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Method for promoting the conversion of rare earth carbonate into rare earth fluoride and recycling ammonia

A rare-earth carbonate and rare-earth fluoride technology, applied in rare-earth metal fluorides, rare-earth metal halides, chemical instruments and methods, etc., can solve the problems of high fluorine content, unmentioned ammonia water recovery, etc., and improve the conversion of fluorine rate effect

Active Publication Date: 2022-06-14
BAOTOU RES INST OF RARE EARTHS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method uses excess hydrogen fluoride to further promote the fluorination conversion rate, resulting in high fluorine content in the wastewater, and does not mention the recovery of ammonia water

Method used

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  • Method for promoting the conversion of rare earth carbonate into rare earth fluoride and recycling ammonia

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Hydrofluoric acid is mixed with ammonia to give a fluorine ammonia composite fluorination agent. The concentration of fluoride ions in the fluorine ammonia composite fluorinating agent is 4mol / L, F - with NH 4 + The molar ratio is 1:1 and the pH is 6.3.

[0053] 100g lanthanum carbonate (REO is 45.3wt%) with 50ml deionized water to form lanthanum carbonate slurry, heated to 60 °C for later use.

[0054] 208ml of fluorine ammonia composite fluorination agent was added to the lanthanum carbonate slurry to form a mixture. The mixture was reacted at 60 °C and the mixture was blown with air to a pH of 7.1. The exhaust gas is absorbed through the water cycle to obtain ammonia with a concentration of 18.3wt%.

[0055] The mixture after the reaction was separated from the solid liquid, and the filter cake was dried to obtain lanthanum fluoride. The fluorine conversion rate was 99.6%.

Embodiment 2

[0057] The sodium fluoride was mixed with ammonia to obtain a fluorine-ammonia composite fluorination agent and heated to 40 °C for use. The concentration of fluoride ions in the fluorine ammonia composite fluorinating agent is 2mol / L, F - with NH 4 + The molar ratio is 1:0.5 and the pH is 7.5.

[0058]100g of basic lanthanum carbonate (REO is 47.6wt%) was added to 438ml of fluorine ammonia composite fluorinizing agent to form a mixture. The mixture was reacted at 40 °C and the mixture was blown with air to a pH of 7.1. The exhaust gas is absorbed by the water cycle to obtain ammonia with a concentration of 17.6wt%.

[0059] The mixture after the reaction was separated from the solid liquid, and the filter cake was dried to obtain lanthanum fluoride. The fluorine conversion rate was 99.7%.

Embodiment 3

[0061] Sodium fluoride is mixed with ammonia to give a fluorine compound fluorination agent. The concentration of fluoride ions in the fluorine ammonia composite fluorinating agent is 6mol / L, F - with NH 4 + The molar ratio is 1:0.8 and the pH is 8.2.

[0062] The 100g lanthanum carbonate cerium carbonate (REO is 43.2wt%) with 50ml of deionized water to uniformly mix the pulp to form lanthanum cerium carbonate slurry, heated to 60 °C for later use.

[0063] 128ml of fluorine ammonia composite fluorination agent was added to the lanthanum cerium carbonate slurry to form a mixture. The mixture is reacted at 60 °C and the mixture is blown with air to a pH of 7. The exhaust gas is absorbed by the water cycle to obtain a concentration of 17.5wt% ammonia.

[0064] The mixture after the reaction is separated from the solid liquid, and the filter cake is dried to obtain lanthanum cerium fluoride. The fluorine conversion rate was 99.9%.

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Abstract

The invention discloses a method for promoting the conversion of rare-earth carbonates into rare-earth fluorides and recovering ammonia water, which comprises the following steps: heating the mixed solution of fluorine-ammonia composite fluorinating agent and rare-earth carbonate, blowing the mixed solution with gas, At the same time, water is used to absorb ammonia in the tail gas; wherein, the fluorine-ammonia composite fluorinating agent is a mixed solution of fluorine-containing inorganic substances and ammonia water; the pH value of the fluorine-ammonia composite fluorinating agent is greater than or equal to 6. The method can convert the rare earth carbonate into rare earth fluoride almost completely, the conversion rate of fluorine is high, and ammonia water can be recovered at the same time.

Description

Technical field [0001] The present invention relates to a wet method for preparing rare earth fluoride, in particular to a method of promoting the conversion of rare earth carbonates into rare earth fluoride and recovering ammonia water. Background [0002] The preparation methods of rare earth fluoride can be divided into two categories: wet process and dry process. Dry processes are generally performed at high temperatures, and fluorinating agents include hydrogen fluoride gases and ammonium bifluoride solids. When using hydrogen fluoride gas to fluorinate rare earth oxides, it is necessary to protect the strong corrosive hydrogen fluoride gas, the furnace body needs anti-corrosion treatment, and the utilization rate of hydrogen fluoride is low. The process of preparing rare earth fluoride by solid fluorination of ammonium bifluoride is carried out under high temperature and low vacuum, which can avoid the emission of strongly corrosive hydrogen fluoride gas, but after fluorina...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/265C01C1/02
CPCC01C1/022
Inventor 崔建国徐萌陈禹夫高婷蔚腊先侯睿恩李雪菲王哲郭金铖
Owner BAOTOU RES INST OF RARE EARTHS