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Anhydrous samarium chloride and preparation method thereof

A technology of samarium chloride and ammonium chloride, which is applied in the preparation/treatment of rare earth metal compounds, rare earth metal chlorides, rare earth metal halides, etc., and can solve the problem of long production process, generation of by-product oxyhalides, and complicated production process and other problems, to achieve the effect of simple operation, avoiding pollution, and short process flow

Pending Publication Date: 2021-12-10
TIANJIN BAOGANG RES INST OF RARE EARTHS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process of the above method is complicated, the production process is long, and the by-product oxyhalide is produced during the preparation process, so it cannot be practically applied in industries such as high-purity rare earth metals, scintillation crystal materials, and organic synthesis catalysts.

Method used

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  • Anhydrous samarium chloride and preparation method thereof
  • Anhydrous samarium chloride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Take by weighing 500g of samarium oxide, and gradually add it in batches and completely dissolve it in a certain amount of commercially available concentrated hydrochloric acid (mass fraction is about 37%, the same below) (the mol ratio of samarium oxide to concentrated hydrochloric acid is approximately 1:3), adjust the pH of the solution to 5-7 (the solution is weakly acidic), heat to 140°C to concentrate the crystals, and centrifuge to obtain samarium chloride hydrate crystals.

[0041] (2) Mix the obtained samarium chloride hydrate crystals with ammonium chloride evenly (the stoichiometric ratio is 1:4), transfer to a vacuum rotary evaporator, vacuumize the system to below 0.01MPa, and start gradient temperature program dehydration, respectively Insulate at 120°C, 180°C and 240°C for 2 hours to obtain a mixture of anhydrous samarium chloride and ammonium chloride from which most of the crystal water has been removed.

[0042] (3) Anhydrous samarium chloride and ...

Embodiment 2

[0046] (1) Weigh 500g of samarium oxide, and gradually add it in batches and completely dissolve it in a certain amount of commercially available concentrated hydrochloric acid (the molar ratio of samarium oxide to concentrated hydrochloric acid is approximately 1:3), and adjust the pH of the solution to 5- 7 (the solution is weakly acidic), heated to 140°C to concentrate the crystals, and centrifuged to obtain samarium chloride hydrate crystals.

[0047] (2) Mix the obtained samarium chloride hydrate crystals with ammonium chloride evenly (the stoichiometric ratio is 1:3), transfer to a vacuum rotary evaporator, vacuumize the system to below 0.01MPa, and start gradient temperature-programmed dehydration, respectively Insulate at 140°C, 220°C and 260°C for 2 hours to obtain a mixture of anhydrous samarium chloride and ammonium chloride from which most of the crystal water has been removed.

[0048] (3) Place the mixture of anhydrous samarium chloride and ammonium chloride obta...

Embodiment 3

[0052] (1) Weigh 500g of samarium oxide, and gradually add it in batches and completely dissolve it in a certain amount of commercially available concentrated hydrochloric acid (the molar ratio of samarium oxide to concentrated hydrochloric acid is approximately 1:3), and adjust the pH of the solution to 5- 7 (the solution is weakly acidic), heated to 140°C to concentrate the crystals, and centrifuged to obtain samarium chloride hydrate crystals.

[0053] (2) Mix the obtained samarium chloride hydrate crystals with ammonium chloride evenly (the stoichiometric ratio is 1:2), transfer to a vacuum rotary evaporator, vacuumize the system to below 0.01MPa, and start gradient temperature-programmed dehydration, respectively Insulate at 120°C, 200°C and 260°C for 2 hours to obtain a mixture of anhydrous samarium chloride and ammonium chloride from which most of the crystal water has been removed.

[0054] (3) Place the mixture of anhydrous samarium chloride and ammonium chloride obta...

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Abstract

The invention provides anhydrous samarium chloride and a preparation method thereof. The preparation method comprises the steps: after samarium oxide reacts with hydrochloric acid, separating out crystals after evaporation, carrying out oncentration and cooling, and obtaining SmCl3.6H2O crystals are obtained after the crystals are filtered; uniformly mixing SmCl3.6H2O crystals with ammonium chloride, and carrying out gradient heating for pre-dehydration under a vacuum condition; carrying out gradient heating on a mixture of the pre-dehydrated SmCl3.6H2O crystal and ammonium chloride under the protection of inert gas to obtain dehydrated and ammonium-removed crude anhydrous SmCl3; heating the obtained crude anhydrous SmCl3 to 600-800 DEG C in a gradient manner under a vacuum condition, and respectively carrying out impurity removal and vacuum sublimation processes to obtain a high-purity anhydrous SmCl3 product. Compared with the conventional process, the preparation method disclosed by the invention has the advantages that different substances in the material can be separated through process control, the hydrolysis reaction of the raw material in the treatment process is avoided, and finally, the anhydrous samarium chloride with extremely high absolute purity is obtained through impurity removal and vacuum distillation processes.

Description

technical field [0001] The invention belongs to the field of preparation of rare earth materials, and in particular relates to anhydrous samarium chloride and a preparation method thereof. Background technique [0002] Rare earth elements are the general term for group IIIB yttrium and lanthanide elements in the periodic table. They are elements with a strategic position in the 21st century. They have unique physical and chemical properties such as light, electricity, and magnetism. They are widely used in various fields of national economy and national defense industry. Known as "industrial gold", it is called "treasure house of new materials in the 21st century". [0003] High-purity anhydrous rare-earth halides are important chemical raw materials and the core raw materials for the preparation of high-purity rare-earth metals and a new generation of high-performance rare-earth scintillation crystals, and have extremely broad application prospects. However, during the pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/271C01F17/10
CPCC01F17/271C01F17/10C01P2002/72C01P2006/80
Inventor 汪瑞高淞张瑞森张光睿李璐赵长玉彭维王安丽
Owner TIANJIN BAOGANG RES INST OF RARE EARTHS