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Method for recovering rhodium from inactivated rhodium-phosphine complex catalyst

A catalyst and complexation technology, applied in the field of rhodium recovery, can solve problems such as complex recovery process and pollution, and achieve the effects of simplified process flow, simple equipment and low pollution

Active Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to overcome problems such as complex recovery process and serious pollution in the prior art method, the present invention provides a simple and efficient organic one-phase method for recovering rhodium from the deactivated rhodium-phosphine complex catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The used catalyst waste liquid is an inactivated catalyst in the process of producing butyraldehyde through the hydroformylation reaction of propylene, carbon monoxide and hydrogen, and its activity is reduced to below 30% of that of the fresh catalyst.

[0032]The catalyst waste liquid was concentrated on a scraped thin film evaporation device. The concentration of rhodium in the resulting concentrated waste liquid is 1700ppm, containing 6.5wt% of triphenylphosphine, 11.1% of triphenylphosphine oxide, and the rest are butyraldehyde trimers and polymers, high-boiling point organic by-products, and other small amounts of metals Impurities.

[0033] Weigh 24.97 g of the above-mentioned concentrated catalyst waste liquid and add it into a 500 ml three-neck flask, then add 200 ml of absolute ethanol, and stir to make it evenly mixed. Air is introduced into the mixed solution in the flask, and the air is bubbled through the bottom of the liquid through an immersion tube, so...

Embodiment 2

[0035] Weigh 26.79 g of the concentrated catalyst waste liquid in Example 1 and add it into a 500 ml three-neck flask, then add 200 ml of absolute ethanol, and stir to make it evenly mixed. Air is introduced into the liquid in the flask, and the air is bubbled through the bottom of the liquid through an immersion tube, so that the oxygen and the catalyst waste liquid are fully contacted and reacted, and the flow rate of the air is 100ml / min. Stir and slowly raise the temperature to 90°C, stop feeding air after 24 hours of reaction. During this process triphenylphosphine has been substantially completely oxidized to triphenylphosphine oxide. Then the temperature of the reaction system was lowered to 70° C., 50 ml of 20% NaOH ethanol solution was added to the flask, and the reaction was continued at 70° C. for 5 h, and then cooled to room temperature. Filter, remove the solvent, wash with distilled water and ethanol respectively, and dry under vacuum at 50°C to obtain 0.31 g of...

Embodiment 3

[0037] Weigh 25.54 g of the concentrated catalyst waste liquid in Example 1 and add it into a 500 ml three-necked flask, then add 100 ml of absolute ethanol, and stir to make it evenly mixed. Add 2ml of tert-butyl hydroperoxide to the flask, slowly heat to 60°C, and react for 15h. Then add 5.06g of NaOH powder, heat to 70°C, continue the reaction for 3h, then cool down to room temperature. Filter, remove the solvent, wash with distilled water and ethanol respectively, and dry under vacuum at 50°C to obtain 0.28 g of a yellow-brown solid. Elemental analysis showed that the yield was 65% based on rhodium atoms.

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PUM

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Abstract

The invention provides an easy and effective organic one-phase method. The method comprises dissolving, oxidizing, adding alkaline substances and filtering. Rhodium is recovered from the inactivated rhodium-phosphine complex catalyst by separating. An obtained rhodium-containing solid can be directly used for synthesizing the rhodium-phosphine complex catalyst, and is not required to be reduced into simple substance rhodium, so that the conventional process flow is simplified. The method has the advantages of wide application range, mild process condition, simple needed requirement, no need of burning or high-temperature treatment, small pollution, and easiness for operating.

Description

technical field [0001] The invention relates to a method for recovering precious metals, in particular to a method for recovering rhodium from deactivated rhodium-phosphine complex catalysts. Background technique [0002] The hydroformylation process of reacting olefins with hydrogen and carbon monoxide to form aldehyde products using a rhodium-tertiary organophosphorus complex as a catalyst is well known in the art. The most common example is with RhH(CO)(TPP) 3 As a catalyst, butyraldehyde is prepared from propylene with hydrogen and carbon monoxide. In the long-term continuous industrial production process, rhodium-phosphine complex catalysts are often deactivated by various high-boiling by-products and impurities carried by raw materials during the reaction process. Even if there is basically no impurity entrained in the raw material, the catalyst will generate inactive rhodium cluster complexes under the comprehensive action of reaction temperature, reactant partial p...

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B3/04C22B3/46C22B11/00
CPCY02P10/20
Inventor 李彤吕顺丰黄凤兴王世亮刘博秦燕璜
Owner CHINA PETROLEUM & CHEM CORP
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