Method for preparing high purity rare earth metal and its apparatus

A rare-earth metal, high-purity technology, applied in the direction of improving process efficiency, can solve the problems of small removal effect, low production efficiency, high content of metal gas impurities and non-rare earth metal impurities, so as to reduce the content of gas impurities and improve utilization The effect of improving the efficiency and improving the purity

Inactive Publication Date: 2012-05-23
GRIREM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this process are: 1) the removal effect of impurities other than carbon is very small, and the removal effect of carbon impurities itself is not ideal, and the purity of the metal is not high; 2) due to the use of neodymium oxide, Neodymium fluoride and calcium oxide, therefore, it is inevitable to introduce a large amount of oxygen, and because of the high melting point of neodymium oxide and calcium oxide, there will be a large amount of inclusions of neodymium oxide and calcium oxide in metal neodymium
The disadvantages of this process are: 1) rare earth metals with high purity cannot be obtained, especially the gas impurity content is high; 2) this process uses calcium chloride as an auxiliary salt bath, which will cause a large amount of chlorides to exist in the metal
The disadvantages of this process are: 1) the metal gas impurities and non-rare earth metal impurities obtained by this process have high content; 2) this process has high requirements for the purity of raw materials and related auxiliary materials, even reaching the fluorescence level
The disadvantages of this process are:

Method used

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  • Method for preparing high purity rare earth metal and its apparatus
  • Method for preparing high purity rare earth metal and its apparatus
  • Method for preparing high purity rare earth metal and its apparatus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Attached Figure 1 The equipment and device shown, add 500g of anhydrous lanthanum chloride with a purity of 99.9wt.% and 45g of lithium metal with a purity of 99.9wt.% to a titanium crucible made of titanium with a purity of 99.5wt.%, in a 99.999% argon atmosphere (>0.1MPa), raise the temperature to 950°C (the pressure of the reaction system is kept below 0.5MPa during the heating process), and keep it warm for 1 hour, then pump the system down to below 0.1Pa for distillation and removal of impurities, and keep it warm for 3 hours at 1100°C After finishing the distillation, refill with argon and cool to room temperature. Reduction obtained 263.4g of metal lanthanum, the yield was 93%, and the absolute purity of lanthanum was 99.957%. The analysis results are as follows:

[0032] Table 1 Metal Lanthanum Composition Analysis Unit: ppm (wt.)

[0033]

Embodiment 2

[0035] Attached Figure 1 For the equipment and device shown, add 500g of anhydrous lanthanum chloride with a purity of 99.9wt.% and 48g of lithium metal with a purity of 99.9wt.% to a tantalum crucible made of a tantalum material with a purity of 99.9wt.%, in a 99.999% argon atmosphere (>0.1MPa), raise the temperature to 950°C (the pressure of the reaction system is kept below 0.5MPa during the heating process), and keep it warm for 1 hour, then pump the system down to below 0.1Pa for distillation and removal of impurities, and keep it warm for 3 hours at 1100°C After finishing the distillation, refill with argon and cool to room temperature. The reduction obtained 265.1 g of metal lanthanum, the yield was 93.6%, and the absolute purity of lanthanum was 99.964%. The analysis results are as follows:

[0036] Table 2 Analysis of metal lanthanum components Unit: ppm (wt.)

[0037]

Embodiment 3

[0039] Attached Figure 1 The equipment and device shown, add 500g of anhydrous neodymium chloride with a purity of 99.9wt.% and 45g of lithium metal at 99.9wt.% to a titanium crucible made of titanium with a purity of 99.5wt.%, in a 99.999% argon atmosphere (>0.1MPa), raise the temperature to 1050°C (the pressure of the reaction system is kept below 0.5MPa during the heating process), and keep it warm for 1 hour, then pump the system down to below 0.1Pa for distillation and removal of impurities, and keep it warm for 3 hours at 1100°C After finishing the distillation, refill with argon and cool to room temperature. The reduction obtained 264.4g of neodymium metal, the yield was 92%, and the absolute purity of neodymium was 99.952%. The analysis results are as follows:

[0040] Table 3 Analysis of metal neodymium composition Unit: ppm (wt.)

[0041]

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Abstract

The invention relates to a method for preparing a high purity rare earth metal and its apparatus, which is characterized in that a lithium thermal reduction-vacuum distillation combined technology is used for preparing the high purity rare earth metal. The method comprises the following steps: taking rare earth chloride as a raw material and lithium metal as a reducing agent, placing in a reaction container, in a reaction system, carrying out a liquid-liquid displacement reaction of lithium metal and rare earth chloride under the inert gas protection (the pressure is 0.1-0.5 MPa) and the temperature of 850-1100 DEG C, then vacuum-pumping the reaction system to 10<-1>-10<-3> Pa, wherein the temperature is controlled at 900-1200 DEG C, evaporating lithium metal and lithium chloride, separating slag and metal to obtain the high purity rare earth metal. The reaction apparatus is composed of a furnace cover (1), a communicating pipe (2), a collector (3), a furnace body (4), a thermal baffle (5), a reactor (6), a heating device (7), an inflation system (8) and a vacuum system (9). The invention has the advantages of short process flow, high yield of rare earth metal and low production cost; the purity of the prepared rare earth metal is high. The used apparatus is simple and is easy to enlarge, and is suitable for large batch of industrial production.

Description

technical field [0001] The invention relates to a method and a device for preparing high-purity rare earth metals by a combination method of metallothermic reduction and vacuum distillation, belonging to the field of rare earth pyrometallurgy. Background technique [0002] Due to their irreplaceable excellent magnetic, optical and electrical properties, rare earths have become indispensable basic raw materials for high-tech functional materials such as magnetism, luminescence, laser, hydrogen storage, and superconductivity. They are widely used in computers, high-density information storage, and communications. , conversion, high-precision guidance, ray particle detection and recording, information highway and national security protection and other high-tech fields, such as Magneto NdFeB permanent magnets are widely used in VCM, motors, MRI and audio, etc., high specific energy Ni-MH battery materials Widely used in communications and electric vehicles, TbDyFe giant magnetos...

Claims

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Application Information

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IPC IPC(8): C22B59/00C22B5/04
CPCY02P10/20
Inventor 王志强李宗安颜世宏王祥生庞思明陈德宏周林徐立海陈博雨
Owner GRIREM ADVANCED MATERIALS CO LTD
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