Preparation method of crystalline rare-earth carbonate

A technology of rare earth carbonate and crystal form, which is applied in the field of hydrometallurgy, can solve the problems of difficult formation of rare earth carbonate of crystal form, unqualified quality of rare earth products, and low purity of rare earth products, so as to achieve less loss of rare earth, improve economic benefits of enterprises and Social benefits, the effect of improving the recovery rate of rare earths

Inactive Publication Date: 2014-12-10
HUBEI POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second is to use ammonium bicarbonate as a precipitant to precipitate rare earths, but no matter whether oxalic acid is used as a precipitant or ammonium bicarbonate is used as a precipitant, there are impurities such as iron, aluminum, and calcium contained in the rare earth leaching solution, which makes the obtained The quality of rare earth products is unqualified
Especially impurity Al 3+ When ammonium bicarbonate precipitates rare earths, aluminum

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Select the weathering crust leaching type rare earth ore (such as Jiangxi Longnan weathering crust leaching type heavy rare earth ore), adopt the method of in-situ leaching, and prepare ammonium sulfate and ammonium chloride at a mass ratio of 1:1 to a mass fraction of 2 % of the mixed leaching agent, add 0.05% ammonium acetate in the mass of the mixed leaching agent, and after stirring evenly, leaching the ore in situ according to the liquid-solid ratio of 0.1:1; Wash the ore with top water, collect the leaching solution, put in the ammonium bicarbonate precipitant after clarification, the ratio of the ammonium bicarbonate precipitant to the leaching solution is 0.1:1, stir thoroughly for more than 30 minutes, let stand and age for 6 hours, filter, and wash the precipitate with water Twice, filter again, and dry at 110°C to obtain crystalline rare earth carbonate; the recovery rate is 78%, and the purity is 92%.

Embodiment 2

[0017] Select weathering crust leaching type rare earth ores (such as Jiangxi Longnan weathering crust leaching type heavy rare earth ore), adopt the method of in-situ leaching, and prepare ammonium sulfate and ammonium nitrate at a mass ratio of 4:1 to a mass fraction of 2% 0.05% ammonium acetate in the mass of the mixed leaching agent, and after stirring evenly, leaching the ore in situ at a liquid-solid ratio of 2:1; Wash the ore with water, collect the leaching solution, and put the ammonium carbonate precipitant after clarification. The ratio of the ammonium carbonate precipitant to the leaching solution is 0.5:1, fully stir for more than 30 minutes, let stand and age for 24 hours, filter, and wash the precipitate twice with water. Filter again and dry at 110°C to obtain crystalline rare earth carbonate; the recovery rate is 83%, and the purity is 91%.

Embodiment 3

[0019] Select weathering crust leaching type rare earth ores (such as Jiangxi Longnan weathering crust leaching type heavy rare earth ore), adopt the method of in-situ leaching, and prepare ammonium chloride and ammonium nitrate at a mass ratio of 2:1 to make a mass fraction of 2 % of the mixed leaching agent, add 0.05% ammonium acetate in the mass of the mixed leaching agent, and after stirring evenly, leaching the ore in situ according to the liquid-solid ratio of 1.5:1; Wash the ore with top water, collect the leaching solution, put in the ammonium bicarbonate precipitant after clarification, the ratio of the ammonium bicarbonate precipitant to the leaching solution is 0.2:1, fully stir for more than 30 minutes, let stand and age for 12 hours, filter, and wash the precipitate with water Twice, filter again, and dry at 110°C to obtain crystalline rare earth carbonate; the recovery rate is 85%, and the purity is 95%.

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Abstract

The invention relates to a preparation method of crystalline rare-earth carbonate. According to the scheme, the method comprises the following steps: selecting ion absorpt deposit and carrying out an in-situ leaching method, wherein the in-situ leaching method comprises the following steps: preparing a mixed leaching agent with the mass fraction being 2% by using two ammonium salts which are in a mass ratio of (1-4) to 1, adding an aluminum inhibitor which is 0.05% of mass of the mixed leaching agent, stirring evenly, and then carrying out in-situ leaching according to a liquid-solid ratio of (0.1-2) to 1; after the leaching solution completely seeps, adding top wash ore which is 10% of mass of the leaching agent, collecting the leaching solution, clarifying, and adding a precipitator, wherein the mass ratio of the precipitator to the leaching solution is (0.1-0.5) to 1; fully stirring for over 30 minutes, and standing and ageing for 6-24hours; filtering, washing sediment twice with clear water, filtering again, and baking at 110 DEG C, so as to obtain the crystalline rare-earth carbonate, wherein the recovery rate is 70-85%, and the purity is 90-95%. The crystalline rare-earth carbonate is prepared from easily available raw materials and is low in cost, high in recovery rate and high in product purity.

Description

technical field [0001] The invention relates to a new process method for in-situ leaching of rare earth carbonate in the field of hydrometallurgy, in particular to a preparation method of crystalline rare earth carbonate. Background technique [0002] my country is a country with a large reserve of rare earth carbonate resources, as well as a major country in the production, application and export of rare earth carbonate products. Rare earth carbonate has the characteristics of improving the elasticity, toughness and strength of metals. It is an important part of jet aircraft, missiles, engines and heat-resistant machinery, and can also be used as a protective shell for radiation protection. Rare earth carbonates are mainly derived from weathering crust leaching type rare earth deposits, which have the characteristics of wide distribution, mostly in hilly areas, low grade, and fine ore particle size. Rare earth carbonates are mainly adsorbed on clay minerals with hydrated io...

Claims

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Application Information

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IPC IPC(8): C22B3/14C22B3/44C22B59/00
CPCY02P10/20
Inventor 左小华刘庆斌邓祥义刘凯池汝安
Owner HUBEI POLYTECHNIC UNIV
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