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Preparation method and system of high-purity rare earth carbonate

A rare earth carbonate, high-purity technology, applied in the direction of improving process efficiency, can solve the problems of difficult rare earth recovery, serious rare earth encapsulation, low direct recovery rate of rare earth, etc.

Active Publication Date: 2019-11-08
GANZHOU NONFERROUS METALLURGICAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (3) The concentration of rare earths in the early and late stages of the leaching mother liquor is generally low. In order to collect the rare earths in the low-concentration feed liquid, the consumption ratio of the precipitant is greatly increased, resulting in a large unit consumption of the precipitant, especially when the concentration of rare earths is lower than 0.10g / When L, the rare earth is difficult to recover, which affects the rare earth yield;
Especially when Al in mixed rare earth carbonate 2 o 3 When the content is high, the neutralization and impurity removal effect of the rare earth decomposition liquid is poor, and it takes a long aging time to separate the solid and liquid, the amount of slag is large, and the direct recovery rate of rare earth is low
The aluminum hydroxide and ferric hydroxide precipitates contained in the neutralization slag produced during the impurity removal process are colloidal in the pH range, which is not easy to filter, and the slag has a high moisture content and is heavily wrapped with rare earths, which can be as high as 8% to 10% of the total amount of rare earths. , leading to a low direct recovery rate of rare earth
In order to recover the rare earths in the iron-aluminum slag, it is necessary to consume a large amount of hydrochloric acid to remelt the slag and oxalic acid to precipitate and recover the rare earths, resulting in repeated consumption of acid and alkali

Method used

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  • Preparation method and system of high-purity rare earth carbonate
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  • Preparation method and system of high-purity rare earth carbonate

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preparation example Construction

[0033] The invention provides a kind of preparation method of high-purity rare earth carbonate, comprising the following steps:

[0034] (1) filtering the rare earth feed liquid to obtain a filtrate;

[0035] (2) passing the filtrate into a cation exchange resin for adsorption to obtain a loaded resin; the cation in the cation exchange resin is a cation capable of forming a soluble carbonate;

[0036] (3) leaching the loaded resin with a leaching agent to obtain a loaded rare earth ion resin; the leaching agent is ammonia water or a metal hydroxide solution;

[0037] (4) Use a desorbent to desorb the loaded rare earth ion resin to obtain blank resin and rare earth carbonate precipitation; the desorbent is a carbonate solution or a bicarbonate solution;

[0038] (5) washing after filtering the rare earth carbonate precipitate to obtain high-purity rare earth carbonate;

[0039] Wherein, the cation species in the cation exchange resin, the eluent and the desorbent are the same...

Embodiment 1

[0071] choose C (REO) =1.52g / L, C (总Fe) =0.44mg / L, C (Al 3+ ) = 0.35g / L mine leaching mother liquor, filter the sediment and suspended solids with a ceramic filter, and then enter the Φ100×1000mm ion exchange column to be mixed with NH 4 + The type TP207 resin is dynamically adsorbed to equilibrium (when the concentration of REO in the adsorbed liquid and the adsorbed mother liquid is equal, it is regarded as the adsorption equilibrium). The height of the resin column is 600mm. L of ammonia water was rinsed at a rate of 0.25 L / min, and after the rinse was completed, rinsed once with pure water, and the obtained loaded rare earth ion resin was desorbed with a saturated ammonium bicarbonate solution under the action of air flow to obtain NH 4 + Type TP207 resin and rare earth carbonate were precipitated, and the rare earth carbonate precipitate was filtered and washed to obtain high-purity rare earth carbonate. The test results are shown in Table 1.

[0072] Table 1 NH 4...

Embodiment 2

[0075] choose C (REO) =1.02g / L, C (总Fe) =0.34mg / L, C (Al 3+ ) = 0.26g / L mine leaching mother liquor, filter the sediment and suspended solids with a ceramic filter, and then enter the ion exchange column of Φ100×1000mm to be mixed with Na + The type TP207 resin is dynamically adsorbed to equilibrium (when the concentration of REO in the adsorbed liquid and the adsorbed mother liquid is equal, it is regarded as the adsorption equilibrium). The height of the resin column is 600mm. L of ammonia water is rinsed at a speed of 0.15L / min, and rinsed once with pure water after the rinse is completed, and the resulting loaded rare earth ion resin is desorbed with a saturated sodium carbonate solution under the action of air flow to obtain Na + Type TP207 resin and rare earth carbonate were precipitated, and the rare earth carbonate precipitate was filtered and washed to obtain high-purity rare earth carbonate. The test results are shown in Table 2.

[0076] Table 2 Na + Systemati...

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Abstract

The invention relates to the technical field of a rare earth material and provides a preparation method of high-purity rare earth carbonate. The preparation method comprises the following steps: firstly, filtering rare earth material liquid, introducing the filtered rare earth material liquid into cation exchange resin to adsorb and adsorbing rare earth ions and impurity ions to the resin to obtain loaded resin; then performing drip washing on the loaded resin and eluting the impurity ions to obtain rare earth ion loaded resin; finally, desorbing the rare earth ion loaded resin by a carbonateor hydrocarbonate solution, filtering rare earth carbonate precipitate obtained through desorption and washing to obtain the high-purity rare earth carbonate. Desorption of the rare earth ion loaded resin, resin transformation and rare earth carbonate precipitation are synthesized into one process, so the operation process is simplified, the production cost is reduced, the civil engineering investment is reduced, the investment utilization rate is increased and resources are saved. The invention also provides a preparation system of the high-purity rare earth carbonate. The system is simple instructure and small in occupied area and can be integrally moved along with transfer of a mining point.

Description

technical field [0001] The invention relates to the technical field of rare earth materials, in particular to a method and system for preparing high-purity rare earth carbonate. Background technique [0002] During the mining and extraction of rare earths, a large amount of low-concentration rare earth feed liquid (REO concentration ≤ 2g / L) will be produced. The mine leaching mother liquid, tailings leachate, tailings leaching water, Lime slag leaching solution, etc. are low-concentration rare earth feed liquids, and the feed liquids also contain more impurity ions, such as iron and aluminum. When preparing rare earth products, rare earths need to be enriched and removed. [0003] Taking the process of preparing ionic rare earth ore mother liquor into the tank as an example, in the process of preparing rare earth products, ammonium sulfate leaching-ore leaching mother liquor pH adjustment and impurity removal-mine leaching mother liquor carbonate precipitation-rare earth car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B3/22C22B3/24
CPCC22B3/22C22B3/24C22B59/00Y02P10/20
Inventor 周洁英陈东英张积锴杨新华赖兰萍伍莺
Owner GANZHOU NONFERROUS METALLURGICAL RES INST