Method for preparing low-sulfur rare earth oxide through hydroxide precipitation

A technology of rare earth oxides and hydroxides, applied in the direction of improving process efficiency, etc., can solve the problem of high sulfate radicals, achieve the effect of preventing chemical adsorption and the process is simple and easy to control

Active Publication Date: 2016-07-27
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims at the problem that the sulfate group in the rare earth hydroxide precipitation obtained by the precipitation of rare earth sulfuric acid solution is too high, and provides a method for preparing low-sulfur rare earth oxides by direct precipitation with simple process and convenient operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]Take 10L of ion-adsorption type rare earth ore leach solution after impurity removal treatment, its rare earth concentration is 0.5g / L (REO calculation), and the sulfate concentration is 15g / L. First add acetylacetone in the leaching solution, make its concentration in the leaching solution be 0.5g / L, then add sodium hydroxide precipitating agent, the amount of used precipitating agent is 110wt.% of the completely required theoretical dosage of rare earth ion precipitation in the leaching solution, After reacting at 30° C. for 2 hours, solid-liquid separation was carried out to obtain rare earth hydroxide precipitate and precipitate mother liquor. The rare earth hydroxide precipitate is subjected to a water washing step to remove the water-soluble sulfate radical in the precipitate, and the water washing is stopped when the sulfate radical in the water washing filtrate is less than 10 ppm; then, the rare earth oxide is obtained by calcining at 800°C. The sulfur content i...

Embodiment 2

[0029] Take 10L of lanthanum sulfate solution, whose rare earth concentration is 5g / L (calculated by REO). First add lactic acid in leachate, make its concentration in lanthanum sulfate solution be 1g / L, then add calcium oxide precipitant, the amount of used precipitant is 105wt.% of the required theoretical dosage completely of rare earth ion precipitation in leachate, in After reacting at 40°C for 2 hours, solid-liquid separation is carried out to obtain lanthanum hydroxide precipitation and precipitation mother liquor, and the lanthanum hydroxide precipitation is subjected to a water washing step to remove water-soluble sulfate radicals in the precipitate, and stop washing when the sulfate radicals in the water washing filtrate are less than 10 ppm; Then it is calcined at 600°C to obtain lanthanum oxide. The sulfur content in the obtained lanthanum oxide was 0.46 wt%.

Embodiment 3

[0031] Take 10L of yttrium sulfate solution, whose rare earth concentration is 15g / L (calculated by REO). First add malonic acid in leachate, make its concentration in yttrium sulfate solution be 3g / L, then add sodium hydroxide precipitation agent, the amount of used precipitation agent is 115wt. %, after reacting at 15°C for 2 hours, solid-liquid separation is carried out to obtain yttrium hydroxide precipitation and precipitation mother liquor, and the yttrium hydroxide precipitation precipitation is carried out in a water washing step to remove the water-soluble sulfate radical in the precipitation. When the sulfate radical in the water washing filtrate is less than 10ppm Stop washing with water; then calcined at 700°C to obtain lanthanum oxide. The sulfur content in the obtained yttrium oxide was 0.47wt%.

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Abstract

The invention discloses a method for preparing a low-sulfur rare earth oxide through hydroxide precipitation. The method mainly comprises the following steps: 1, adding a soluble organic matter containing malic acid, acetylacetone and the like into a rare earth sulfate solution for mixing, so as to prepare a primary precipitation solution; 2, adding one or more alkaline precipitants into the primary precipitation solution for a precipitation reaction, wherein the consumption of the alkaline precipitants is 105-120% of the theoretical consumption of rare earth precipitating in the rare earth sulfate solution; and 3, carrying out solid-liquid separation to obtain a rare earth hydrate precipitate and a precipitation mother liquor, and subjecting the rare earth hydrate precipitate to calcination at 600-900 DEG C to obtain the low-sulfur rare earth oxide. The method provided by the invention has the advantages that through competitive coordination with sulfate, chemical adsorption of sulfate ions is avoided; meanwhile, a homogeneous-phase-like precipitation system can be formed, the forming of a crystalline precipitation is facilitated, and the precipitation process is simple and easy to control; the organic matter entering rare earth hydrate can be removed through roasting; and finally, the low-sulfur rare earth oxide can be obtained

Description

technical field [0001] The invention relates to the field of rare earth hydrometallurgy, in particular to a method for preparing low-sulfur rare earth oxides by a hydroxide precipitation method. Background technique [0002] Due to their unique 4f sublayer electronic structure, large atomic magnetic moment, strong spin-orbit coupling, and variable coordination numbers, the compounds formed by rare earth elements have very rich magnetic, optical, electrical, and catalytic properties. Functional properties, known as "the vitamin of modern industry" and "treasure house of new materials". Among them, rare earth oxides are an important class of rare earth compounds. They are also the main raw materials for the preparation of other rare earth compounds, and are widely used in the preparation of rare earth magnetic materials, luminescent materials, hydrogen storage materials, crystal materials, catalytic materials and other high-tech materials. . [0003] At present, there are va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/44C22B59/00
CPCC22B3/44C22B59/00Y02P10/20
Inventor 肖燕飞徐志峰廖家隆倪志聪万章豪
Owner JIANGXI UNIV OF SCI & TECH
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