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Method for removing iron in noble metal rhodium recovery process

A precious metal, ferric chloride technology, applied in the direction of improving process efficiency, can solve the problems of complex analysis process, reducing the recovery rate of precious metal rhodium, difficult recovery and purification of precious metal rhodium, etc., and achieves high purity, high recovery rate and simple process. Effect

Active Publication Date: 2020-02-07
LUXI CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the use of the catalyst, due to factors such as equipment pipeline corrosion and raw material entrainment, some iron ions will inevitably be brought in, causing difficulties in the recovery and purification of precious metal rhodium.
At present, the resin adsorption method is generally used in the rhodium compound iron removal process in China, but because the resin also has a certain adsorption capacity for the rhodium compound, the recovery rate of the precious metal rhodium is reduced. At the same time, the repeated adsorption and analysis process of the resin is relatively complicated, and a large amount of Waste acid wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] concentrating and incinerating the recovered triphenylphosphine acetylacetonate rhodium carbonyl catalyst waste solution to obtain a mixture; chlorinating the mixture to obtain a mixture of rhodium chloride and ferric chloride. The rhodium chloride mixture containing a certain amount of ferric chloride after taking 20.9g of chlorination (simultaneously as sample No. 0 sample) is dissolved in 100ml mass concentration 1% hydrochloric acid solution, adds 36.3g sodium chloride, at 50 ℃ of conditions Stir to dissolve completely. After removing the insoluble matter by suction filtration, the filtrate was decompressed to remove most of the liquid, and then dried in an oven at 110°C to obtain a rose-red solid. The obtained solid was ground into powder and then transferred to 200ml of absolute ethanol, stirred and dissolved at 50°C for 1 hour, and then suction-filtered. The recovered sodium chlororhodium acid sample 1 was obtained, and the sample 1 was ground into powder again,...

Embodiment 2

[0033] Weigh 20.9g of the rhodium chloride mixture containing a certain amount of ferric chloride prepared in Example 1 and dissolve it in 100ml of 1% hydrochloric acid solution, add 36.3g of sodium chloride, stir and fully dissolve at 50°C. After removing the insoluble matter by suction filtration, the filtrate was decompressed to remove most of the liquid, and then dried in an oven at 110°C to obtain a rose-red solid. The obtained solid was ground into powder and then transferred to 200ml of absolute ethanol, stirred and dissolved at 50°C for 1 hour, and then suction-filtered. To obtain the recovered sodium chlororhodium acid sample, transfer the dried sodium chlororhodium acid to a reduction furnace, replace it with nitrogen, and heat up to 600°C and pass in hydrogen for 30 minutes to obtain elemental rhodium. The recovery rate of rhodium is 99.0-99.5%, and the purity is 99.92%. %.

Embodiment 3

[0035] Weigh 20.9g of the rhodium chloride mixture containing a certain amount of ferric chloride prepared in Example 1 and dissolve it in 100ml of 1.2% hydrochloric acid solution, add 37.3g of sodium chloride, stir and fully dissolve at 50°C. After removing the insoluble matter by suction filtration, the filtrate was decompressed to remove most of the liquid, and then dried in an oven at 110°C to obtain a rose-red solid. The obtained solid was ground into powder and transferred to 200ml of absolute ethanol, stirred and dissolved at 40°C for 1.5h, and then suction filtered; this washing step was repeated twice. To obtain the recovered rhodium chlororhodium sample, transfer the dried rhodium chlororhodium to the reduction furnace, replace it with nitrogen, heat up to 620°C, and pass in hydrogen for 30 minutes to obtain elemental rhodium. The recovery rate of rhodium is 98.7-99.3%, and the purity is 99.93%. %.

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Abstract

The invention discloses a method for removing iron in a noble metal rhodium recovery process. The method comprises the steps of concentrating and incinerating a recovered waste solution of a triphenylphosphine acetylacetone carbonyl rhodium catalyst to obtain a solid rhodium and iron oxide mixture; chlorinating the mixture to obtain a mixture of rhodium chloride and iron chloride; adding chloridesalt and a hydrochloric acid solution into the mixture of rhodium chloride and iron chloride, and evaporating the mixture to dryness after reaction to obtain a mixture of chlorine rhodate and iron chloride; washing the mixture of chlorine rhodate and iron chloride with a polar organic solvent to remove iron chloride; and preparing residual chlorine rhodate into metal rhodium or rhodium chloride; and concentrating and incinerating the waste solution of the triphenylphosphine acetylacetone carbonyl rhodium catalyst to obtain a solid rhodium and iron oxidation mixture.

Description

technical field [0001] The invention relates to a method for removing iron in the recovery process of precious metal rhodium, which is suitable for the purification process of precious metal rhodium compounds, especially for the removal of iron ions in the recovery process of spent rhodium carbonyl acetylacetonate catalysts, and has high application value in the aspect of iron removal of rhodium compounds. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] At present, the industrial production of butanol and octanol generally uses propylene hydroformylation to synthesize butyraldehyde and then synthesize butanol and octanol. Triphenylphosphine acetylacetonate carbonyl rhodiu...

Claims

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Application Information

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IPC IPC(8): C22B11/06C22B7/00
CPCC22B11/026C22B11/048C22B11/06Y02P10/20
Inventor 谭学苓郭喜文谭承刚蒋巨光张照飞
Owner LUXI CATALYST
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