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Preparation method of high-purity anhydrous rare earth chloride

A technology of water chlorination and rare earth oxide, applied in the preparation/processing of rare earth metal compounds, rare earth metal halides, rare earth metal chlorides, etc., can solve the problems of impure products, poor dehydration effect, and undisclosed yields. , to avoid rare earth oxychloride, facilitate long-term storage, and reduce the generation of impurities

Active Publication Date: 2020-12-01
内蒙古中科蒙稀新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (2) Ammonium chloride sublimation method: In the presence of ammonium chloride, rare earth oxides are transformed into anhydrous rare earth chlorides at high temperatures. pure
[0008] (4) Chinese patent application CN108455650A discloses a preparation method of anhydrous samarium chloride, using samarium oxide as raw material, reacting with ammonium chloride solid, then feeding dry hydrogen chloride gas, heating until the reaction is complete, and drying the product , to obtain anhydrous chloride thorium, inert gas needs to be introduced in the preparation process, which increases the cost, and this method also needs hydrogen chloride gas to protect
The dehydration effect of crystallization water and rare earth chloride dehydration method is not good, and the product purity is not high
[0011] At present, none of the prior art discloses a high-purity anhydrous rare earth chloride preparation method with high yield, high purity and low water content.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A preparation method of high-purity anhydrous cerium chloride, comprising the steps of:

[0049](1) Mix cerium oxide and ammonium chloride at a molar ratio of 1:20, and heat the reaction. The heating method is as follows: from 100°C to 300°C at a heating rate of 15°C / min, and then from 300°C to 5°C / min heating rate to 500°C to obtain mixture A.

[0050] (2) The mixture A was mixed with 18% hydrochloric acid for 0.5 h, and the amount of hydrochloric acid added was 1:3 g / mL according to the mass volume ratio of cerium oxide and hydrochloric acid to obtain solution B.

[0051] (3) Concentrate and dry solution B to obtain solid C.

[0052] (4) Program the temperature of solid C at -0.05MPa, room temperature -100°C, the heating rate is 10°C / min, keep it at 100°C for 1h; 100-260°C, the heating rate is 1°C / min, keep it at 260°C 2h; 260-320°C, the heating rate is 0.5°C / min, keep at 320°C for 0.5h; 320-400°C, the heating rate is 5°C / min, keep at 400°C for 2h, that is.

Embodiment 2

[0054] A preparation method of high-purity anhydrous neodymium chloride, comprising the steps of:

[0055] (1) Mix neodymium oxide and ammonium chloride at a molar ratio of 1:35, and heat the reaction. The heating method is as follows: heating from 100°C to 300°C at a heating rate of 20°C / min, and then heating from 300°C to 10°C / min heating rate to 500°C to obtain mixture A.

[0056] (2) Mix the mixture A with 22% hydrochloric acid for 1 h, and add the hydrochloric acid according to the mass volume ratio of neodymium oxide and hydrochloric acid at 1:4 g / mL to obtain solution B.

[0057] (3) Concentrate and dry solution B to obtain solid C.

[0058] (4) Program the temperature of solid C at -0.08MPa, room temperature -100°C, heating rate is 15°C / min, keep at 100°C for 2h; 100-260°C, heating rate is 5°C / min, keep at 260°C 4h; 260-320°C, the heating rate is 1.5°C / min, keep at 320°C for 1h; 320-400°C, the heating rate is 10°C / min, keep at 400°C for 4h.

Embodiment 3

[0060] A kind of preparation method of high-purity anhydrous lanthanum chloride comprises the steps:

[0061] (1) Mix lanthanum oxide and ammonium chloride at a molar ratio of 1:30, and heat the reaction. The heating method is as follows: heating from 100°C to 300°C at a heating rate of 17°C / min, and then heating from 300°C to 8°C / min heating rate to 500°C to obtain mixture A.

[0062] (2) The mixture A was mixed with 20% hydrochloric acid for 0.75h, and the amount of hydrochloric acid was added according to the mass volume ratio of lanthanum oxide and hydrochloric acid being 1:3.5g / mL to obtain solution B.

[0063] (3) Concentrate and dry solution B to obtain solid C.

[0064] (4) Program the temperature of solid C at -0.06MPa, room temperature -100°C, the heating rate is 12°C / min, keep it at 100°C for 1.5h; 100-260°C, the heating rate is 3°C / min, at 260°C Heat preservation for 3 hours; 260-320°C, heating rate is 1°C / min, heat preservation at 320°C for 0.75h; 320-400°C, he...

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Abstract

The invention relates to the technical field of preparation of rare earth materials, in particular to a preparation method of high-purity anhydrous rare earth chloride. The preparation method comprises the following steps: (1) mixing rare earth oxide and ammonium chloride, and carrying out heating for a reaction to obtain a mixture A; (2) mixing the mixture A with hydrochloric acid to obtain a solution B; (3) concentrating and drying the solution B to obtain a solid C; and (4) carrying out programmed heating on the solid C to obtain the product. The method has the advantages of high yield, high purity and low water content.

Description

technical field [0001] The invention relates to the technical field of rare earth material preparation, in particular to a preparation method of high-purity anhydrous rare earth chloride. Background technique [0002] Rare earth elements account for about one-seventh of the elements in the periodic table, including scandium, yttrium and 15 lanthanides. In-depth research on rare earth elements will not only help to discover new properties and explore new materials, but also promote the development of inorganic chemistry. Rare earth elements are known as a treasure house of new materials due to their excellent optical, electrical, and magnetic properties, and have become important strategic elements. [0003] Rare earth chloride is mainly used as a raw material for electrolysis of mixed rare earth metals, rare earth alloys and extraction of a single rare earth element, and can also be used as a petrochemical catalyst, co-catalyst and raw material for rare earth polishing powd...

Claims

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Application Information

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IPC IPC(8): C01F17/271C01F17/10
CPCC01P2006/80C01P2006/82C01F17/10C01F17/271
Inventor 不公告发明人
Owner 内蒙古中科蒙稀新材料有限责任公司
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