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Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method

A temperature-programmed, praseodymium chloride technology, applied in inorganic chemistry, rare earth metal compounds, chemical instruments and methods, etc., can solve the problem of not containing water-insoluble substances

Active Publication Date: 2012-06-20
BAOTOU JINGRUI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods do not analyze the water content and water-insoluble matter in anhydrous praseodymium chloride or neodymium chloride products, while organic synthesis catalysts require high-purity anhydrous praseodymium chloride or neodymium chloride to be dissolved in water immediately, and the aqueous solution is clear and transparent after dissolution , can not contain water-insoluble matter, and the water content of high-purity anhydrous praseodymium chloride or neodymium chloride is required to be less than 0.1%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] 130kg PrCl 3 ·6H 2 O crystals and 65kg of ammonium chloride crystals are mixed evenly in a mixer, and the mixed materials are respectively put into porcelain bowls, and then the porcelain bowls containing materials are evenly placed in a programmed temperature-raising furnace, and vacuumed by a vacuum pump with water. , when the vacuum degree reaches 0.08Pa, set the heating program to start heating. The heating program is: room temperature ~ 150 ° C, the heating rate is 1.08 ° C / min, the heating time is 2 hours, and the holding time at 150 ° C is 2 hours; 150 ° C ~ 240 ℃, the heating rate is 0.75°C / min, the heating time is 2 hours, and the holding time is 4 hours at 240°C; 240°C~300°C, the heating rate is 0.5°C / min, the heating time is 2 hours, and the holding time is 2 hours at 300°C; 300℃~350℃, the heating rate is 0.42℃ / min, the heating time is 2 hours, and the holding time at 350℃ is 6.5 hours. When the temperature of the furnace body naturally drops to 50℃, the m...

Embodiment 2

[0009] 130kgNdCl 3 ·6H 2 O crystals and 65kg of ammonium chloride crystals are mixed evenly in a mixer, and the mixed materials are respectively put into porcelain bowls, and then the porcelain bowls containing materials are evenly placed in a programmed temperature-raising furnace, and vacuumed by a vacuum pump with water. , when the vacuum degree reaches 0.08Pa, set the heating program to start heating. The heating program is: room temperature ~ 150 ° C, the heating rate is 1.08 ° C / min, the heating time is 2 hours, and the holding time at 150 ° C is 2 hours; 150 ° C ~ 240 ℃, the heating rate is 0.75°C / min, the heating time is 2 hours, and the holding time is 4 hours at 240°C; 240°C~300°C, the heating rate is 0.5°C / min, the heating time is 2 hours, and the holding time is 2 hours at 300°C; 300℃~350℃, the heating rate is 0.42℃ / minute, the heating time is 2 hours, and the holding time at 350℃ is 6.6 hours. When the temperature of the furnace body naturally drops to 50℃, the...

Embodiment 3

[0011] 130kg NdCl 3 ·6H 2 O crystals and 65kg of ammonium chloride crystals are mixed evenly in a mixer, and the mixed materials are respectively put into porcelain bowls, and then the porcelain bowls containing materials are evenly placed in a programmed temperature-raising furnace, and vacuumed by a vacuum pump with water. , when the vacuum degree reaches 0.08Pa, set the heating program to start heating. The heating program is: room temperature ~ 150 ° C, the heating rate is 1.08 ° C / min, the heating time is 2 hours, and the holding time at 150 ° C is 2 hours; 150 ° C ~ 240 ℃, the heating rate is 0.75°C / min, the heating time is 2 hours, and the holding time is 4 hours at 240°C; 240°C~300°C, the heating rate is 0.5°C / min, the heating time is 2 hours, and the holding time is 2 hours at 300°C; 300℃~350℃, the heating rate is 0.42℃ / min, the heating time is 2 hours, and the holding time at 350℃ is 6.8 hours. When the temperature of the furnace body naturally drops to 50℃, the m...

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Abstract

The invention relates to preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by a programmed heating method, and belongs to the field of preparation of rare-earth materials. PrCl3.6H2O or NdCl3.6H2O and ammonium chloride are mixed in a weight ratio of 2:1, and vacuumizing is performed by using a water jet pump; when the vacuum degree reaches 0.08Pa, a heating program is set for heating at the temperature of between room temperature and 350 DEG C, and the sectional heating speed and the heat preservation time are controlled; by analysis and detection, the water content of the obtained anhydrous praseodymium chloride or neodymium chloride is less than 0.1 percent; and the anhydrous praseodymium chloride or neodymium chloride is immediately dissolved when added into water, the aqueous solution obtained after the anhydrous praseodymium chloride or neodymium chloride is dissolved is clear and transparent, and the purity of the product is over 99.9 percent. The method has already been applied to a production line capable of producing 90 kilograms of anhydrous praseodymium chloride or neodymium chloride in each batch in an industrial-scale programmed heating furnace.

Description

technical field [0001] The invention relates to a temperature-programmed method for preparing high-purity anhydrous praseodymium chloride or neodymium chloride, which belongs to the field of rare earth material preparation. Background technique [0002] Anhydrous praseodymium chloride and neodymium chloride can be respectively used in the application fields of organic synthesis catalyst, synthetic rubber catalyst, preparation of high-purity praseodymium or neodymium metal. The preparation methods of anhydrous praseodymium chloride or neodymium chloride include hydrated chloride dehydration method, oxide chlorination method and thionyl chloride dehydration method, etc. Literature "NdCl 3 -LiCl and NdCl 3 -Research on the phase diagram of LiCl-NaCl system", Acta Chemie Sinica, 1989, 47 (1): 14-18. Provides a kind of preparation method of anhydrous neodymium chloride, mixes NdCl 3 ·6H 2 O on P 2 o 5 Preliminary dehydration in the desiccator, then suction and decompression...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 郝先库张瑞祥马显东许宗泽胡珊珊刘海旺王士智
Owner BAOTOU JINGRUI NEW MATERIAL
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