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Process for preparing high pure rare earth metals by layered distillation method and device

A rare earth metal, high-purity technology, applied in the direction of improving process efficiency and energy efficiency, can solve the problems of low output of resistance furnace, low product purity, and non-reusable condenser

Inactive Publication Date: 2008-11-19
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a method for the preparation of high-purity rare earth metals samarium, europium, thulium, ytterbium, low yield of resistance furnaces, low product purity due to the simple structure of the condenser, and non-reusable condensers. Pure rare earth metal layer distillation process and device, using vacuum intermediate frequency induction furnace, design layer distillation device to realize multiple condensation and evaporation of metal vapor for purification, use heat-resistant metal material as reusable condensation receiver, device structure is compact, cooperate with corresponding The technological conditions make the output of the single furnace of the equipment large, the productivity is improved, the purity of the metal product is high, and it is suitable for the preparation of samarium, europium, thulium, and ytterbium

Method used

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  • Process for preparing high pure rare earth metals by layered distillation method and device
  • Process for preparing high pure rare earth metals by layered distillation method and device

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1 adopts 10kg purity to be 99% samarium oxide, 11Kg metal lanthanum as raw material, vacuumize to 10 -1 Below Pa, power on to raise the temperature, power 40kw, heating rate 5°C / min, keep warm at 1200°C for 6 hours, power off and fill with argon for protection, cool down for 3 hours and release from the furnace, the metal yield is 97%, and the metal purity is 99.996%.

[0025] Sm / TREM

Embodiment 2

[0026] Embodiment 2 adopts 10kg purity to be 99% europium oxide, 11Kg metal lanthanum as raw material, vacuumize to 10 -1 Below Pa, power on to raise the temperature, power 40kw, heating rate 10°C / min, keep warm at 1000°C for 6 hours, power off and fill with argon for protection, cool down for 3 hours and release from the furnace, the metal yield is 96%, and the metal purity is 99.998%.

[0027] Eu / TREM

Embodiment 3

[0028] Embodiment 3 adopts thulium oxide, 22Kg metal lanthanum as raw material that 20kg purity is 99%, vacuumizes to 10 -1 Below Pa, power on to raise the temperature, power 40kw, heating rate 11°C / min, keep warm at 1250°C for 6 hours, power off and fill with argon for protection, cool down for 3 hours and release from the furnace, the metal yield is 96%, and the metal purity is 99.99%.

[0029] Tm / TREM

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PUM

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Abstract

The invention relates to a process and a device for preparing high-purity rare earth metal by a layer distillation method. The process takes ordinary rare earth metal with a purity of 99 percent as raw material to directly perform distillation purification, or takes rare earth oxide as raw material and metal lanthanum as reducing agent to synchronously finish the reduction and the distillation purification in the same equipment, certain heating rate and vacuum degree are maintained during the reduction and distillation process, and the heat preservation is performed for certain time at a final reaction temperature. The distillation purification process is finished through a layer distillation device, the device comprises an insulating sleeve, a multi-layer baffle, a guide ring, a condensing cover plate, and a supporting ring, an insulating cylinder is arranged on a reduction reactor and is formed by a double-layer heat-resisting metal ring and heat insulating material, and the multi-layer baffle is arranged above the reactor and comprises the supporting ring, a partition and a connecting piece. The condensing cover plate and the supporting ring are arranged on the insulating cylinder and are used to condense and collect the metal. The process and the device are mainly suitable for preparing the purification of metal samarium, europium, thulium and ytterbium, the metal yield is more than 93 percent, and the purity is more than 99.99 percent.

Description

technical field [0001] The invention relates to the field of pyrometallurgy, in particular to a high-purity rare earth metal distillation purification process. Background technique [0002] At present, reduction distillation is commonly used in China to prepare metal samarium, europium, thulium, and ytterbium, and vacuum distillation is used for purification. However, the collection devices used by relevant domestic manufacturers are relatively simple, and there is no partition or partition between the heating element and the collector. A simple separator can easily condense the impurities entrained by the metal vapor, and at the same time evaporate and condense under the strong radiation of the heating element, causing ash to be entrained in the condensed metal. Therefore, the purity of the rare earth metal obtained is low. In addition, most of the existing technologies use resistance heating equipment such as carbon tube furnaces, which have slow heating and cooling speeds...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B5/16C22B9/02C22B59/00
CPCY02P10/20Y02P10/25
Inventor 李宗安颜世宏李振海李红卫赵斌杨启山王志强庞思明贺圣于敦波
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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