A method for recovering rare earth from rare earth-containing wastewater

A rare earth and wastewater technology, applied in the direction of improving process efficiency, can solve the problems of poor thermal stability of catalytic cracking catalyst, high investment cost, high organic content, and achieve obvious economic and environmental protection benefits, simple recovery process, The effect of high rare earth recovery rate

Active Publication Date: 2017-06-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Domestic catalyst factories generally use the ammonia precipitation method to recover rare earths in the filtrate, but the concentration of the rare earth solution recovered by this method is low, the content of impurities is high, the exchange rate of rare earths is low when the rare earths are reused, and the thermal stability of the catalytic cracking catalyst obtained is deteriorated. When using catalysts, the ratio of the added amount of recovered rare earths to the amount of fresh rare earths needs to be less than 15%. Compared with the ammonia water method, the recovery of rare earths in the filtrate by the extraction method has the advantages of high recovery rate, good quality, simple recovery process, less pollution, and low production costs. Low advantages, but the extraction method has defects such as high investment cost and high content of organic matter in the generated wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Take 300g of rare earth-containing molecular sieve production wastewater (among them, RECl 3 The content is 0.1212g, wherein the rare earth metal elements, La accounts for 43% by weight, Ce accounts for 57% by weight) and 0.1213g of NaHCO 3 with Na 2 CO 3 mixture (Na 2 CO 3 with NaHCO 3 The weight ratio is 1:1), the reaction is carried out at a pH value of 7.5 and normal temperature (20°C), the reaction time is 20 minutes, solid-liquid separation is carried out after sedimentation for 120 minutes, and the rare earth precipitate and the first solution are obtained;

[0039](2) Add the obtained rare earth precipitate to 500g of a mixed aqueous solution of hydrofluoric acid HF and HCl (the weight ratio of HF and HCl is 4.4:1), and the molar ratio of hydrofluoric acid to rare earth metal elements is 1:0.25, The pH value of the solution is 2.5, react for 20 minutes, and settle for 120 minutes to separate the solid and liquid to obtain the rare earth fluoride and the...

Embodiment 2

[0042] (1) Take 500g of rare earth-containing molecular sieve production wastewater (among them, RECl 3 The content is 0.1868g, wherein the rare earth metal elements, La accounts for 43% by weight, Ce accounts for 57% by weight) and 0.2413g of NaHCO 3 with Na 2 CO 3 mixture (Na 2 CO 3 with NaHCO 3 The weight ratio is 1:2), the reaction is carried out at pH 8.5 and normal temperature (20°C), the reaction time is 30 minutes, the solid-liquid separation is carried out after 180 minutes of sedimentation, and the rare earth precipitate and the first solution are obtained;

[0043] (2) Add the obtained rare earth precipitate to 300g of a mixed aqueous solution of hydrofluoric acid HF and HCl (the weight ratio of HF and HCl is 1.6:1), and the molar ratio of hydrofluoric acid to rare earth metal elements is 1:0.2, The pH value of the solution is 2, react for 30 minutes, and settle for 180 minutes to separate the solid and liquid to obtain the rare earth fluoride and the second so...

Embodiment 3

[0046] (1) Take 400g of rare earth-containing molecular sieve production wastewater (among them, RECl 3 The content is 0.1348g, wherein the rare earth metal elements, La accounts for 43% by weight, Ce accounts for 57% by weight) and 0.1863g of NaHCO 3 with Na 2 CO 3 mixture (Na 2 CO 3 with NaHCO 3 The weight ratio is 1:3), the reaction is carried out at a pH value of 8 and normal temperature (20°C), the reaction time is 10 minutes, solid-liquid separation is carried out after 30 minutes of sedimentation, and the rare earth precipitate and the first solution are obtained;

[0047] (2) Add the obtained rare earth precipitate to 1000g of a mixed aqueous solution of hydrofluoric acid HF and HCl (the weight ratio of HF and HCl is 2.7:1), and the molar ratio of hydrofluoric acid to rare earth metal elements is 1:0.1, The pH value of the solution is 2.7, react for 10 minutes, and settle for 30 minutes to separate the solid and liquid to obtain the rare earth fluoride and the sec...

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PUM

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Abstract

The invention provides a method for recovering rare earth from rare earth-containing wastewater. The method comprises the following steps: 1, allowing the rare earth-containing wastewater to contact with an alkaline precipitating agent capable of precipitating rare earth metal elements, and carrying out solid-liquid separation after settlement to obtain a first solution and a rare earth precipitate; and 2, allowing the rare earth precipitate to contact with an aqueous solution containing hydrofluoric acid, and carrying out solid-liquid separation after settlement to obtain a second solution and rare earth fluoride. The method allows the rare earth metal elements to be effectively recovered, the recovery rate of the rare earth metal elements to be high and rare earth and fluoride in a raffinate obtained after recovery to reach environmental protection standard requirements, and the final raffinate subjected to an acid-base neutralization reaction is basically neutral and basically has no pollution to environment; and the rare earth fluoride obtained after recovery through the method is purified rare earth, can be used for molecular sieve modification, and can also be used in production of arc carbon rods and special steel alloys as an additive.

Description

technical field [0001] The invention belongs to the field of recovery and treatment of valuable metals, and in particular relates to a method for recovering rare earths from rare earth-containing wastewater produced in the production process of catalytic cracking catalysts. Background technique [0002] In the molecular sieve production process, it is processed by adding rare earth chloride (mainly composed of chlorides containing rare earth metal elements such as La, Ce, Pr, Nd and Sm, among which the content of rare earth metal elements La+Ce exceeds 80%) Modification, therefore, the molecular sieve production wastewater contains a large amount of pollutants, and its main discharge point is the wastewater discharged from the gelation of the molecular sieve production process and the filtration process of the washing unit. Among them, the main pollutant is suspended solids; and the direct discharge of wastewater Not only pollute the environment, but also cause the loss of r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B59/00
CPCY02P10/20
Inventor 崔龙鹏高峰桑军强马欣
Owner CHINA PETROLEUM & CHEM CORP
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