Preparation of rare earth chloride from long-chain fatty acid extracting transformation and back-extraction process thereof

A long-chain fatty acid, rare earth chloride technology, applied in the direction of improving process efficiency, can solve problems such as difficult degradation, pollute the environment, and process discontinuity, and achieve the effects of less consumption of chemical reagents, reduced environmental pollution, and simple process flow

Inactive Publication Date: 2003-11-12
BAOTOU RES INST OF RARE EARTHS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The annual production capacity of Baotou rare earth concentrate is 80,000 tons. At present, the rare earth industry mainly adopts the high-temperature roasting and decomposition process of concentrated sulfuric acid. The roasted ore is leached with water to obtain a leaching solution containing rare earth and impurities such as iron and calcium. Magnesium oxide is used to adjust the pH to 3-4 to remove iron, etc. Rare earth sulfate solution is obtained after impurity. There are two follow-up processes in the industry to prepare rare earth chloride for the rare earth sulfate solution. The first process is to precipitate with ammonium bicarbonate, and obtain rare earth carbonate products through centrifugation, and then use it as needed. The rare earth chloride solution obtained by dissolving hydrochloric acid is used to separate a single rare earth product. The intermittent operation of this process is discontinuous. The high sulfate content in the rare earth carbonate is not conducive to subsequent separation operations, and produces acidic wastewater containing a large amount of ammonium salts to pollute the environment. The second The process is to use P204 extraction and back extraction with hydrochloric acid to prepare rare earth chloride solution. On the one hand, this process requires high acidity of stripping to strip rare earth and a small amount of iron. The obtained rare earth chloride solution has high acidity and cannot be directly used for subsequent separation. The feed liquid of a single rare earth needs to be adjusted in acidity, and the process is discontinuous. After a period of production and operation, the iron in the extractant accumulates, which reduces the extraction capacity of the organic phase. On the other hand, P204 is an acidic phosphate lipid extractant. It is not easy to degrade, has certain toxicity, and produces a large amount of waste water containing organic phosphorus to pollute the environment, and the process flow is discontinuous

Method used

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  • Preparation of rare earth chloride from long-chain fatty acid extracting transformation and back-extraction process thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Example 1: A rare earth enterprise in Baotou concentrated sulfuric acid high-temperature roasting water immersion solution, rare earth sulfate solution after removing impurities by magnesium oxide, that is, the feed liquid used for carbon precipitation in the original process, rare earth concentration 38g / l, acidity PH4, organic phase composition It is fatty acid 1.0M-isooctanol 15% V / V-sulfonated kerosene, concentrated ammonia water saponification, saponification degree is 0.4M, 3-stage extraction, 2-stage washing, 5-stage stripping, organic phase: feed liquid: washing liquid: Stripping liquid 1: the flow ratio of stripping liquid 2 is 3: 1: 0.5: 0.18: 0.06, the rare earth chloride solution concentration that obtains is 205g / l, and acidity is PH1, and sulfate radical content is less than 0.02%, and rare earth yield is greater than 99%.

Embodiment 2

[0013] Example 2: A rare earth enterprise in Baotou concentrated sulfuric acid high-temperature roasting water immersion solution, rare earth sulfate solution after removing impurities by magnesium oxide, that is, the feed liquid used in the original process for P204 extraction transformation, rare earth concentration 36g / l, acidity PH2, other conditions Same as Example 1, the concentration of the obtained rare earth chloride solution is 203g / l, the acidity is PH1, the sulfate content is less than 0.02%, and the rare earth yield is greater than 99%.

Embodiment 3

[0014] Embodiment 3: The feed liquid is the same as in Example 1, the organic phase is composed of fatty acid 0.85M-isooctanol 15% V / V-sulfonated kerosene, saponified with concentrated ammonia water, and the degree of saponification is 0.4M. 3-stage extraction, 2-stage washing, 5-stage back-extraction, the flow ratio of organic phase: feed liquid: washing liquid: stripping liquid 1: stripping liquid 2 is 4: 1: 1: 0.18: 0.04, and the obtained rare earth chloride The solution concentration is 184g / l, the acidity is PH2, the sulfate radical content is less than 0.02%, and the rare earth yield is greater than 99%.

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Abstract

The present invention uses rare earth sulfate obtained by using sulfuric acid to roast immersion liquor magnesia to regulate pH value to 3-4 and removing iron and impurity as raw material, and uses long-chain fatty acid, cosolvent and sulfonated kerosene to form orgnaic phase, the long-chain fatty acid is dehydrated on non-dehydrated ricinus oil fatty acid, and uses ammonia water, sodium hydroxide, ammonium hydrogen carbonate or sodium carbonate to make saponficiation, and adopts multi-stage extraction and washing processes to obtain the invented rare earth chloride solution whose concentration is greater than 200 g / l, acidity pH is 1-2 and sulfuric acid radical is less than 0.02%, and the rare earth yield is greater than 99%.

Description

1. Technical field: [0001] The invention belongs to the processing field of metallurgical rare earth metals, and in particular relates to a long-chain fatty acid extraction transformation to prepare rare earth chloride and its stripping process. 2. Background technology: [0002] The annual production capacity of Baotou rare earth concentrate is 80,000 tons. At present, the rare earth industry mainly adopts the high-temperature roasting and decomposition process of concentrated sulfuric acid. The roasted ore is leached with water to obtain a leaching solution containing rare earth and impurities such as iron and calcium. Magnesium oxide is used to adjust the pH to 3-4 to remove iron, etc. Rare earth sulfate solution is obtained after impurity. There are two follow-up processes in the industry to prepare rare earth chloride for the rare earth sulfate solution. The first process is to precipitate with ammonium bicarbonate, and obtain rare earth carbonate products through centri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/32
CPCY02P10/20
Inventor 许延辉马鹏起张希霞武国琴
Owner BAOTOU RES INST OF RARE EARTHS
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