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Preparation method for anhydrous rare earth chloride

The technology of rare earth chloride and lanthanum chloride is applied in the directions of rare earth metal chloride, rare earth metal compound, rare earth metal halide, etc., and achieves the effects of low preparation cost, simple operation and good dehydration effect.

Inactive Publication Date: 2018-03-23
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problems existing in the above-mentioned prior art, the present invention provides a preparation method of anhydrous rare earth chloride, the preparation method has the advantages of simple process, high dehydration efficiency, low preparation temperature, and alleviates the problem of equipment corrosion, while the environment Little pollution, and the prepared anhydrous rare earth chloride has high purity

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  • Preparation method for anhydrous rare earth chloride
  • Preparation method for anhydrous rare earth chloride

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preparation example Construction

[0026] The invention provides a preparation method of anhydrous rare earth chloride. The preparation method uses rare earth chloride heptahydrate as a raw material, and specifically performs segmental fluidized dehydration under a hydrogen chloride protective atmosphere to obtain high-purity, dehydrated Good effect anhydrous rare earth chloride.

[0027] It is worth noting that the preparation method of anhydrous rare earth chlorides according to the present invention is based on a fluidized dehydration device with three chambers.

[0028] It will be understood that, although the terms "first", "second", etc. may be used herein to describe various elements, these elements should not be limited by these terms. These terms are only used to distinguish one element from another.

[0029] Specific reference figure 1 , the fluidized dehydration device includes a first fluidized chamber 11, a second fluidized chamber 12 and a third fluidized chamber 13 which are connected in sequen...

Embodiment 1

[0060] In Example 1, the dehydration raw material is a mixture of lanthanum chloride heptahydrate and praseodymium chloride heptahydrate, and the feed rate is controlled to be 100kg / h, and the temperature of one-stage fluidized dehydration, two-stage fluidized dehydration and three-stage fluidized dehydration 60°C, 120°C, and 135°C, respectively, and at the same time, the time for the first-stage fluidized dehydration, the second-stage fluidized dehydration, and the third-stage fluidized dehydration were all 20 minutes, and finally obtained anhydrous lanthanum chloride and anhydrous praseodymium chloride Mixed products.

[0061] The anhydrous rare earth chloride product obtained in this embodiment was analyzed, wherein the water-insoluble content was 5.5% (wt%); the moisture content was 7.2% (wt%) detected by the Karl Fischer moisture analyzer; XRD analysis shows that the main components of the product are anhydrous lanthanum chloride and anhydrous praseodymium chloride.

Embodiment 2

[0063] In Example 2, the dehydration raw material is a mixture of lanthanum chloride heptahydrate and neodymium chloride hexahydrate, and the feed rate is controlled to be 100kg / h, and the temperature of one-stage fluidized dehydration, two-stage fluidized dehydration and three-stage fluidized dehydration 80°C, 130°C, and 140°C, respectively, and at the same time, the time for the first-stage fluidized dehydration, the second-stage fluidized dehydration, and the third-stage fluidized dehydration were all 20 minutes, and finally obtained anhydrous lanthanum chloride and anhydrous neodymium chloride Mixed products.

[0064] The anhydrous rare earth chloride product obtained in this embodiment was analyzed, wherein the water-insoluble content was 5.0% (wt%); the moisture content was 3.6% (wt%) detected by the Karl Fischer moisture analyzer; meanwhile, the XRD analysis shows that the main components of the product are anhydrous lanthanum chloride and anhydrous neodymium chloride. ...

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Abstract

The invention discloses a preparation method for an anhydrous rare earth chloride. The method comprises the following steps: step 1, performing first-stage fluidization dehydration on a rare earth chloride heptahydrate under the temperature of 60 DEG C-100 DEG C to obtain a crude product of a rare earth chloride trihydrate; step 2, performing second-stage fluidization dehydration on the crude product of the rare earth chloride trihydrate under the temperature of 120 DEG C-130 DEG C to obtain a crude product of a rare earth chloride monohydrate; and step 3, performing third-stage fluidization dehydration on the crude product of the rare earth chloride monohydrate under the temperature of 140 DEG C-160 DEG C to obtain the anhydrous rare earth chloride, wherein the third-stage fluidization dehydration is carried out in a hydrogen chloride gas atmosphere. According to the preparation method for the anhydrous rare earth chloride provided by the invention, the rare earth chloride heptahydrate is subjected to staged fluidization dehydration, and the hydrogen chloride protection gas atmosphere is provided, so that hydrolysis in the process of dehydration of the intermediate product rare earth chloride monohydrate to the anhydrous rare earth chloride is effectively inhibited, and the product purity is greatly improved; and the preparation method for the anhydrous rare earth chloride hasthe advantages of a low dehydration temperature, low preparation costs and good dehydration effects.

Description

technical field [0001] The invention belongs to the technical field of rare earth material preparation, and specifically relates to a method for preparing anhydrous rare earth chloride by using heptahydrate rare earth chloride as a raw material. Background technique [0002] Rare earth elements are elements with a strategic position in the 21st century. With their unique physical and chemical properties such as light, electricity, and magnetism, they are widely used in various fields of the national economy and defense industry. Therefore, rare earth elements are called "new materials of the 21st century". treasury". In recent years, rare earth elements have attracted more and more attention due to their important biological activities and pharmacological effects. [0003] The method for preparing anhydrous rare earth chloride has following 4 kinds at present: (1) tetrahydrofuran complex method, namely Deacon in 1979, the method for preparing anhydrous rare earth chloride b...

Claims

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Application Information

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IPC IPC(8): C01F17/00
CPCC01F17/271C01P2002/72C01P2006/82
Inventor 韩继龙都永生孙庆国韩凤清李斌凯
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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