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A method for precipitation and separation of rare earth in calcium-containing rare earth solution

A rare earth solution, precipitation separation technology, applied in the field of precipitation and separation of rare earth and calcium, can solve the problems of instability, inability to achieve calcium rare earth separation, difficult to convert calcium carbonate into calcium bicarbonate, etc., and achieve the effect of efficient separation

Active Publication Date: 2022-05-17
GANZHOU ZHANHAI IND & TRADING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can play a catalytic role in the presence of rare earths. It is difficult to convert calcium carbonate into calcium bicarbonate through carbon dioxide carbonization, and the solubility of calcium bicarbonate is not high and unstable. If there is a large amount of calcium carbonate, it cannot be well realized. Separation of calcium rare earth

Method used

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  • A method for precipitation and separation of rare earth in calcium-containing rare earth solution
  • A method for precipitation and separation of rare earth in calcium-containing rare earth solution
  • A method for precipitation and separation of rare earth in calcium-containing rare earth solution

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Experimental program
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Effect test

Embodiment 1

[0042] First, add bottom water and cerium carbonate seed crystals to the reaction kettle, and then add a calcium-containing rare earth solution with a cerium ion concentration of 0.3 mol / L and a calcium ion concentration of 0.30 mol / L and a sodium bicarbonate solution of 0.30 mol / L in parallel Carry out the precipitation reaction, control the reaction temperature to 25°C, control the feeding rate of the calcium-containing rare earth solution to 2.0ml / min, adjust the feeding rate of the sodium bicarbonate solution to control the pH of the reaction process to be 4.6, filter and wash after the reaction to obtain crystalline carbonic acid Cerium precipitate and filtrate; crystalline cerium carbonate phase as image 3 As shown in XRD, it can be seen that it is cerium carbonate hexahydrate with high purity and good crystallinity. The cerium carbonate precipitate was calcined at 900°C for 3 hours to obtain ceria with a purity of 99.0%.

Embodiment 2

[0044] First add the bottom water in the reactor, and then add the calcium-containing rare earth solution and the sodium bicarbonate solution of 0.30 mol / L with the cerium ion concentration of 0.3mol / L and the calcium ion concentration of 0.30mol / L in parallel to carry out the precipitation reaction. The reaction temperature is 25°C, the feeding rate of the calcium-containing rare earth solution is controlled to be 2.0ml / min, the pH of the reaction process is controlled to be 4.6 by adjusting the feeding rate of the sodium bicarbonate solution, and the crystalline cerium carbonate precipitate and filtrate are obtained by filtering and washing after the reaction , The cerium carbonate precipitate was calcined at 900°C for 3h to obtain ceria with a purity of 98.2%.

Embodiment 3

[0046] First, add bottom water and cerium carbonate seed crystals to the reaction kettle, and then add a calcium-containing rare earth solution with a cerium ion concentration of 1.2 mol / L and a calcium ion concentration of 0.20 mol / L and a sodium bicarbonate solution of 0.80 mol / L in parallel Carry out the precipitation reaction, control the reaction temperature to 40°C, control the feeding rate of the calcium-containing rare earth solution to 7.0ml / min, adjust the feeding rate of the sodium bicarbonate solution to control the pH of the reaction process to be 5.1, filter and wash after the reaction to obtain the crystal form Cerium carbonate precipitate and filtrate, the cerium carbonate precipitate was calcined at 900°C for 3 hours to obtain cerium oxide with a purity of 99.2%. The physical properties of cerium oxide are as follows: Figure 4 As shown, it is a pure ceria phase with no miscellaneous peaks and high purity.

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Abstract

The invention discloses a method for precipitating and separating rare earths in a calcium-containing rare earth solution. Specifically, the concentration of rare earths is 0.1-1.5 mol / L, the concentration of calcium ions is 0.1-1.0 mol / L, and the molar ratio of rare earths to calcium is 0.7≤ The calcium-containing rare earth solution with X≤8.0 is the object, and the rare earth in the calcium-containing rare earth solution is precipitated by bicarbonate, and the conditions such as temperature, pH, and feeding speed during the precipitation process are adjusted and controlled according to the molar ratio of rare earth and calcium in the solution, so that Adjust the concentration of bicarbonate in the solution to control the stability of calcium bicarbonate and the supersaturation of rare earth carbonate, so that rare earth ions precipitate to form crystalline rare earth carbonate, and calcium ions form soluble calcium bicarbonate, so as to realize calcium-containing rare earth solution High-efficiency separation of medium rare earth and calcium, and rare earth oxides with a purity greater than 98%.

Description

technical field [0001] The invention relates to the field of rare earth hydrometallurgy, in particular to a method for separating rare earth and calcium by precipitation. Background technique [0002] Due to their unique physical and chemical properties, the compounds formed by rare earth elements have very rich magnetic, optical, electrical, catalytic and other functional properties, and are known as "vitamins of modern industry" and "treasure house of new materials". In the process of rare earth hydrometallurgy, the separation of rare earth and calcium is often encountered; for example, the rare earth concentration in the lanthanum-calcium or lanthanum-cerium-calcium feed solution produced by the rare earth extraction and separation workshop using the calcium saponification process is generally 0.5-1.5mol / L, the calcium ion concentration is 10g / L-40g / L; the rare earth concentration in the leaching solution of bastnaesite concentrate is 0.1-0.7mol / L, and the calcium ion co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B59/00C22B3/44
CPCC22B59/00C22B3/44Y02P10/20
Inventor 祝文才任卫熊伟高亮赖启飞肖燕飞罗威祝寅鸣林英金霞饶明璐贺强邱江赖安邦
Owner GANZHOU ZHANHAI IND & TRADING
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