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Method for preparing high-purity superfine palladium powder from waste palladium-carbon catalyst

A technology of palladium-carbon catalyst and ultra-fine palladium powder, applied in the direction of improving process efficiency, etc., can solve the problems of dioxin risk, easy-to-corrosion equipment, increased energy consumption, etc., to avoid high energy consumption and small footprint of complete equipment , the effect of less time spent

Active Publication Date: 2022-04-08
SHANGHAI SECOND POLYTECHNIC UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned method has remarkable effect on the recovery of palladium in the palladium-carbon catalyst, but it also contains its own defects.
For example, high-temperature treatment will increase energy consumption; organic matter will decompose during high-temperature process, resulting in potential dioxin risk; strong acid and strong alkali treatment will easily corrode equipment and cause secondary pollution, etc.

Method used

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  • Method for preparing high-purity superfine palladium powder from waste palladium-carbon catalyst
  • Method for preparing high-purity superfine palladium powder from waste palladium-carbon catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In this example, 150 g of spent palladium-carbon catalyst powder was weighed into a 500 mL thick-walled beaker, 150 mL of absolute ethanol was slowly added, and placed in a 40 Hz ultrasonic instrument for 30 min and then left to stand. Add 50 ml of 5wt% hydrochloric acid solution to it, stir at 100-200 rpm, react for 1 hour, filter, wash, and dry. Then add 4 mol / L of hydrochloric acid and 250 mL of 2 mol / L sodium hypochlorite successively to the filter residue, react for 40 minutes under the condition of stirring speed of 80 rpm, filter and separate to obtain the filter residue and palladium-containing filtrate, the filter residue is washed with water and dried to obtain Activated carbon, palladium-containing filtrate was further processed.

[0029] Inject Phaneroderma chrysosporium (inoculum size 5vol%) into 50 mL of culture medium (glucose 20 g / L, sucrose 15 g / L, yeast powder 2 g / L, wheat bran 15 g / L, sulfuric acid heptahydrate Magnesium 0.5 g / L, potassium dihydrogen...

Embodiment 2

[0031] In this example, 100 g of spent palladium-carbon catalyst powder was weighed into a 500 mL thick-walled beaker, slowly added with 150 mL of absolute ethanol, and placed in a 40 Hz ultrasonic instrument for 30 minutes of sonication and then left to stand. Add 50 mL of 5wt% hydrochloric acid solution to it, stir at 100-200 rpm, react for 1 hour, filter, wash, and dry. Add 4 mol / L of hydrochloric acid and 250ml of sodium hypochlorite of 2 mol / L successively in the filter residue, react for 60min under the condition of stirring speed of 80 rpm, filter and separate to obtain filter residue and palladium-containing filtrate, filter residue is washed with water and dried to obtain activated carbon, and the filtrate is further processed.

[0032] Take the above filtrate, put Phaneroderma chrysosporium (10vol% inoculum) into 50 mL culture solution (glucose 20g / L, sucrose 15g / L, yeast powder 2g / L, wheat bran 15g / L, sulfuric acid heptahydrate Magnesium 0.5g / L, potassium dihydroge...

Embodiment 3

[0034] In this example, 50 g of spent palladium-carbon catalyst powder was weighed into a 500 mL thick-walled beaker, 150 mL of absolute ethanol was slowly added, and placed in a 40 Hz ultrasonic instrument for 30 minutes of sonication and then left to stand. Add 50 ml of 5wt% hydrochloric acid solution to it, stir at 100-200 rpm, react for 1 hour, filter, wash, and dry. Add 4 mol / L of hydrochloric acid and 250ml of sodium hypochlorite of 2 mol / L successively in the filter residue, react for 90min under the condition of stirring speed of 80 rpm, filter and separate to obtain filter residue and palladium-containing filtrate, filter residue is washed with water and dried to obtain Activated carbon, palladium-containing filtrate was further processed.

[0035] Inject Phaneroderma chrysosporium (15vol% inoculum) into 50 mL of culture medium (glucose 20 g / L, sucrose 15 g / L, yeast powder 2 g / L, wheat bran 15 g / L, magnesium sulfate heptahydrate 0.5 g / L, potassium dihydrogen phosphat...

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Abstract

The invention discloses a method for preparing high-purity superfine palladium powder from a waste palladium-carbon catalyst. The method comprises the following steps: (1) carrying out graded pretreatment on waste palladium-carbon catalyst powder through absolute ethyl alcohol-diluted hydrochloric acid, and removing impurity metals Ni, Al, Fe and the like; (2) treating the filter residue subjected to impurity removal in the step (1) through hydrochloric acid and sodium hypochlorite, so that palladium in the filter residue is fully leached out, and filtering and drying to obtain activated carbon; (3) reducing the palladium filtrate obtained in the step (2) with domesticated white-rot fungi to obtain palladium powder; and (4) the palladium powder obtained in the step (3) is subjected to freeze-drying treatment, and the superfine palladium powder is prepared. The preparation process is short in flow and high in efficiency, particularly, the oxidation leaching process is efficient and mild, and the white-rot fungus reduced palladium leachate is green and low-carbon. The palladium-gold extraction rate is high, the purity of the prepared palladium powder is not lower than 99.95%, and the impurity content is smaller than 0.005%.

Description

technical field [0001] The invention belongs to the technical field of precious metal extraction, and in particular relates to a method for preparing high-purity ultrafine palladium powder from waste palladium-carbon catalysts. Background technique [0002] Platinum group metals are strategic mineral resources, which are widely used in automobile exhaust catalysts, chemical catalysts, jewelry and electrical and electronic industries. [0003] Due to the accumulation of hydrocarbons (ethanol, acetone, etc.) in the palladium-carbon catalyst during the reaction process, the catalyst is deactivated. The deactivation of the palladium catalyst is mainly due to the growth of palladium grains, which reduces the catalytic active area and the coverage of impurities. . The loss of palladium in the reaction process is not very large, that is, the palladium content difference between the spent palladium catalyst and the fresh catalyst is not large, so it is possible to extract and recov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B11/00C22B3/18B22F9/24C22B1/00
CPCY02P10/20
Inventor 黄庆丁国栋顾卫华郁丰善王临才苑文仪李永敏
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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