Method for treating and recycling rare earth oxalate precipitation mother solution

A recovery method and technology for precipitating mother liquor, applied in chemical instruments and methods, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problems of complex process, low oxalic acid extraction efficiency, and high equipment requirements. Simple method, significant economic and social benefits

Inactive Publication Date: 2013-03-20
NANCHANG UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods have their own advantages and disadvantages. For example, although the neutralization method can eliminate the impact of acid on the environment, it consumes alkali and discharges a large amount of saline wastewater.
Using the extraction method, oxalic acid can be extracted, but under acidic conditions, the

Method used

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  • Method for treating and recycling rare earth oxalate precipitation mother solution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Get the supernatant after the precipitation of 100ml high-purity yttrium oxalic acid respectively, add different volumes of high-purity yttrium feed liquid (Y 2 o 3 / REO≥99.999%, 5NY), there is obvious white precipitate, stir and age for a certain period of time, filter, take the filtrate for analysis, and calculate the residual rate or removal rate of oxalate according to the oxalate content in the solution before and after precipitation. The results are shown in Table 1.

[0010] It can be seen from the results in Table 1 that with the increase of the amount of 5NY feed solution, the precipitation of yttrium oxalate increases, the content of oxalate in the solution decreases correspondingly, and the removal rate of oxalate increases. At the beginning, the removal rate of oxalic acid caused by the addition of each milliliter of feed liquid increased rapidly, and the increase after 6 milliliters was small, and the removal rate was above 70%. When feeding, the ...

Embodiment 2

[0016] Prepare stripping acid (5 mol / l hydrochloric acid solution) with the above-mentioned solutions with different oxalic acid contents (concentration from 0.027-0.16mol / l) obtained through different degrees of treatment, and carry out stripping with P507-kerosene organic phase loaded with high-purity yttrium Experiment, compared to O / W=1:4. The results show that although the hydrochloric acid prepared from the untreated oxalic acid precipitation mother liquor is directly used for stripping the yttrium in the organic phase of P507-kerosene, no obvious white precipitate will be produced, but the rare earth analysis in the solution will be affected, and the end point will be delayed when titrated with EDTA. The tail is serious, and the concentration of oxalic acid in the water phase is also significantly reduced, generally below 0.04mol / l. It is proved that the presence of oxalic acid will affect the stripping of rare earths, and a part of oxalic acid will enter the organi...

Embodiment 3

[0018] Get the supernatant after the precipitation of 100ml high-purity yttrium oxalic acid respectively, add different weights of high-purity yttrium carbonate solid (Y 2 o 3 / REO≥99.999%, containing about 40% yttrium oxide, reacted with 5NY feed liquid and sodium bicarbonate to form yttrium carbonate precipitate, filtered after aging and crystallization, and dried at 50°C). Carbon dioxide gas is produced, and as the dissolved amount increases, the solution begins to appear turbid, and yttrium oxalate precipitates are formed. After aging for a certain period of time, filter and analyze the filtrate. Calculate the residual rate or removal rate of oxalate according to the oxalate content in the solution before and after precipitation, and the results are shown in Table 2. As the amount of yttrium carbonate increases, the precipitation of yttrium oxalate increases, the content of oxalate in the solution decreases accordingly, and the acidity also decreases. However, the decre...

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Abstract

The invention discloses a method for treating and recycling a rare earth oxalate precipitation mother solution. The method comprises the steps of: adding a corresponding high-purity rare earth solution or high-purity rare earth carbonate into the precipitation mother solution to separate oxalic acid out in the form of rare earth oxalate precipitates, wherein the filtered mother solution can be directly used for preparing hydrochloric acid solutions of different concentrations to serve as refluxing acid or washing acid for extraction separation of rare earth elements, so that water and hydrochloric acid in the mother solution can be recycled totally; and returning the filtered rare earth oxalate precipitates to a rare earth precipitation process to serve as crystal seeds which can be added in a refined oxalic acid dissolution process or in a precipitation barrel before precipitation starts respectively, and ageing, washing, filtering and calcining the precipitates to obtain a high-purity rare earth product, thereby recycling originally non-precipitated rare earth and subsequently added rare earth completely. According to the invention, the comprehensive recycling problem of the rare earth oxalate precipitation mother solution of a rare earth separation plant is solved, and the method is simple and feasible, is suitable for recycling all rare earth oxalate precipitation mother solutions, and has a wide application prospect.

Description

technical field [0001] The invention belongs to the field of rare earth hydrometallurgy and industrial wastewater treatment, and mainly solves the problem of recycling rare earth products, especially the rare earth oxalate precipitation mother liquor in the production of high-purity rare earth, and can make the mother liquor absolutely Most of the water, oxalic acid, hydrochloric acid and rare earths are recycled, saving costs and reducing wastewater discharge. technical background [0002] The rare earth feed liquid after rare earth extraction and separation is usually separated from water and a large amount of inorganic salts and acids by precipitation. Oxalic acid precipitation is generally used to precipitate rare earth elements from high-purity single rare earth solutions. In the rare earth oxalate precipitation process, in order to ensure the precipitation rate of rare earth and the separation selectivity of impurity ions, it is necessary to add excess oxalic acid. ...

Claims

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Application Information

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IPC IPC(8): C02F9/04C22B59/00
CPCY02P10/20
Inventor 李永绣谢爱玲王悦宋丽莎周新木周雪珍刘艳珠李静蔡立林徐欣何德华邬元旭
Owner NANCHANG UNIV
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