High-purity calcium vacuum distillation purification device and method

A purification method and vacuum technology are applied in the field of high-purity calcium vacuum distillation and purification devices, which can solve the problems of unstable quality and low purity of batch products, and achieve the effects of stable batch product quality, stable distillation rate and good separation effect.

Inactive Publication Date: 2015-07-08
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Abstract
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Problems solved by technology

[0003] The present invention aims at the disadvantages of low purity of existing domestic high-purity calcium products and

Method used

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  • High-purity calcium vacuum distillation purification device and method
  • High-purity calcium vacuum distillation purification device and method
  • High-purity calcium vacuum distillation purification device and method

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Embodiment 1

[0045] Adopt high-purity calcium vacuum distillation purification device of the present invention, carry out high-purity calcium vacuum distillation purification, its steps are as follows:

[0046] 1) System pressure rise rate test: ensure that the system pressure rise rate is 0.6Pa / h. If the pressure rise rate of the system is high, the distillation unit needs to be checked for leaks.

[0047]2) Furnace installation: In a drying room environment with room temperature and humidity 99%, and the impurity content is shown in Table 1.

[0048] 3) Dehydration and degassing: Connect the vacuum system, turn on the rotary vane mechanical pump and the cooling water circulation system, when the vacuum degree of the system is -3 ~10 -2 Pa, close the vacuum butterfly valve, and energize the upper and lower resistance wires of the heating furnace at the same time. Control the current to raise the temperature of the reaction tank to 200°C within 1 hour, and keep it at 200°C for 0.5 hours ...

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Abstract

The invention discloses a high-purity calcium vacuum distillation purification device and a method. The high-purity calcium vacuum distillation purification device comprises a heating furnace; a distillation reaction pot arranged in the heating furnace; and a crucible and a crucible cover which are arranged on the bottom of the distillation reaction pot, wherein the crucible cover is provided with holes; coarse calcium is placed in the crucible; the upper end of the distillation reaction pot is provided with a vacuum pipeline and a reaction pot furnace cover, wherein the vacuum pipeline is used for connecting with a vacuum system, and the cross section of the reaction pot furnace cover shapes like T; the top of the reaction pot furnace cover is provided with a water cooled jacket; the lower T-shaped part of the reaction pot furnace cover is provided with a condensation plate; and the external edge of the condensation plate not covered by the lower end of the lower T-shaped part of the reaction pot furnace cover is provided with a plurality of small holes uniformly. A combination of a rotary vane mechanical pump with an oil diffusion pump is adopted by a vacuum system of the high-purity calcium vacuum distillation purification device; the high-purity calcium vacuum distillation purification device is simple in structure, and high in separation effect, and is convenient for maintenance; compared with the prior art, distillation rate is stable, product purity is high, batch quality is stable, and obtained calcium metal is high in activity.

Description

technical field [0001] The invention relates to a high-purity calcium vacuum distillation purification device and method, belonging to the technical field of metal vacuum distillation purification. Background technique [0002] In the preparation of many high-purity rare earth metals, high-purity calcium is an ideal reducing agent, and its purity directly affects the purity of the obtained product, and then affects its final use performance. Especially in the production and preparation of some nuclear materials, high-purity calcium has an indispensable position. At present, due to the unreasonable structure, material selection and process of the distillation equipment, the domestic high-purity calcium is often not high in purity, and the quality of batch products is unstable, so it has to rely on high-priced imports and is restricted. In view of this, a high-purity calcium vacuum distillation device and method are specially developed and disclosed. Contents of the inventi...

Claims

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Application Information

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IPC IPC(8): C22B9/02C22B26/20
CPCY02P10/20
Inventor 胡志方尹延西田丽森江洪林王力军罗远辉陈松
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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