Method for environment-friendly recovery of palladium from palladium-containing waste

A waste and green technology, applied in the field of iron ion oxidation, selective adsorption of palladium by anion exchange resin and tail liquid circulation, can solve the problems of large acid consumption and high waste water volume, and achieve the elimination of waste water discharge, low cost, low material consumption and energy consumption. Effect

Active Publication Date: 2018-12-07
UNIV OF SCI & TECH BEIJING
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the problems of chlorine gas generation, large acid consumption, and high waste water volume in the extraction of palladium by using aqua regia, cyanide, sodium chlorate, chlorine gas, hydrogen peroxide, etc. as oxidants in the traditional palladium recovery process, the present invention provides a green, economical, and environmentally friendly recovery process. The method of palladium, method of the present invention adopts Fe 3+ As an oxidant, it prevents the side reaction of generating chlorine gas; at the same time, anion exchange resin is used to selectively adsorb [PdCl 4 ] 2- , to realize the recycling of the tail liquid; finally desorb and reduce to obtain elemental palladium

Method used

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  • Method for environment-friendly recovery of palladium from palladium-containing waste

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Effect test

Embodiment 1

[0036] The scrap hydrogen peroxide containing palladium catalyst is distilled to remove organic matters. Preparation of palladium oxidation complexing agent, its formula is FeCl 3 1.0mol / L, hydrochloric acid 0.5 mol / L, NaCl 6.0 mol / L. Stir and heat the palladium-containing catalyst that removed the organic matter by distillation and the oxidation complexing agent to 100 ° C, react for 30 min, and filter to obtain the filter residue and [PdCl-containing 4 ] 2- filtrate, followed by R 410 Selective adsorption of [PdCl in filtrate by piperidine anion resin 4 ] 2- . Adsorption [PdCl 4 ] 2- R 410 Piperidine anion resin treated with 8% NH 3 +40 g / LNH 4 Cl desorption, hydrazine hydrate reduction to obtain elemental palladium, the purity of palladium is 99.5%, and the recovery rate of palladium is 97.8%. Fe 2+ Oxidized to Fe 3+ The post cycle is used to oxidize the complexing agent.

Embodiment 2

[0038] The waste petrochemical hydrogenation palladium catalyst is ball milled, calcined and reduced to remove organic matter and improve the reactivity of palladium. Preparation of palladium oxidation complexing agent, its formula is FeCl 3 0.8 mol / L, hydrochloric acid 1.0 mol / L, NaCl 5.0 mol / L. Stir and heat the activated palladium-containing catalyst and oxidative complexing agent to 95°C, react for 40 min, and filter to obtain filter residue and [PdCl-containing 4 ] 2- filtrate, and then use 9335 type anion resin to selectively adsorb [PdCl in the filtrate 4 ] 2- . Adsorption [PdCl 4 ] 2- The 9335 type anion resin was treated with 8% NH 3 +40 g / L NH 4 Cl desorption, formaldehyde reduction to obtain elemental palladium, the purity of palladium is 99.2%, and the recovery rate of palladium is 98.4%. Fe 2+ Oxidized to Fe 3+ The post cycle is used to oxidize the complexing agent.

Embodiment 3

[0040] The scrapped nitric acid industrial palladium-containing catalyst is crushed and reduced to improve the reactivity of palladium. Preparation of palladium oxidation complexing agent, its formula is FeCl 3 0.7 mol / L, hydrochloric acid 3.0 mol / L, NaCl 2.0 mol / L, KCl 1.0 mol / L. Stir and heat the activated palladium-containing catalyst and oxidative complexing agent to 90°C, react for 60 min, and filter to obtain filter residue and [PdCl-containing 4 ] 2- filtrate, and then use polyamide resin to selectively adsorb [PdCl in the filtrate 4 ] 2- . Adsorption [PdCl 4 ] 2- The polyamide resin was desorbed with 5% thiourea+0.5mol / L HCl and reduced with formic acid to obtain elemental palladium. The purity of palladium was 99.7%, and the recovery rate of palladium was 99.3%. Fe 2+ Oxidized to Fe 3+ The post cycle is used to oxidize the complexing agent.

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Abstract

The invention mainly belongs to the field of secondary precious metal, and relates to a method for environment-friendly recovery of palladium from palladium-containing waste. The method comprises thesteps that the palladium-containing waste is subjected to pre-treatment such as ball grinding, calcination, reduction and distillation, palladium is oxidized in an acid system with Fe3+ as an oxidizing agent, and combined with chloride ions to enter a liquid phase, leachate selectively adsorbs [PdCl4]2 through anion exchange resin, elemental palladium is obtained in desorption and reduction modes,and Fe2+ is oxidized into Fe3+ for recycling. According to the method, the environment-friendly pollution-free Fe3+ oxidizing agent is adopted, palladium is adsorbed through the anion resin, tail liquid is recycled, and the method has the advantages of economical efficiency, environment friendliness, energy saving, emission reduction and the like and is suitable for industrial application.

Description

technical field [0001] The invention mainly belongs to the field of regenerated precious metals, and relates to a method for green recovery of palladium from palladium-containing waste materials, in particular to a method for iron ion oxidation, anion exchange resin selective adsorption of palladium and tail liquid circulation. Background technique [0002] Due to its unique physical and chemical properties such as corrosion resistance, good thermal stability and catalytic activity, palladium is widely used in modern technology and industrial fields such as aerospace, military industry, electronic appliances, transportation, petrochemical industry, etc., and is called "the vitamin of modern industry". ", is an important strategic metal. [0003] Palladium is mainly produced in South Africa, the United States, Canada, Russia, Australia and other countries. In these countries, palladium reserves account for more than 99% of the global total. In 2017, my country's palladium co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B11/00C22B7/00
CPCC22B11/046C22B11/048Y02P10/20
Inventor 张深根丁云集刘波
Owner UNIV OF SCI & TECH BEIJING
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