Method for preparing neodymium chloride hydrate through programmed temperature increasing method

A technology of neodymium chloride monohydrate and temperature programming, which is applied in chemical instruments and methods, rare earth metal chlorides, inorganic chemistry, etc., can solve the problems of not containing water-insoluble substances and high energy consumption, and can reduce dehydration costs and pollutants Emissions and low energy consumption

Active Publication Date: 2017-07-04
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] 200kg of NdC1 3 ·6H 2 O into the dehydration reactor, start the dehydration reactor to stir, pass in nitrogen preheated by low-pressure steam, start the vacuum pump to vacuum, when the vacuum degree 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; from 100°C to 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 is 0.167℃ / min, heating time is 2 hours, holding time at 140℃ is 4 hours; 140℃~158℃, heating rate is 0.15℃ / min, heating time is 2 hours, holding time at 158℃ After 10 hours, when the temperature of the kettle body dropped to 50° C. naturally, the obtained neodymium chloride monohydrate 155 kg was analyzed and detected to have a water content of 6.8%.

[0016] Since this embodiment is implemented on an industrial device, ...

Embodiment 2

[0018] 200kg of NdC1 3 ·6H 2 O is put into the dehydration reaction kettle, start the dehydration kettle to stir, pass in the nitrogen preheated by the low-pressure steam, start the vacuum pump to evacuate, when the vacuum degree reaches 50kpa, set the heating program and start heating. The heating program is as follows: from room temperature to 100°C, the heating rate is 0.625°C / min, the heating time is 2 hours, and the holding time at 100°C is 3 hours; from 100°C to 120°C, the heating rate is 0.167°C / min, and the heating time is 2 hours. 120°C holding time 6 hours; 120°C~140°C, heating rate 0.167°C / min, heating time 2 hours, 140°C holding time 4 hours; 140°C~158°C, heating rate 0.15°C / min, heating time 2 hours, 10 hours at 158 ​​DEG C of holding time, when the temperature of the kettle body naturally dropped to 50 DEG C, the obtained neodymium chloride monohydrate 151 kg was analyzed and detected to have a water content of 7.6%.

[0019] Since this embodiment is implemente...

Embodiment 3

[0021] 200kg of NdC1 3 ·6H 2 O is put into the dehydration reaction kettle, start the dehydration kettle to stir, pass in the nitrogen preheated by the low-pressure steam, start the vacuum pump to evacuate, when the vacuum degree reaches 50kpa, set the heating program and start heating. The heating program is as follows: from room temperature to 100°C, the heating rate is 0.625°C / min, the heating time is 2 hours, and the holding time at 100°C is 3 hours; from 100°C to 120°C, the heating rate is 0.167°C / min, and the heating time is 2 hours. The holding time at 120°C is 6 hours; from 120°C to 140°C, the heating rate is 0.167°C / min, and the heating time is 2 hours; at 140°C, the holding time is 4 hours; 2 hours, 10 hours at 158 ​​DEG C of holding time, when the kettle body temperature naturally dropped to 50 DEG C, the obtained neodymium chloride monohydrate 155 kg was analyzed and detected to have a water content of 6.6%.

[0022] Since this embodiment is implemented on an ind...

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PUM

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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 programming 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 about 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] "NdCl 3 -LiCl and NdCl 3 -Research on the phase diagram of the LiCl-NaCl system", Acta Chemie Sinica, 1989, 47 (1): 14-18. A preparation method of anhydrous neodymium chloride is provided, and NdCl 3 ·6H 2 O on P 2 o 5 Preliminary dehydration in a desiccator, then dehydration step by step while heating in HCl atmosphere to obtain ...

Claims

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Application Information

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Patent Type & Authority Applications(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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