Method for preparing high-purity mixed rare earth chloride by sulfuric acid rare earth water leaching liquid neutralization, impurity removal and recycling

A technology of rare earth chloride and rare earth sulfate, applied in the direction of improving process efficiency, etc., can solve the problems of rare earth ammonium sulfate double salt precipitation, sulfate crystallization, etc., to reduce the difficulty of treatment, reduce contact, and prevent the production of rare earth ammonium sulfate double salt Effect

Active Publication Date: 2019-01-15
BAOTOU RES INST OF RARE EARTHS +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem solved by the present invention is to provide a method for neutralizing and removing impurities in rare earth sulfate water immersion liquid and circulating to prepare high-purity mixed rare earth chloride, which solves the process of neutralizing rare earth sulfate pulp clear liquid, removing calcium, magnesium, and sulfate wastewater The crystallization of sulfate in medium, and the precipitation of rare earth ammonium sulfate double salt in the process of ammonia neutralization and precipitation

Method used

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  • Method for preparing high-purity mixed rare earth chloride by sulfuric acid rare earth water leaching liquid neutralization, impurity removal and recycling

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) The deployment of neutralizer: mixed rare earth carbonate: ammonia water=10:1 (molar ratio);

[0022] (2) Neutralization: the 30°C ore pulp clear liquid is neutralized with the prepared neutralizer to a pH value of 4.0, and the water immersion liquid and neutralized slag are obtained by separation. After the neutralized slag is mixed with water, it returns to the roasted ore leaching process;

[0023] (3) Precipitation transformation: water immersion liquid and ammonium bicarbonate precipitant co-flow and precipitate until the final pH value is 6.8, which is prepared as rare earth carbonate, and pure ammonium sulfate wastewater is obtained by separation, with a concentration of MgO of 0.21g / L and a concentration of CaO of 0.26g / L, ammonium sulfate by-product and reused water are obtained through concentrated crystallization;

[0024] (4) Recycling: Take mixed rare earth carbonate compounds according to demand, continue to be used to neutralize the clear liquid of o...

Embodiment 2

[0026] (1) The deployment of neutralizing agent: mixed alkaline rare earth compound: ammonium bicarbonate: ammoniacal liquor=1:5:10 (molar ratio of effective substance);

[0027] (2) Neutralization: The pulp clear liquid at 20°C is neutralized with the prepared neutralizer to a pH value of 4.2, and the water immersion liquid and neutralized slag are obtained by separation. After the neutralized slag is mixed with water, it returns to the roasted ore leaching process;

[0028] (3) Precipitation transformation: Ammonia water and ammonium bicarbonate are prepared as a mixed precipitant according to the molar ratio of 2:1, and the water immersion liquid and the mixed precipitant are precipitated in parallel until the final pH value is 6.2, and a mixed alkaline rare earth compound is prepared. Separate and obtain pure ammonium sulfate wastewater, its MgO concentration is 0.23g / L, CaO concentration is 0.32g / L, ammonium sulfate by-product and reuse water are obtained through concentr...

Embodiment 3

[0031] (1) Preparation of neutralizing agent: mixed rare earth carbonate: ammonium carbonate=99:1 (molar ratio).

[0032] (2) Neutralization: the 40°C ore pulp clear liquid is neutralized with the prepared neutralizer to a pH value of 3.8, and the water immersion liquid and neutralized slag are obtained by separation. After the neutralized slag is slurried with water, it returns to the roasted ore leaching process.

[0033] (3) Precipitation transformation: Ammonia water and ammonium bicarbonate are prepared as a mixed precipitant according to the molar ratio of 1:1, and the water immersion liquid and the mixed precipitant are precipitated in parallel until the final pH value is 6.5, and the mixed rare earth carbonate is prepared, separated Obtain pure ammonium sulfate waste water, its MgO concentration is 0.1g / L, CaO concentration is 0.2g / L, obtain ammonium sulfate by-product and reuse water through concentration and crystallization.

[0034] (4) Recycling: Collect mixed rar...

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Abstract

The invention discloses a method for preparing a high-purity mixed rare earth chloride by sulfuric acid rare earth water leaching liquid neutralization, impurity removal and recycling. The method comprises the steps that mixed rare earth ore concentrate is subjected to concentrated sulfuric acid high-temperature roasting and water leaching, then water leaching slag and slurry clear liquid are obtained, and the temperature of the slurry clear liquid is less than or equal to 40 DEG C; the slurry clear liquid is neutralized with a neutralizing agent to a pH of 3.8-4.5, separation is carried out,and water leaching liquid and neutralization slag are obtained; the water leaching liquid is subjected to ammonia precipitant cocurrent flow precipitation and prepared into a mixed alkaline rare earthcompound so as to obtain ammonium sulfate wastewater and the mixed alkaline rare earth compound; and mixed rare earth carbonate in the mixed alkaline rare earth compound is subjected to hydrochloricacid dissolution and transformed into the high-purity mixed rare earth chloride suitable for extraction and separation. The problems of sulphate crystallization in the sulphuric acid rare earth slurryclear liquid neutralization calcium-and-magnesium removal and sulphate wastewater concentration process and ammonia double salt precipitation of sulfuric acid rare earth in the ammonia neutralizationand precipitation process are solved.

Description

technical field [0001] The invention relates to a hydrometallurgical technology, in particular to a method for neutralizing and removing impurities in a sulfuric acid rare earth immersion solution and circulating to prepare a high-purity mixed rare earth chloride. Background technique [0002] The mixed rare earth concentrates in Baotou area are mainly processed by concentrated sulfuric acid high-temperature roasting process. The process includes mixed high-temperature roasting of rare earth concentrates and concentrated sulfuric acid, water leaching, magnesium neutralization and impurity removal, transformation (carbon precipitation or extraction) and other links. Although the process is simple and has strong applicability to mineral grades, it also has the problem of "three wastes" that are difficult to deal with, and among the "three wastes" is the problem of wastewater. [0003] In the current production process, in the process of extracting rare earth minerals into rare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B1/06C22B3/04C22B59/00C22B3/44
CPCC22B1/06C22B3/04C22B3/44C22B59/00Y02P10/20
Inventor 崔建国刘磊王哲张正中侯睿恩彭靖高婷徐萌孟志军
Owner BAOTOU RES INST OF RARE EARTHS
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