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Device and method for purifying rare earth halide

A halide and rare earth technology, which is applied in the field of rare earth material preparation, can solve the problems of complex process, high oxygen content of rare earth halides, and long time consumption, and achieve simple purification process, which is conducive to energy saving and environmental protection and large-scale industrial production , The effect of short electrolysis time

Active Publication Date: 2013-11-27
GRIREM ADVANCED MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems that the existing process for purifying rare earth halides is complicated, takes a long time, and the prepared rare earth halides contain high oxygen content, the present invention provides a device and method for purifying rare earth halides

Method used

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  • Device and method for purifying rare earth halide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1000gLaF 3 Place in a molybdenum crucible, place the graphite anode and cathode tungsten rod coated with solid oxygen-permeable film in the molybdenum crucible, the lower edge of the anode and cathode is 4cm away from the inner plane of the bottom of the crucible, the distance between the cathode and the anode is 7cm, and the solid oxygen-permeable film The material is Y 2 o 3 Stable ZrO 2 ; Connect the entire ventilation pipeline system, and inject high-purity argon to test the airtightness of the pipeline; heat the LaF 3 to 1500°C, forming molten LaF 3 ; Adjust the electrolysis voltage to 2.5V, for molten LaF 3 Electrolysis 2h.

[0034] The purified LaF was measured by dynamic gas adsorption (IGA) 3 O content in medium. The measurement results showed that the purified LaF 3 The O content in the medium is 50ppm. This is because: during the electrolysis process, oxygen ions and graphite rods generate CO or CO 2 while being discharged, thereby achieving de-LaF ...

Embodiment 2

[0036] 1000g CeCl 4 Place in a molybdenum crucible, place the anode and cathode tungsten rods coated with solid oxygen-permeable film in the molybdenum crucible, the lower edge of the anode and cathode is 5cm away from the inner plane of the bottom of the crucible, the distance between the cathode and the anode is 7cm, the material of the solid oxygen-permeable film Use Y 2 o 3 Stable ZrO 2 , the anode is a Li-doped graphite rod; connect the entire ventilation pipeline system, and feed high-purity argon to detect the airtightness of the pipeline; heat CeCl 4 to 590°C, forming molten CeCl 4 ; Adjust the electrolysis voltage to 2.3V, for molten CeCl 4 Electrolysis 4h.

[0037] The purified CeCl was measured by dynamic gas adsorption (IGA) 4 O content in medium. The measurement results show that the CeCl obtained after purification 4 The O content is 40ppm. This is because: during the electrolysis process, some oxygen ions react with active Li to form Li 2 O, some oxyge...

Embodiment 3

[0039] Put 1000g of PrBr in the molybdenum crucible, place the anode and cathode tungsten rod coated with solid oxygen permeable film in the molybdenum crucible, the lower edge of the anode and cathode is 4.5cm away from the inner plane of the bottom of the crucible, the distance between the cathode and the anode is 7cm, solid Oxygen permeable membrane material adopts Y 2 o 3 Stable ZrO 2 , the anode is a graphite rod doped with Na; connect the entire ventilation pipeline system, and feed high-purity argon to detect the airtightness of the pipeline; heat the PrBr 3 to 700°C, forming molten PrBr 3 ; Adjust the electrolysis voltage to 2.8V, for melting PrBr 3 Electrolysis 1.5h.

[0040] Determination of purified PrBr by dynamic gas adsorption (IGA) 3 O content in medium. The measurement results show that the PrBr obtained after purification 3 The O content is 40ppm. This is because: during the electrolysis process, some oxygen ions react with active Na to form Na 2 O, s...

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Abstract

The invention discloses a device and a method for purifying rare earth halide. The device comprises a crucible used for electrolytic purification, a positive pole, a negative pole and a ventilation pipeline system used for supplying shielded gas into an electrolytic system, wherein the positive pole and the negative pole are arranged in the crucible; a solid oxygen permeation membrane is arranged on the surface of the positive pole; the melting point of the solid oxygen permeation membrane is larger than that of to-be-purified rare earth halide. The method comprises the step of electrolytically purifying rare earth halide by adopting the device provided by the application. The electrolytic device is simple, purification technology is simple, the stability is high, the electrolysis voltage is low, the electrolysis time is short, and energy conservation, environmental protection and large scale industrial production are facilitated. Rare earth halide obtained by using the device and the purifying method provided by the invention is high in purity, and the oxygen content is less than 50 ppm.

Description

technical field [0001] The invention relates to the technical field of rare earth material preparation, in particular to a device and method for purifying rare earth halides. Background technique [0002] High-purity rare-earth halides are very important chemical reagents, which are used to prepare high-purity rare-earth metals and a new generation of high-performance rare-earth scintillation crystal LnX 3 : The core raw material of Ce has very broad application prospects. Rare earth halides are prone to hydrolysis and oxygen absorption during the preparation process, which has a great impact on the performance of rare earth materials prepared by using rare earth halides. For example, when the oxygen content in the giant magnetostrictive material prepared by using high-purity rare earth halide exceeds 1000 ppm, its magnetostrictive property almost completely disappears. The absolute purity of rare earth halide raw materials in scintillation crystals cannot be lower than 99...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/24C25B11/02
CPCY02P20/10
Inventor 朱琼陈德宏王志强李宗安颜世宏苗睿瑛张小伟张志琦周林庞思明徐立海王祥生
Owner GRIREM ADVANCED MATERIALS CO LTD
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