Method for preparing light rare earth hydride by high-temperature direct method

A light rare earth and hydride technology, applied in the direction of transition element hydrides, etc., to achieve safe and stable storage, simple operation, and improved production level

Active Publication Date: 2015-01-21
BEIJING INSTITUTE OF TECHNOLOGYGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention is a high-purity light rare earth hydride preparation technology and related process method by high-temperature direct hydrogenation method. Compared with the existing lanthanum and cerium hydride preparation methods, it has essential differences and differences. Industria

Method used

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  • Method for preparing light rare earth hydride by high-temperature direct method

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Effect test

Embodiment 1

[0022] In a glove box filled with argon, 500 g of praseodymium with a purity of 99% was packed in a quartz glass test tube and sealed with a rubber stopper. The test tube is placed in a heating furnace cabin capable of evacuating, hydrogen and argon, and the cabin is set to an argon atmosphere in advance. Quickly pull out the rubber plug and close the furnace compartment. Keep the hydrogen and argon valves closed, open the exhaust valve, pump the furnace cabin pressure to a negative pressure of 0.026MPa; close the exhaust valve, open the argon valve to inflate the furnace cabin, close the argon valve, and open the exhaust valve Carry out vacuuming, repeat operation 2 times. Close all valves, quickly heat the furnace chamber to 360°C, open the hydrogen valve, input high-purity hydrogen into the reaction furnace, control the inflow of hydrogen at 770ml / min, and heat at a heating rate of 15°C / min for 20 minutes to 585°C Stop the temperature rise, keep the hydrogen flow rate con...

Embodiment 2

[0024] In a glove box filled with argon, 308 g of praseodymium with a purity of 99% was packed in a quartz glass test tube and sealed with a rubber stopper. The test tube is placed in a heating furnace cabin capable of evacuating, hydrogen and argon, and the cabin is set to an argon atmosphere in advance. Quickly pull out the rubber plug and close the furnace compartment. Keep the hydrogen and argon valves closed, open the exhaust valve, and pump the furnace cabin to a negative pressure of 0.030MPa; close the exhaust valve, open the argon valve to inflate the furnace cabin, close the argon valve, and open the exhaust valve Carry out vacuuming, repeat operation 2 times. Close all valves, quickly heat the furnace chamber to 375°C, open the hydrogen valve, input high-purity hydrogen into the reaction furnace, control the inflow of hydrogen at 580ml / min, and heat at a heating rate of 12°C / min for 18 minutes to 565°C Stop the temperature rise, keep the hydrogen flow rate constant...

Embodiment 3

[0026]In a glove box filled with argon, 1012 g of praseodymium with a purity of 99% was packed in a quartz glass test tube and sealed with a rubber stopper. The test tube is placed in a heating furnace cabin capable of evacuating, hydrogen and argon, and the cabin is set to an argon atmosphere in advance. Quickly pull out the rubber plug and close the furnace compartment. Keep the hydrogen and argon valves closed, open the exhaust valve, pump the furnace cabin pressure to a negative pressure of 0.019MPa; close the exhaust valve, open the argon valve to inflate the furnace cabin, close the argon valve, and open the exhaust valve Carry out vacuuming, repeat operation 3 times. Close all valves, quickly heat the temperature of the furnace chamber to 395°C, open the hydrogen valve, input high-purity hydrogen into the reaction furnace, control the inflow of hydrogen to 1318ml / min, and heat at a heating rate of 10°C / min for 25 minutes to 605°C Stop the temperature rise, keep the hy...

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Abstract

The invention belongs to the field of material science and technology and specifically relates to a method for preparing a light rare earth hydride by a high-temperature direct method. The method comprises the following main implementation steps: placing light rare earth with purity being greater than 99% and particle size being 2-15mm into a quartz glass test tube under the inert gas protection, removing air in a boiler room by the use of inert gas, closing an air evaporation valve, rapidly heating the boiler room at the heating rate of 2-20 DEG C/min until heating to 300-1000 DEG C, controlling inflow of hydrogen to 200-10,000 ml/min, and keeping the temperature and continuously reacting until a hydrogen pressure gauge and pressure in a heating reaction furnace are completely balanced, so as to obtain the required light rare earth hydride and corresponding light rare earth hydride powder. Purity of the light rare earth hydride prepared by the above method is 97-99.99%, and conversion rate of the light rare earth hydride powder is 97-99.99%. Thus, the hydride preparation purity problem in an industrial preparation technology is solved. The method is safe, reliable and is pollution-free, and is of great significance for industrialized and large-scale production of the light rare earth hydride.

Description

technical field [0001] The invention relates to a method for preparing light rare earth hydrides, in particular to a method for preparing light rare earth hydrides using a high-temperature direct method, and belongs to the field of hydrogen metal material preparation. Background technique [0002] Energy is one of the three pillars of the world's new technological revolution. With the development of human society and technological progress, human demand for energy is increasing. At the same time, due to non-renewable resources and serious environmental pollution, fossil fuels have huge limitations and have been difficult to adapt to the development needs of modern science and technology. Scientists have been committed to finding clean and efficient energy sources to replace fossil fuels, and clean energy sources such as solar energy, wind energy, hydrogen energy, and nuclear energy have emerged as the times require. Among these forms of energy acquisition, solar energy and ...

Claims

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Application Information

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IPC IPC(8): C01B6/02
CPCC01B6/02
Inventor 刘吉平于敦波汪玲李扩社亓云霞罗阳彭海军
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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