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Method for reclaiming precious metal palladium from waste palladium-carbon catalyst

A palladium-carbon catalyst and precious metal technology, applied in the direction of improving process efficiency, etc., can solve the problems of low palladium recovery rate, long process, high cost, etc., and achieve the effect of good product quality, high recovery rate and low production cost

Active Publication Date: 2008-05-28
SINOPEC NANJING RES INST OF CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these methods have long process, high cost and low palladium recovery rate

Method used

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  • Method for reclaiming precious metal palladium from waste palladium-carbon catalyst

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Experimental program
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Effect test

Embodiment 1

[0017] Get waste palladium-carbon catalyst 10kg (dry), palladium content is 0.33% (wt), puts into tube furnace and roasts, and roasting temperature is 600 ℃, fully gas supply, and roasting ash adds formic acid reduction, and add-on is every kilogram of palladium ash Add 300 milliliters of formic acid, heat to 70 DEG C, keep for 3 hours, filter, filter residue is leached with aqueous solution of hydrochloric acid, sodium hypochlorite, hydrogen peroxide, wherein palladium ash: hydrochloric acid: sodium hypochlorite: hydrogen peroxide: water=1:5:5:5:3, temperature 75°C, 4 hours, filtration, recovery of filter residue, ion exchange of filtrate, ammonia complexation, filtration, recovery of complexation slag, acidification of complexation liquid, collection of acidification tail liquid, acidification precipitation and drying, then put into roasting furnace, 600°C Calcined at lower temperature for 4 hours, and reduced with hydrogen to obtain 32.71 g of product metal palladium.

Embodiment 2

[0019] Get spent catalyst 10kg (dry), palladium content is 0.33% (wt), puts into tube furnace and roasts, and roasting temperature is 650 ℃, fully gas supply, roasting ash is added formic acid reduction, and add-on is every kilogram of palladium ash plus 400 Milliliter of formic acid, heated to 75°C, kept for 4 hours, filtered, and the filter residue was leached with aqueous solution of hydrochloric acid, sodium hypochlorite, and hydrogen peroxide, wherein palladium ash: hydrochloric acid: sodium hypochlorite: hydrogen peroxide: water=1:6:5:8:4, temperature 80°C , time 5 hours, filtration, filter residue recovery, filtrate ion exchange, ammonia complexation, filtration, complexation slag recovery, complexation liquid acidification, acidification tail liquid collection, acidification precipitation, drying, put into roasting furnace, roasting at 550 °C After 4.5 hours, it was reduced with hydrogen to obtain 32.79 g of the product metal palladium.

Embodiment 3

[0021] Get spent catalyst 10kg (dry), palladium content is 0.33% (wt), puts into tube furnace and roasts, and roasting temperature is 700 ℃, fully gas supply, and roasting ashes adds formic acid reduction, and add-on is every kilogram of palladium ashes and adds 500 Milliliter of formic acid, heated to 80 ° C, kept for 5 hours, filtered, and the filter residue was leached with aqueous solution of hydrochloric acid, sodium hypochlorite, hydrogen peroxide, wherein palladium ash: hydrochloric acid: sodium chlorate: hydrogen peroxide: water=1:7:5:10:3, temperature 85°C, time 6 hours, filtration, recovery of filter residue, ion exchange of filtrate, ammonia complexation, filtration, recovery of complexation slag, acidification of complexation liquid, collection of acidification tail liquid, acidification precipitation and drying, then put into roasting furnace, 550°C Calcined at lower temperature for 4 hours, and reduced with hydrogen to obtain 32.75 g of product metal palladium.

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Abstract

The invention belongs to the technical field of recycling solid waste, in particular relating to a process of recycling noble metal palladium from dead palladium carbon catalysts. The process includes roasting, reduction, leaching out, impurity removal of ion-exchange, ammonia complexingk, acidifying, roasting and hydrogen reduction, and then the metal palladium is obtained. The invention is simple in technique and low in costs, the palladium recovery ratio is more than 99%, and the purity of metal palladium is more than 99.9%.

Description

Technical field: [0001] The invention belongs to the technical field of recycling solid waste, and in particular relates to a method for recycling precious metal palladium in waste palladium-carbon catalysts. Background technique: [0002] Palladium-carbon catalysts are widely used in chemical production. For example, palladium-carbon catalysts are used in the synthesis of fluoropiperidine and toluene diisocyanate, the purification of caprolactam, and the hydroprocessing of terephthalic acid. After long-term use, the palladium in the catalyst is polluted by impurities and loses its activity, becoming a spent catalyst. Since palladium is a precious metal, its resources are scarce and expensive, so its regeneration and recovery are of great significance. [0003] The palladium-carbon catalyst is based on activated carbon and contains about 0.1-10% palladium. Compared with the fresh catalyst, the palladium content of the spent palladium-carbon catalyst has decreased, and the ...

Claims

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Application Information

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IPC IPC(8): C22B11/00C22B7/00C22B1/02C22B3/06C22B3/44
CPCY02P10/20
Inventor 李玉杰孙盛凯黄伟金汉强贾艳秋王金质
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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