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A kind of method for preparing neodymium chloride monohydrate by temperature-programmed method

A neodymium chloride monohydrate, temperature-programmed technology, applied in chemical instruments and methods, rare earth metal chlorides, inorganic chemistry, etc., can solve the problems of high energy consumption and cannot contain water-insoluble substances, and achieve low energy consumption and reduced energy consumption. The cost of dehydration and the effect of pollutant discharge

Active Publication Date: 2019-04-09
PETROCHINA CO LTD +1
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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%.
[0006] CN201110346246 discloses a temperature-programmed method for preparing high-purity anhydrous praseodymium chloride or neodymium chloride, but the preparation method needs to be heated to 350°C, and the energy consumption is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 200kg of NdC1 3 ·6H 2 Put O into the dehydration reactor, start stirring the dehydration kettle, pass in nitrogen preheated by low-pressure steam, start the vacuum pump to vacuum, when the vacuum reaches 50kpa, set the heating program to start heating, the heating program is: room temperature ~ 100 ℃, the heating rate is 0.625°C / min, the heating time is 2 hours, and the holding time at 100°C is 3 hours; 100°C~120°C, the heating rate is 0.167°C / min, the heating time is 2 hours, and the holding time at 120°C is 6 hours; 120℃~140℃, heating rate 0.167℃ / min, heating time 2 hours, holding time at 140℃ 4 hours; 140℃~158℃, heating speed 0.15℃ / min, heating time 2 hours, holding at 158℃ After 10 hours, when the temperature of the kettle body naturally dropped to 50°C, 155 kg of neodymium chloride monohydrate obtained was analyzed and the water content was 6.8%.

[0016] Since this embodiment is implemented on an industrial device, a deviation of ±1°C is allowed during temperatur...

Embodiment 2

[0018] Put 200kg of NdC1 3 ·6H 2 O is put into the dehydration reaction kettle, the dehydration kettle is started to stir, the nitrogen gas preheated by low pressure steam is introduced, and the vacuum pump is started to vacuum. When the vacuum degree reaches 50kpa, the heating program is set to start heating. The heating program is: room temperature~100℃, heating speed 0.625℃ / min, heating time 2 hours, holding time at 100℃ 3 hours; 100℃~120℃, heating speed 0.167℃ / min, heating time 2 hours, 120℃ holding time 6 hours; 120℃~140℃, heating speed 0.167℃ / min, heating time 2 hours, heating time 4 hours at 140℃; 140℃~158℃, heating speed 0.15℃ / min, heating time 2 hours, 10 hours of holding time at 158°C, when the temperature of the kettle body naturally drops to 50°C, 151 kg of neodymium chloride monohydrate obtained is analyzed and the water content is 7.6%.

[0019] Since this embodiment is implemented on an industrial device, a deviation of ±1°C is allowed during temperature control.

Embodiment 3

[0021] Put 200kg of NdC1 3 ·6H 2 O is put into the dehydration reaction kettle, the dehydration kettle is started to stir, the nitrogen gas preheated by low pressure steam is introduced, and the vacuum pump is started to vacuum. When the vacuum degree reaches 50kpa, the heating program is set to start heating. The heating program is: room temperature~100℃, heating speed 0.625℃ / min, heating time 2 hours, holding time at 100℃ 3 hours; 100℃~120℃, heating speed 0.167℃ / min, heating time 2 hours, 120℃ holding time 6 hours, 120℃~140℃, heating speed 0.167℃ / min, heating time 2 hours, heating time 4 hours at 140℃; 140℃~158℃, heating speed 0.15℃ / min, heating time 2 hours, 10 hours of holding time at 158°C, when the temperature of the kettle body naturally drops to 50°C, 155 kg of neodymium chloride monohydrate obtained is analyzed and the water content is 6.6%.

[0022] Since this embodiment is implemented on an industrial device, a deviation of ±1°C is allowed during temperature control.

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Abstract

The invention relates to a method for preparing a neodymium chloride hydrate through a programmed temperature increasing method. The method comprises: loading a granular crystal NdC13.6H2O into a dehydration reaction kettle, starting the dehydration reaction kettle to stir, introducing nitrogen being subjected to low temperature steam preheating, starting a vacuum pump, vacuumizing, setting a temperature increasing program to start heating when the vacuum degree achieves 50 kpa, and naturally cooling the kettle temperature to 50 DEG C to obtain the neodymium chloride hydrate product, wherein the temperature increasing program comprises that the heating is performed for 2 h at the heating rate of 0.625 DEG C / min within the temperature range from room temperature to 100 DEG C and the thermal insulation time is 3 h at a temperature of 100 DEG C, the heating is performed for 2 h at the heating rate of 0.167 DEG C / min within the temperature range of 100-120 DEG C and the thermal insulation time is 6 h at a temperature of 120 DEG C, the heating is performed for 2 h at the heating rate of 0.167 DEG C / min within the temperature range of 120-140 DEG C and the thermal insulation time is 4 h at a temperature of 140 DEG C, and the heating is performed for 2 h at the heating rate of 0.15 DEG C / min within the temperature range of 140-158 DEG C and the thermal insulation time is 10 h at a temperature of 158 DEG C.

Description

Technical field [0001] The invention belongs to the field of rare earth material preparation, and relates to a method for preparing neodymium chloride monohydrate by a temperature programmed method. Background technique [0002] Neodymium chloride monohydrate can be used in application fields such as the preparation of organic synthesis catalysts and synthetic rubber catalysts. However, most of the current literature is the preparation method of anhydrous neodymium chloride, and the preparation methods of anhydrous neodymium chloride include dehydration method, oxide chlorination method and thionyl chloride dehydration method. [0003] Zhang Xufeng published "NdCl 3 -LiCl and NdCl 3 -LiCl-NaCl system phase diagram", Acta Chimica Sinica, 1989, 47(1): 14-18. A method for preparing anhydrous neodymium chloride is provided, and NdCl 3 ·6H 2 O is placed in P 2 O 5 Preliminary dehydration in a desiccator, and then in an HCl atmosphere while heating and suction decompression, dehydration ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
CPCC01F17/271C01P2006/80C01P2006/82
Inventor 孙福权周爱文韩明哲孙伟赵宇徐刚杨欢陈加平宋玉萍贾芳成李科录朱晓峰赵卿波
Owner PETROCHINA CO LTD
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