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Rare earth fluoride and preparation method and application thereof

A technology of rare earth fluorides and waste materials, which is applied to the preparation/treatment of rare earth metal fluorides, rare earth metal compounds, rare earth metal halides, etc., and can solve the problems of high cost, large water consumption, and low added value

Pending Publication Date: 2021-05-04
JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, the above-mentioned treatment process is cumbersome to operate, high in cost, low in added value, and large in water consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] This embodiment provides a method for preparing rare earth fluorides from scintillation crystal waste, which specifically includes the following steps:

[0042] (1) After 500 g of lutetium silicate scintillation crystal waste is crushed through a 100-mesh sieve, it is washed 3 times with 50 L of deionized water, and filtered;

[0043] (2) Then put it into a vacuum drying smelting furnace and keep vacuum drying at 600°C for 10 hours;

[0044] (3) Put the dried powder into the high-purity graphite crucible of the fluorination reaction furnace, feed dry HF gas: a mixed gas with a volume ratio of Ar gas of 1:3 for reaction, react at 700°C for 48h, and generate gaseous SiF 4 and H 2 O and other tail gases are absorbed by sodium hydroxide solution;

[0045] (4) the prepared lutetium fluoride is naturally cooled to room temperature under nitrogen protection;

[0046] The prepared rare earth lutetium fluoride has a purity of 99.99%, a yield of 98.5%, an oxygen content of 85 p...

Embodiment 2

[0048] This embodiment provides a method for preparing rare earth fluorides from scintillation crystal waste, which specifically includes the following steps:

[0049] (1) After 500 g of yttrium lutetium silicate scintillation crystal waste material is crushed through a 100 mesh sieve, it is washed 3 times with 50L deionized water, and filtered;

[0050] (2) Then put it into a vacuum drying smelting furnace, and keep vacuum drying at 800°C for 20h;

[0051] (3) Put the dried powder into the high-purity graphite crucible of the fluorination reaction furnace, feed a mixed gas with a volume ratio of dry HF gas and nitrogen gas of 1:3 to react, react at 900°C for 10h, and generate gaseous SiF 4 and H 2 O and other tail gases are absorbed by potassium hydroxide solution;

[0052] (4) the prepared yttrium lutetium fluoride is naturally cooled to room temperature under the protection of argon;

[0053] The prepared rare earth yttrium lutetium fluoride has an analyzed purity of 99...

Embodiment 3

[0055] This embodiment provides a method for preparing rare earth fluorides from scintillation crystal waste, which specifically includes the following steps:

[0056] (1) After 500 g of yttrium lutetium silicate scintillation crystal waste material is crushed through a 100 mesh sieve, it is washed 2 times with 50L deionized water, and filtered;

[0057] (2) Then put it into a vacuum drying smelting furnace, and keep vacuum drying at 800°C for 20h;

[0058] (3) Put the dried powder into the high-purity graphite crucible of the fluorination reaction furnace, feed a mixed gas with a volume ratio of dry HF gas and nitrogen gas of 1:7 to react, and react at 700°C for 17h, during the reaction process The gaseous SiF produced 4 and H 2 O and other tail gases are absorbed by potassium hydroxide solution;

[0059] (4) the prepared yttrium lutetium fluoride is naturally cooled to room temperature under the protection of argon;

[0060] The prepared rare earth yttrium lutetium fluor...

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Abstract

The invention relates to a rare earth fluoride and a preparation method and application thereof. The method comprises the following steps: carrying out heat treatment on powder of scintillation crystal waste in a mixed atmosphere, and then cooling in a protective atmosphere to obtain the rare earth fluoride. The method is characterized by crushing and grinding the scintillation crystal waste into fine powder, performing washing and then, carrying out vacuum high-temperature drying to remove water and impurities; and carrying out high-temperature treatment to make silicon and oxygen elements in lutetium(yttrium)oxyorthosilicate converted into gaseous SiF4 and H2O, discharging the gaseous SiF4 and H2O, and absorbing the gaseous SiF4 and H2O by alkali liquor. The high-purity rare earth fluoride in the fluorination reaction furnace is taken out after being naturally cooled, can be used for preparing high-purity metal, fluorescent materials, special additives and other high-end materials, and can be used for preparing high-purity rare earth metal through a reduction method due to the fact that the impurity content and the oxygen content of the high-purity rare earth fluoride are extremely low.

Description

technical field [0001] The invention relates to the field of solid waste reuse, in particular to a rare earth fluoride and its preparation method and application. Background technique [0002] Rare earth is known as the "gold" of industry. It has excellent optical, electromagnetic and other physical properties. It can form a variety of new materials with different properties and varieties with other materials. It is widely used in metallurgical machinery, petrochemical industry, light industry and agriculture, and electronic information. More than 40 industries in 13 fields, such as energy and environmental protection, national defense and military industry, and high-tech materials, are indispensable strategic materials for the transformation of traditional industries in various countries in the world today and the development of high-tech and cutting-edge national defense technologies. [0003] In recent years, lutetium-based compounds have aroused great interest due to the...

Claims

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Application Information

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IPC IPC(8): C01F17/265C01F17/10H01S3/16C22C28/00
CPCC01F17/265C01F17/10H01S3/1603C22C28/00C01P2006/80
Inventor 肖吉昌宗国强安华英余东海
Owner JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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