Method for preparing anhydrous halogenated rare earth through vacuum microwave dehydration

A vacuum microwave and vacuum microwave drying technology, which is applied in the direction of drying solid materials, lighting and heating equipment, drying solid materials, etc., can solve the problem of reducing the one-time yield of anhydrous rare earth halides, easy formation of rare earth oxyhalides, and dehydration Long time and other problems, to achieve the effect of improving equipment utilization, high heat energy utilization, and high dehydration efficiency

Pending Publication Date: 2021-04-20
TIANJIN BAOGANG RES INST OF RARE EARTHS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

External heating dehydration is heat transferred from the outside to the surface of the rare earth halide containing crystal water, and then the heat is gradually transferred to the inside, which will easily cause the dehydrated rare earth halide to react with the water released from the inside, and the surface is easy to generate halogen oxidation. For rare earths, pure anhydrous rare earth halides can only be obtained by stripping off the rare earth oxyhalides generated on

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0018] Example 1

[0019] 800g of cerium chloride heptahydrate with a water content of 33% was placed in a ceramic container, and then the ceramic container was placed in a vacuum microwave drying oven. The radiation frequency of the microwave magnetron was 2450MHz and the output power was 2000W. The equipment was pumped. Vacuum treatment, the vacuum degree is maintained at -0.09MPa, the temperature range in the equipment is 80 °C for 20 minutes, rise to 150 °C for 40 minutes, and then rise to 250 °C for 60 minutes, after cooling, take out the material, anhydrous cerium chloride is added to the water quickly Dissolved, the dissolved aqueous solution is clear and transparent, the water content of anhydrous cerium chloride is 0.38% by detection and analysis, and the purity of anhydrous cerium chloride is greater than 99.5%.

Example Embodiment

[0020] Example 2

[0021] 3000g of neodymium chloride hexahydrate with a water content of 30% was placed in a ceramic container, and then the ceramic container was placed in a vacuum microwave drying oven. The radiation frequency of the microwave magnetron was 2450MHz and the output power was 6000W, and the equipment was pumped. Vacuum treatment, the vacuum degree is kept at -0.094MPa, the temperature range in the equipment is 80 °C for 10 minutes, rise to 150 °C for 30 minutes, and then rise to 240 °C for 100 minutes, after cooling, take out the material, anhydrous neodymium chloride is added to the water quickly Dissolved, the dissolved aqueous solution is clear and transparent, the water content of the anhydrous neodymium chloride is 0.35% by detection and analysis, and the purity of the anhydrous neodymium chloride is greater than 99.5%.

Example Embodiment

[0022] Example 3

[0023] Put 200g of lanthanum bromide heptahydrate with a water content of 25% in a ceramic container, and then put the ceramic container into a vacuum microwave drying oven. The radiation frequency of the microwave magnetron is 2450MHz and the output power is 1000W, and the equipment is pumped. Vacuum treatment, the vacuum degree is kept at -0.097MPa, the temperature range in the equipment is 60 °C for 5 minutes, rise to 130 °C for 5 minutes, then rise to 220 °C for 10 minutes, after cooling, take out the material, anhydrous lanthanum bromide is added to the water quickly Dissolved, the dissolved aqueous solution is clear and transparent, the water content of the anhydrous lanthanum bromide is 0.43% by detection and analysis, and the purity of the anhydrous lanthanum bromide is greater than 99.5%.

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Abstract

The invention provides a method for preparing anhydrous halogenated rare earth through vacuum microwave dehydration. The method comprises the following steps that halogenated rare earth containing crystal water is filled into a container, and the container is dehydrated in a vacuum microwave drying oven at the dehydration temperature of 60-260 DEG C; and the temperature of the vacuum microwave drying oven is programmed, the vacuum degree is -0.09 MPa to -0.1 MPa, and the microwave frequency is 2450 MHz +/-50 Hz. According to the method for preparing the anhydrous halogenated rare earth through vacuum microwave dehydration, the inside and the outside of the halogenated rare earth containing the crystal water can be simultaneously heated, the dehydration rate of each part of the halogenated rare earth containing the crystal water tends to be consistent, the heating is uniform, the temperature rise is fast, and the generation of by-products can be effectively inhibited; and meanwhile, the dehydration efficiency is high, the dehydration time is greatly shortened, and the water content of the finally obtained anhydrous halogenated rare earth is less than or equal to 0.5%.

Description

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Claims

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Application Information

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Owner TIANJIN BAOGANG RES INST OF RARE EARTHS
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