygen high-purity rare earth alloy
CN112159995A (en) * 2020-09-28 2021-01-01 中铝郑州有色金属研究院有限公司 Siphon rare earth metal device and method for rare earth electrolytic tank
US11952674B2 (en) 2022-04-25 2024-04-09 Phoenix Tailings, Inc. Systems and methods for recovery of molten metal

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105696027A (en) * 2014-11-27 2016-06-22 江苏永昌新能源科技有限公司 Lithium electrolytic tank lifting structure
CN105369293A (en) * 2015-09-01 2016-03-02 包头市玺骏稀土有限责任公司 Rare earth electrolysis cell tapping device and method
CN105369293B (en) * 2015-09-01 2017-11-03 包头市玺骏稀土有限责任公司 The apparatus and method that a kind of rare earth electrolysis cell goes out metal
CN107012486A (en) * 2017-03-27 2017-08-04 包头稀土研究院 Large-scale rare earth molten salt electrolytic goes out metal equipment
CN109680302A (en) * 2019-03-01 2019-04-26 赣州有色冶金研究所 A kind of lithium electrolysis vacuum pumping lithium system and method
CN110528030A (en) * 2019-09-17 2019-12-03 益阳鸿源稀土有限责任公司 A kind of Rare Earth Electrolysis device
CN111621815A (en) * 2020-05-27 2020-09-04 赣州市华新金属材料有限公司 Short-process method for preparing low-oxygen high-purity rare earth metal
CN111621815B (en) * 2020-05-27 2022-05-13 赣州市华新金属材料有限公司 Short-process method for preparing low-oxygen high-purity rare earth metal
CN111962102A (en) * 2020-08-21 2020-11-20 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院) Preparation method of low-oxygen high-purity rare earth alloy
CN111962102B (en) * 2020-08-21 2021-06-25 江西省钨与稀土产品质量监督检验中心(江西省钨与稀土研究院) Preparation method of low-oxygen high-purity rare earth alloy
CN112159995A (en) * 2020-09-28 2021-01-01 中铝郑州有色金属研究院有限公司 Siphon rare earth metal device and method for rare earth electrolytic tank
US11952674B2 (en) 2022-04-25 2024-04-09 Phoenix Tailings, Inc. Systems and methods for recovery of molten metal
US11952673B2 (en) 2022-04-25 2024-04-09 Phoenix Tailings, Inc. Systems and methods for recovery of molten metal

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