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Method for separating highly-pure rare-earth oxide from sulphating roasting rare earth mine

A rare earth oxide and rare earth ore technology, applied in the field of hydrometallurgy, can solve the problems of large equipment loss, difficult stripping, complicated operation, etc., achieve the effect of reducing the amount of slag, improving the recovery rate, and ensuring normal operation

Inactive Publication Date: 2007-08-08
YANGZHOU UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] ① Heavy rare earth element stripping acid concentration is high, especially scandium is difficult to strip completely;
[0020] ③In hydrochloric acid or sulfuric acid medium, the extraction rate of heavy rare earth ions is slow, and it takes a long time to reach extraction equilibrium, which will affect the improvement of productivity and economic benefits
[0021] (2) Problems with extraction equipment
[0024] (3) The connection between processes and the "three wastes" problem
This method not only consumes a lot of energy, a large amount of residual acid cannot be recovered, the operation is complicated, the equipment loss is large, and it pollutes the environment and produces new "three wastes".

Method used

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  • Method for separating highly-pure rare-earth oxide from sulphating roasting rare earth mine
  • Method for separating highly-pure rare-earth oxide from sulphating roasting rare earth mine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Main production equipment: stirring batching mixing tank, ultrasonic leaching equipment, ultrasonic extraction equipment, ionic membrane electrochemical reactor, stirring neutralization precipitation tank, ultrasonic crystallization tank, filtration solid-liquid separation device, pure water and pure acid equipment and analysis and testing Instruments etc.

[0064] Main raw materials: sulfuric acid, hydrochloric acid, liquid ammonia, ammonium bicarbonate, ammonium carbonate, P204 extraction agent, P507 extraction agent, sulfuric acid intensified roasting method to smelt rare earth ores.

[0065] The process steps are as follows:

[0066] (1) Ultrasonic leaching: In a 1L stirred tank, add water, weigh 45g of the concentrated sulfuric acid roasting material of rare earth ore (the content of mixed rare earth oxide is greater than 30%), and add it to the ultrasonic leaching device, using an ultrasonic frequency of 19.8kHz, 250W For the probe-type ultrasonic generator, add ...

Embodiment 2

[0081] The purified rare earth sulfuric acid solution is used as the feed liquid for the fractional distillation extraction of neodymium-samarium, the concentration of the rare earth is 45.38g / L, the acidity of the feed liquid is 0.06mol / L sulfuric acid, and the organic phase has a P204 content of 1.0mol / L No. 260 solvent oil solvent, the acidity of the lotion is 0.572mol / L sulfuric acid, 4 stages of extraction section, 7 stages of washing section, 11 stages in total, and the flow ratio of organic phase, feed liquid and lotion is 15 milliliters: 66 milliliters: 5.5 milliliters, the contact time between the organic phase and the aqueous phase is 6 minutes, the extraction temperature is 27°C, and the percentage of each rare earth element in the feed liquid is La 2 o 3 27.53, CeO 2 49.70, Pr 6 o 11 5.13, Nd 2 o 3 15.44, Sm 2 o 3 1.20, Eu 2 o 3 0.23, Gd 2 o 3 0.33,Y 2 o 3 0.20. The aqueous phase discharged from the outlet of the first-stage aqueous phase in th...

Embodiment 3

[0084] Its experimental condition is basically the same as embodiment 4, and the difference is that the concentration of rare earth in the feed liquid is 30.17g / L rare earth oxide, and the acidity of feed liquid is 0.05mol / L sulfuric acid; The flow ratio of organic phase, feed liquid and washing liquid is 15 ml: 99 ml: 5.5 ml, the extraction temperature was 23°C. The rare earth concentration in the aqueous phase discharged from the organic phase outlet was 27.89g / L rare earth oxide. The concentration of its free acid is 0.089mol / L sulfuric acid, and the rare earth concentration in the discharged organic phase from the organic phase is 3.92g / L rare earth oxide. The composition in the organic phase is Nd 2 o 3 2 o 3 51.23%, Eu 2 o 3 11.55%, the composition of the aqueous phase La 2 o 3 28.21%, CeO 2 50.80%, Pr 6 o 11 5.23%, Nd 2 o 3 16.35%, Sm 2 o 3 2 o 3The recovery rate of 100.12%, Nd 2 o 3 The recovery rate was 99%.

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Abstract

The invention discloses a full-separating method of high-purity rare earth oxide from rare earth rare earth ore reinforced and sintered by sulfuric acid, which is characterized by the following: producing La2O3, Ce2O3, Pr5O11, Nd2O3, Sm2O3, Eu2O3, Gd2O3, Tb4O7, Dy2O3 and Y2O3 through ultrasonic extracting-electrochemical quantivalence-changing synthetic separating technique; oxidizing Ce3+ into Ce4+; reducing Eu3+ into Eu2+ t oseparate from other tervalent rare earths.

Description

Technical field: [0001] The invention relates to the separation of rare earth ores strengthened by sulfuric acid roasting, and belongs to the field of hydrometallurgy. Background technique: [0002] Sulfuric acid roasting method to decompose rare earth ore is to mix rare earth ore (bastnaesite or a mixture of bastnaesite and monazite) with concentrated sulfuric acid and then roast continuously in a rotary kiln at a temperature of 300-800°C. Rare earth and Thorium and other elements generate soluble sulfate, fluorite is transformed into insoluble sulfur concentrated calcium and volatile gas hydrogen fluoride or silicon fluoride, iron, manganese and other minerals are also decomposed to varying degrees and transformed into sulfate. Rare earth ores can be directly leached with water after being roasted with sulfuric acid. The current industrial production method for leaching rare earths is to leaching the materials roasted with sulfuric acid with water. Since the water leachin...

Claims

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Application Information

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IPC IPC(8): C22B3/00C22B3/08C22B3/20C22B3/22C22B3/44C22B59/00C22B1/06
CPCY02P10/20
Inventor 许文林王雅琼魏晓廷朱金玉魏巍赵红坤
Owner YANGZHOU UNIV
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