Method for extracting rare earth from rare earth-containing sludge

A rare earth and sludge technology, applied in the direction of improving process efficiency, etc., can solve problems such as limiting the scope of application, and achieve the effects of increasing extraction rate, low operating cost, and increasing recovery rate of rare earth

Active Publication Date: 2015-09-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN101481161A discloses a method for producing rare earth aluminum iron polysilicon sulfate with rare earth sludge and iron dust sludge, but it only involves the production of rare earth aluminum iron polysilicon sulfate by rare earth sludge and iron dust sludge, not directly Extraction of valuable rare earths or their compounds limits their scope of application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Take the high ammonia nitrogen wastewater containing rare earth sludge (containing La 2 o 3 3.9 wt%, CeO 2 6.4% by weight) mixed with a mixed acid solution containing hydrogen chloride and oxalic acid at a concentration of 2mol / L (the weight ratio of hydrogen chloride and oxalic acid is 1:0.2) at a weight ratio of 1:10, and the contact temperature is 40°C, and the pH value is 2 , the stirring rate is 300r / min, the leaching time is 20min, the leaching rates of La and Ce are 95% and 100% respectively, and the leaching solution containing rare earth elements is obtained, and the leaching solution containing rare earth elements is evaporated and concentrated to make the rare earth elements The concentration reaches 1.2mol / L, then add ammonia water to adjust its pH value to 8;

[0044] (2) Mix the organic extractant (the organic extractant is a mixture of bis(2-ethyl-hexyl phosphate), naphthenic acid and dibutyl sulfoxide, the mass ratio of the three is 4:3:1) with ker...

Embodiment 2

[0047] (1) Take the high ammonia nitrogen wastewater containing rare earth sludge (containing La 2 o 3 5.7 wt%, CeO 2 6.3% by weight) mixed with a mixed acid solution containing hydrogen chloride and oxalic acid at a concentration of 2.5mol / L (the weight ratio of hydrogen chloride and oxalic acid is 1:0.8) at a weight ratio of 1:10, and the contact temperature is 60°C, and the pH value is 3. The stirring rate is 500r / min, the leaching time is 30min, the leaching rates of La and Ce are 96% and 98% respectively, and the leaching solution containing rare earth elements is obtained, and the leaching solution containing rare earth elements is evaporated and concentrated to make the rare earth metals The concentration of the element reaches 1mol / L, then add ammonia water to adjust the pH value to 9;

[0048] (2) Mix the organic extractant (the organic extractant is a mixture of bis(2-ethyl-hexyl phosphate), naphthenic acid and dibutyl sulfoxide, the mass ratio of the three is 5:2:...

Embodiment 3

[0051] The rare earth is recovered according to the method of Example 1, the difference is that in the step (1), the hydrogen chloride solution (with constant concentration) is used for leaching, the leaching temperature is 100°C, and the leaching rates of La and Ce are respectively 95%. and 96%;

[0052] At the same time, the extractant in step (2) The organic extractant is a mixture of bis(2-ethyl-hexyl phosphate), naphthenic acid and dibutyl sulfoxide, the mass ratio of the three is 6:1:1, and La extracts The extraction rate was 92%, and the Ce extraction rate was 65%.

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Abstract

The invention provides a method for extracting rare earth from rare earth-containing sludge. The method comprises the following steps: 1, allowing the rare earth-containing sludge to contact with an acidic aqueous solution in order to leach the rare earth-containing sludge, and separating to obtain a rare earth element-containing leachate; and 2, allowing the leachate to contact with an organic solvent containing an extraction agent, and extracting to obtain a raffinate water phase and a rare earth element-containing extraction organic phase, wherein the extraction agent is a phosphorus-to-oxygen double bond-containing phosphorus-containing extraction agent, carboxylic acid extraction agent and sulfur-to-oxygen double bond-containing sulfur-containing extraction agent mixture. The method allows rare earth to be leached and extracted from the rare earth-containing sludge in a high yield mode and rare earth chloride to be prepared, the recovered rare earth chloride can be used for producing catalysts, and the method has the advantages of simple whole process, environmental protection, low energy consumption, less production device investment and low operating cost.

Description

technical field [0001] The invention belongs to the technical field of secondary resource utilization of rare earth-containing sludge, and more specifically relates to a method for extracting rare earth from rare earth-containing sludge produced in the production process of a catalytic cracking catalyst. Background technique [0002] my country's petrochemical industry has been producing and using rare earth molecular sieve catalysts since the mid-1970s. With the increase of crude oil processing and the expansion of catalytic cracking production capacity, the consumption of cracking catalysts is increasing. Sinopec is a major manufacturer of catalytic cracking catalysts. During the "Twelfth Five-Year Plan" period, the annual output reached more than 200,000 tons. At present, Sinopec uses rare earth chloride as the rare earth raw material for catalyst production. [0003] In catalyst production enterprises, in order to meet the national environmental protection requirements...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B59/00
CPCY02P10/20
Inventor 崔龙鹏张然高峰张超
Owner CHINA PETROLEUM & CHEM CORP
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