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Technique for extracting and separating rare earth elements from non-saponification system

A rare earth element and non-saponification technology, which is applied in the field of extraction and separation of rare earth elements, can solve the problems of medium and heavy rare earth stripping difficulties, large investment in equipment extraction agents, high residual acid in stripping liquid, etc., and achieves cost-saving treatment of three wastes, easy control, and Effect of reducing acid consumption and cost

Active Publication Date: 2007-10-10
GRIREM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first and second methods have good separation effects and are widely used, but they must be saponified with ammonia water or ammonium bicarbonate, which will produce a large amount of ammonia nitrogen wastewater and cause great pollution to the environment.
The third method is the process adopted by France Rhodia and American Molybdenum Company. It is derived from the rare earth nitrate solution obtained when processing monazite ore to separate rare earth. The concentration of nitric acid in the extraction system of this process is high, so the production cost is high. stop state
The fourth process was invented by Beijing General Research Institute of Nonferrous Metals. It is applied to the extraction and separation of rare earth elements from the sulfuric acid rare earth solution obtained from the sulfuric acid roasting method to treat Baotou rare earth mines. The alkali consumption is less, but due to the low concentration of rare earth in the sulfuric acid system (<45g / L), the investment in the equipment extraction agent is large, and P204 has a strong extraction ability under acidic conditions. When the acidity of the feed liquid is low, it is easy to emulsify, and a certain amount of acid, while medium and heavy rare earth stripping is very difficult, the residual acid in the stripping liquid is high, and the acid consumption is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Bastnaesite and monazite mixed rare earth ore (REO 50%) undergoes sulfuric acid roasting, water immersion, neutralization and impurity removal to obtain a pure sulfuric acid rare earth solution with an acidity of pH 4 and main components of REO 40g / L, Fe 2 2 o 3 The content is less than 0.01%.

[0023] The obtained lanthanum cerium praseodymium neodymium raffinate (Sm 2 o 3 content is less than 0.005%), neutralized to PH4 with magnesium oxide, fully extracted with 1.5mol / l non-saponifiable P204, back-extracted with 5.5N hydrochloric acid, to obtain a rare earth chloride solution containing 267g / l of lanthanum, cerium, praseodymium and neodymium, which is produced by concentrated crystallization Rare earth chloride products of lanthanum cerium praseodymium neodymium, of which REO>45%, Sm 2 o 3 The content is less than 0.005%. From the sulfuric acid rare earth solution to the product, the total rare earth yield is 98.2%.

Embodiment 2

[0025]Bastnaesite (REO 60%) undergoes sulfuric acid roasting, water immersion, neutralization and impurity removal to obtain a pure rare earth sulfate solution with an acidity of pH 4.5 and a rare earth concentration of REO 36g / L. Carry out Nd / Sm extraction and grouping, use 10-stage extraction, 18-stage washing, and 9-stage back-extraction. The washing solution is a rare earth chloride solution containing 255g / l of samarium, europium, and gadolinium, and an acidity of 0.3N. The rare earth-loaded organic phase contains 12g / l of rare earth , back-extracted with 5.2N hydrochloric acid to obtain a samarium-europium-gadolinium rare-earth chloride solution containing REO 255g / l and an acidity of 0.3N. After precipitation and oxalic acid precipitation, burning produces samarium-europium-gadolinium enrichment or further extraction and separation of samarium, europium, and europium. Gadolinium single rare earth products.

[0026] The obtained raffinate containing lanthanum, cerium, pr...

Embodiment 3

[0028] Front part process is the same as embodiment 2

[0029] The obtained lanthanum, cerium, praseodymium and neodymium raffinate is neutralized to pH4 with magnesium oxide, then adopts the mixed extractant of 90% 1.5mol / L non-saponification P204 and 10% 1.5mol / L non-saponification C272 (with No. diluted with solvent naphtha) for cerium / praseodymium fractionation extraction grouping. The lotion is stripped with rare earth chloride containing praseodymium and neodymium (REO 258g / L), and the loaded rare earth organic phase is stripped with 6.0N hydrochloric acid; after 23 stages of extraction, 32 stages of washing, and 6 stages of stripping to obtain praseodymium and neodymium chloride (CeO 2 The content is less than 0.05%); the raffinate is neutralized to PH4.5 with magnesium oxide, lanthanum cerium is extracted with 1.5mol / L unsaponified P204, back-extracted with 5.3N hydrochloric acid, and the obtained lanthanum cerium chloride solution is concentrated and crystallized to p...

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Abstract

This invention provides a process for extracting and separating rare earth elements by using non-saponification extractant. The process comprises: utilizing rare earth sulfate solution containing two or more rare earth elements obtained by treating rare earth ore as the raw material, performing Nd / Sm multi-stage fractionation and extraction by using non-saponification extractant P507 to obtain Sm / Eu / Gd enriched product and La / Ce / Pr / Nd extraction raffinate, and further extracting and separating rare earth compounds with non-saponification extractant. The process has such advantages as no emulsification under low-acidity extraction, easy back extraction of medium-molecular-weight rare earth elements, low acid consumption, and high productivity.

Description

technical field [0001] The invention relates to a process for extracting and separating rare earth elements. Specifically, the rare earth sulfate solution containing at least two rare earth elements obtained from the treatment of rare earth ores is used as a raw material, and non-saponified P507 is used for neodymium / samarium extraction grouping to obtain samarium europium gadolinium enrichment and lanthanum cerium praseodymium neodymium raffinate. Then use non-saponifiable P204 or non-saponifiable P204 and non-saponifiable P507, C272, C301, C302, HEOPPA, P350, TBP one or two of the mixed extraction agent prepared in the lanthanum cerium praseodymium neodymium sulfate and chloride A process for extracting and separating rare earth elements from a mixed solution of rare earth or rare earth nitrate. Background technique [0002] Lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lut...

Claims

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Application Information

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IPC IPC(8): C22B3/26C22B59/00C22B3/08C22B3/06C22B3/20
CPCY02P10/20
Inventor 龙志奇黄小卫彭新林李建宁朱兆武赵娜崔大立张顺利
Owner GRIREM ADVANCED MATERIALS CO LTD
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