Method for recovering rhodium from homogeneous waste catalyst containing rhodium

A technology of waste catalyst and catalyst amount, applied in the direction of improving process efficiency, can solve the problems of low overall recovery rate, serious environmental pollution, low rhodium content concentration, etc., and achieve the effect of improving recovery rate, reducing dispersion and easy handling

Active Publication Date: 2020-11-27
XUZHOU GUOMAO VALUABLE & RARE METAL COMPREHENSIVE UTILIZATION INST
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, because the rhodium content concentration in the homogeneous catalyst is low, the binding ability of metal rhodium and the organic phosphine compound is very strong, the multinuclear rhodium complex is stable and the waste rhodium solution is very viscous, etc., the final recovery rate is not high, only to 85% %about
[0005] The adsorption separation method is to add a selective adsorbent to the homogeneous waste catalyst to adsorb the rhodium-phosphine complex catalyst, and then use benzene as a solvent to thoroughly wash off the high-boiling point by-products in the catalyst, and then analyze and purify the purified rhodium. The recovery rate can reach 90%, adopt this method to use a large amount of organic solvents in the recovery process, the pollution to the environment is serious, and the overall recovery rate of rhodium is not high

Method used

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  • Method for recovering rhodium from homogeneous waste catalyst containing rhodium

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Effect test

Embodiment 1

[0028] A method for recovering rhodium from a homogeneous waste catalyst containing rhodium, such as figure 1 As shown, the method includes the following steps:

[0029] Step 1: Take a certain amount of spent catalyst, and at room temperature, first add 5% hydrochloric acid with the amount of spent catalyst to the spent catalyst, and then add 3% hydrogen peroxide with the amount of spent catalyst, heat to 90°C, and keep warm and stir to react 2h;

[0030] Step 2: After step 1 is completed, add a mixed solution of 4% oxalic acid and 3% formic acid with the amount of spent catalyst, continue to keep the temperature and stir for 2.5 hours, and then cool and filter after the completion of the temperature.

[0031] Step 3: Heat the filtrate obtained from step 2 with stirring to 90°C, and add 10% Na with a mass fraction dropwise 2 S solution, add Na 2 The amount of S is 2% of the amount of spent catalyst, keep it for 3 hours, and then cool and filter after keeping it warm;

[0032] 2Rh 3+ +...

Embodiment 2

[0039] A method for recovering rhodium from a homogeneous waste catalyst containing rhodium, such as figure 1 As shown, the method includes the following steps:

[0040] Step 1: Take a certain amount of spent catalyst, at room temperature, first add 20% sulfuric acid of the spent catalyst, and then add 30% hydrogen peroxide of the spent catalyst to the spent catalyst, heat to 70°C, and keep warm and stir to react 0.5h;

[0041] Step 2: Step 1 is finished with heat preservation, then add the mixed solution of 25% oxalic acid and 18% formic acid with the amount of spent catalyst, continue to keep the temperature and stirring reaction for 1h, and then cool and filter after the completion of keeping warm;

[0042] Step 3: The filtrate obtained by filtering in step 2 is heated to 60℃ with stirring, and 30% Na with a mass fraction is added dropwise 2 S solution, add Na 2 The amount of S is 15% of the amount of spent catalyst, keep it for 1 hour, and then cool and filter after keeping it wa...

Embodiment 3

[0047] A method for recovering rhodium from a homogeneous waste catalyst containing rhodium, such as figure 1 As shown, the method includes the following steps:

[0048] Step 1: Take a certain amount of spent catalyst. At room temperature, first add 15% hydrochloric acid with the amount of spent catalyst to the spent catalyst, and then add 16% sodium chlorate with the amount of spent catalyst, heat to 80°C, and heat to react with stirring. 1h;

[0049] Step 2: After step 1 is completed, add a mixed solution of 15% oxalic acid and 10% formic acid with the amount of spent catalyst, continue the temperature keeping and stirring reaction for 2 hours, and then cool and filter after the completion of the keeping warm;

[0050] Step 3: The filtrate obtained by filtering in step 2 is heated to 75°C with stirring, and 20% Na is added dropwise. 2 S solution, add Na 2 The amount of S is 9% of the amount of spent catalyst, keep it for 2h, cool and filter after keeping it warm;

[0051] Step 4: Co...

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Abstract

The invention discloses a method for recovering rhodium from a homogeneous waste catalyst containing rhodium. The method of acidification oxidation-complex precipitation-sulfide precipitation is adopted. Firstly acidification-oxidation is adopted to interrupt the 'bridging' of rhodium in rhodium-phosphine catalyst in the waste catalyst, and then a specific complexing precipitant is adopted to generate a complex precipitate of rhodium, so that the recovery rate of rhodium reaches 95.23% in one step, the main body of rhodium in the waste catalyst is recovered in one step, the dispersion of the rhodium is effectively reduced, and the recovery rate of the rhodium is improved; and in addition, in the acidification-oxidation process step, a small part of rhodium is directly oxidized into Rh3+, the part is recovered by a vulcanization precipitation method, and the final recovery rate of the rhodium can reach more than 97% by combination of the two kinds of recovery. The complex precipitate and the sulfide precipitate generated in the recovery process are easy to treat, toxic substances are not generated, and the method is safe, green and environmentally friendly.

Description

Technical field [0001] The invention belongs to the technical field of comprehensive utilization of precious metal secondary resources, relates to the recovery of precious metal rhodium, and in particular relates to a method for recovering rhodium from a homogeneous waste catalyst containing rhodium. Background technique [0002] Rhodium homogeneous organic complex catalyst has the advantages of high catalytic activity and good selectivity. It plays an important role in the chemical process of catalytic hydrogenation, hydroformylation, oxo synthesis and so on. However, in the process of industrial application, it was discovered that when the homogeneous rhodium catalyst was used for a period of time, various high-boiling by-products and impurities in the raw materials deactivated part of the catalyst. The deactivated homogeneous rhodium catalyst contains 100-800ppm rhodium, which is much higher than the content in the earth's crust, and is an important secondary rhodium resource....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B11/00C22B7/00
CPCC22B7/007C22B11/048Y02P10/20
Inventor 张邦胜姜东刘贵清廖秋玲张帆解雪王芳曲志平龚卫星张保明刘昱辰吴祖璇
Owner XUZHOU GUOMAO VALUABLE & RARE METAL COMPREHENSIVE UTILIZATION INST
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