Method for promoting rare earth carbonate to be converted into rare earth fluoride and recovering ammonia water

A rare earth carbonate and rare earth fluoride technology, applied in the fields of rare earth metal fluoride, rare earth metal halide, chemical instruments and methods, etc., can solve the problems of high fluorine content, no mention of ammonia water recovery, etc., and improve the conversion of fluorine. rate effect

Active Publication Date: 2020-05-29
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 rare earth carbonate to be converted into rare earth fluoride and recovering ammonia water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Mix hydrofluoric acid and ammonia water to obtain a fluoroammonia composite fluorinating agent. The fluoride ion concentration in the fluorine ammonia composite fluorinating agent is 4mol / L, F - with NH 4 + The molar ratio is 1:1, and the pH value is 6.3.

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

[0054] Add 208ml of fluoroammonia composite fluorinating agent into the lanthanum carbonate slurry to form a mixed solution. The mixed solution was reacted at 60° C., and the mixed solution was blown with air until the pH value was 7.1. The tail gas is absorbed by water circulation to obtain ammonia water with a concentration of 18.3 wt%.

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

Embodiment 2

[0057] Sodium fluoride and ammonia water are mixed to obtain a fluoroammonia composite fluorinating agent, and heated to 40°C for use. The fluoride ion concentration in the fluorine ammonia compound fluorinating agent is 2mol / L, F - with NH 4 + The molar ratio is 1:0.5, and the pH value is 7.5.

[0058] Add 100 g of basic lanthanum carbonate (47.6 wt % of REO) into 438 ml of fluoroammonia composite fluorinating agent to form a mixed solution. The mixed solution was reacted at 40° C., and the mixed solution was blown with air until the pH value was 7.1. The tail gas is absorbed by water circulation to obtain ammonia water with a concentration of 17.6wt%.

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

Embodiment 3

[0061] Sodium fluoride and ammonia water are mixed to obtain a fluoroammonia composite fluorinating agent. The fluoride ion concentration in the fluorine ammonia compound fluorinating agent is 6mol / L, F - with NH 4 + The molar ratio is 1:0.8, and the pH value is 8.2.

[0062] 100 g of lanthanum cerium carbonate (43.2 wt % of REO) was uniformly slurried with 50 ml of deionized water to form a lanthanum cerium carbonate slurry, which was heated to 60° C. for later use.

[0063] Add 128ml of fluoroammonia composite fluorinating agent into the lanthanum cerium carbonate slurry to form a mixed solution. The mixed solution was reacted at 60° C., and the mixed solution was blown with air until the pH value was 7. Tail gas is absorbed by water circulation to obtain ammonia water with a concentration of 17.5wt%.

[0064] The reacted mixed liquid is separated from solid and liquid, and the filter cake is dried to obtain lanthanum cerium fluoride. The fluorine conversion rate was 9...

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Abstract

The invention discloses a method for promoting rare earth carbonate to be converted into rare earth fluoride and recovering ammonia water, which comprises the following steps: heating a mixed solutionof a fluorine-ammonia composite fluorinating agent and rare earth carbonate, blowing the mixed solution by using gas, and absorbing ammonia gas in tail gas by using water, wherein the fluorine-ammonia composite fluorinating agent is a mixed solution of a fluorine-containing inorganic matter and ammonia water, and the pH value of the fluorine-ammonia composite fluorinating agent is greater than orequal to 6. According to the method, rare earth carbonate can be almost completely converted into rare earth fluoride, the conversion rate of fluorine is high, and meanwhile ammonia water can be recycled.

Description

technical field [0001] The invention relates to a method for wet preparation of rare earth fluorides, in particular to a method for promoting the transformation of rare earth carbonates into rare earth fluorides and recovering ammonia water. Background technique [0002] The preparation methods of rare earth fluorides can be divided into wet process and dry process. The dry process is generally carried out at high temperature, and the fluorinating agent includes hydrogen fluoride gas and ammonium bifluoride solid. When using hydrogen fluoride gas to fluorinate rare earth oxides, it is necessary to protect the highly 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 fluorides by solid fluorination of ammonium bifluoride is carried out under high temperature and low vacuum, which can avoid the discharge of strong corrosive hydrogen fluoride gas, but after ...

Claims

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Application Information

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Patent Type & Authority Applications(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
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