Process for extracting rare-earth from sulfuric acid treating phosphorite process

A sulfuric acid treatment and rare earth technology, which is applied in the direction of improving process efficiency and can solve the problems of low extraction efficiency of rare earth and difficult recovery of rare earth

Active Publication Date: 2010-09-08
GRIREM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to recover valuable element rare earths from crude phosphoric acid prepared by wet phosphoric acid process, some people also proposed to use organic extractant to directly extract rare earths from crude phosphoric acid, such as using a mixed extractant of P204 and TBP to directly react with crude phosphoric acid, Let rare earth and uranium enter the extraction agent to form an extract, and then back extract to obtain rare earth. However, due to the high total concentration of phosphoric acid in the crude phosphoric acid system, the extraction efficiency of rare earth is low, which brings great difficulties to the recovery of rare earth.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 25%P 2 o 5 Crude phosphoric acid, containing 0.5g / L REO, is directly extracted by TBP (TBP and kerosene volume ratio 1:1), to obtain an organic phase and raffinate loaded with phosphoric acid, and the raffinate contains 10% P 2 o 5 and 0.5g / L REO.

[0024] Under the condition of 25°C, use 1.5M P204 (P204 and n-hexane volume ratio 1:1) to organically extract the raffinate acid, the extraction ratio is 1:1, countercurrent extraction is 20 stages, and the loaded rare earth organic phase and the secondary phase are obtained. raffinate. The rare earth-loaded organic phase was washed with 3M hydrochloric acid, the stripping ratio was O / A=1:10, and the rare earth chloride stripping liquid and blank organic phase were obtained through five stages of stripping. After adjusting the pH of the stripping solution to 3, add oxalic acid for precipitation according to 150% of the theoretical amount to obtain rare earth oxalate, which is calcined to obtain rare earth oxide. The yiel...

Embodiment 2

[0026] 30%P 2 o 5 Crude phosphoric acid, containing 0.15g / L REO, is directly extracted with a mixture of cyclohexanone and isopropyl ether to obtain an organic phase and raffinate loaded with phosphoric acid, and the raffinate contains 20% P 2 o 5 and 0.16g / L REO.

[0027] Under the condition of 30 ℃, use 1.5M P204 and TBP mixture (P204, TBP and kerosene volume ratio 0.8:0.2:1) to organically extract the raffinate acid, the extraction ratio is 1:1, countercurrent extraction is 18 stages, and the loaded Rare earth organic phase and secondary raffinate. The rare earth-loaded organic phase was washed with 3M hydrochloric acid, and the stripping ratio was O / A=20:1. After 20 stages of stripping, the rare earth chloride stripping solution and a blank organic phase were obtained. After adjusting the pH of the stripping solution to 2, potassium oxalate was added to precipitate according to 120% of the theoretical amount to obtain rare earth oxalate, which was calcined to obtain ra...

Embodiment 3

[0029] 35%P 2 o 5 Crude phosphoric acid, containing 1.8g / L REO, was directly extracted with a mixture of cyclohexanone, isopropyl ether and butanol to obtain an organic phase loaded with phosphoric acid and a raffinate containing 25% P 2 o 5 and 4.5g / L REO.

[0030] Under the condition of 40°C, use 2.0M (P204+P507) mixture (extractant and kerosene volume ratio 2:1) to organically extract the raffinate acid, the extraction ratio is 5:1, countercurrent extraction is 10 stages, and the loaded rare earth is obtained Organic phase and secondary raffinate. The rare earth-loaded organic phase was washed with 6M hydrochloric acid, and the stripping ratio was O / A=2:1. After 8 stages of stripping, the rare earth chloride stripping solution and a blank organic phase were obtained. After adjusting the pH of the stripping solution to 3, add ammonium oxalate for precipitation according to 150% of the theoretical amount to obtain rare earth oxalate, and calcinate to obtain rare earth oxi...

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PUM

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Abstract

The invention provides a process for extracting rare earth from a sulfuric acid treating phosphorite process. In the process, a sulfuric acid refining process and a rare earth extracting process are combined, and the rare earth is reclaimed from low-concentrate sulfuric acid raffinate generated in a crude phosphoric acid extracting and refining process so as to realize reclamation of a rare-earth element. The process comprises the following steps of: (1) extracting the rare-earth element from the raffinate by adopting acidic or neutral extractant to obtain rare earth loaded organic phase and secondary raffinate; (2) washing the rare earth loaded organic phase and performing back extracting on the rare earth-loading organic phase by using acid to obtain rare earth strip liquor and blank organic phase; and (3) precipitating the rare earth strip liquor to obtain solid rare earth salt after pH value of the obtained rare earth strip liquor is adjusted, and calcining the strip liquor to obtain rare earth oxide. The process has the advantages of realizing reclamation of the rare-earth element, relatively easily extracting the rare earth, along with high rare earth extraction yield.

Description

technical field [0001] The invention relates to a process for extracting rare earths from sulfuric acid treatment of phosphate rock, in particular to a process for refining phosphoric acid and extracting rare earths from wet process phosphoric acid containing rare earths, belonging to the technical field of wet process phosphoric acid and rare earth smelting. Background technique [0002] Phosphoric acid is a basic industrial raw material with a wide range of uses. The annual output of phosphoric acid in the world is about 40 million tons. The production methods of phosphoric acid are divided into wet method and thermal method. The wet method has been paid more and more attention because of its low energy consumption and low requirements on ore grade. [0003] At present, the treatment methods of wet-process phosphoric acid are mainly hydrochloric acid method, nitric acid method and sulfuric acid method. Among them, sulfuric acid method is the most widely used in China becau...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/26C22B3/32C22B3/08C22B59/00
CPCY02P10/20
Inventor 龙志奇王良士黄小卫李明来韩业斌彭新林罗兴华杨桂林崔大立
Owner GRIREM ADVANCED MATERIALS CO LTD
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