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Green Recovery Method of Expired Palladium Catalyst

A recovery method, palladium catalyst technology, applied in the direction of improving process efficiency, etc., can solve problems such as polluting the environment, increasing the cost of palladium refining, and difficulty in dissolving palladium sulfide, achieving energy-saving environment, improving dissolution rate and recovery rate, and high production efficiency Effect

Active Publication Date: 2020-01-31
GUIYAN RESOURCE YIMEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Using sodium sulfide to precipitate and enrich palladium sulfide concentrate from palladium leaching solution to obtain palladium sulfide concentrate is easy to operate, fast, and the recovery of palladium is high, but there are two disadvantages in obtaining pure palladium from the separation and purification of palladium sulfide concentrate: (1) Palladium sulfide is difficult to dissolve. Repeated dissolution of aqua regia increases the cost of palladium refining
(2) Dissolving palladium sulfide in aqua regia will produce hydrogen sulfide gas and pollute the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The green recovery method of spent palladium catalyst is carried out in sequence as follows:

[0034] A. Crushing ball mill:

[0035] The invalid Pd / Al in the form of pellets or strips with a palladium content of 1000ppm 2 o 3 The catalyst is ground to 40 mesh;

[0036] B. Dissolving:

[0037] Put 1200 liters of industrial hydrochloric acid with a concentration of 3mol / L into the enamel kettle, stir at a stirring speed of 50 rpm, slowly put 300 kg of the crushed and ground material in step A into the enamel kettle, heat to 80°C, and start to drop Sodium chlorate solution, the amount of sodium chlorate added dropwise is 1.5 kilograms, after the sodium chlorate solution is added dropwise, continue to react for 4 hours, stop heating, after cooling to room temperature, filter; repeat the above dissolution process to dissolve the filter residue once more, filter 2 times containing palladium filtrate merged; The content of insoluble filter residue palladium 20ppm;

[003...

Embodiment 2

[0050] The green recovery method of spent palladium catalyst is carried out in sequence as follows:

[0051] A. Crushing ball mill:

[0052] The invalid Pd / Al in the form of pellets or strips with a palladium content of 2246ppm 2 o 3 The catalyst is ground to 50 mesh;

[0053] B. Dissolving:

[0054]Put 1,200 liters of industrial hydrochloric acid with a concentration of 3mol / L into the enamel kettle, stir at a stirring speed of 60 rpm, slowly put 300 kg of the crushed and ground material in step A into the enamel kettle, heat to 85°C, and start adding dropwise Sodium chlorate solution, the amount of sodium chlorate added dropwise is 5.39 kilograms, after the sodium chlorate solution is added dropwise, continue to react for 4.5 hours, stop heating, after cooling to room temperature, filter; repeat the above dissolution process to dissolve the filter residue once more, filter 2 times containing palladium filtrate merged; The content of insoluble filter residue palladium 35p...

Embodiment 3

[0067] The green recovery method of spent palladium catalyst is carried out in sequence as follows:

[0068] A. Crushing ball mill:

[0069] The invalid Pd / Al in the form of pellets or strips with a palladium content of 3168ppm 2 o 3 The catalyst is ground to 60 mesh;

[0070] B. Dissolving:

[0071] Put 1200 liters of industrial hydrochloric acid with a concentration of 4mol / L into the enamel kettle, stir at a stirring speed of 70 rpm, slowly put 300 kg of the crushed and ground material in step A into the enamel kettle, heat to 85°C, and start to add dropwise Sodium chlorate solution, the amount of sodium chlorate added dropwise is 9.5 kilograms, after the sodium chlorate solution is added dropwise, continue to react for 5 hours, stop heating, after cooling to room temperature, filter; repeat the above dissolution process to dissolve the filter residue once more, filter 2 times containing palladium filtrate merged; The content of insoluble filter residue palladium 60ppm;...

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Abstract

The invention relates to the field of secondary resource comprehensive utilization of precious metal, in particular to a green recovery method for a dead palladium catalyst. The green recovery methodfor the dead palladium catalyst is sequentially conducted according to the following steps of (A) breaking for ball milling, (B) dissolving, (C) vulcanization, (D) high-temperature smelting, (E) activation, (F) hydrochloric acid dissolving for removing aluminum and (G) palladium refining. The recovery rate of palladium is higher than 98%, operation is easy, the process is short, the production efficiency is high, and the production process is clean, energy-saving and environmental friendly.

Description

technical field [0001] The invention relates to the field of comprehensive utilization of precious metal secondary resources, in particular to a green recovery method for spent palladium catalysts. Background technique [0002] Palladium has excellent catalytic activity and is widely used in automobile industry, fine chemical industry, petrochemical industry, nitric acid industry, coal chemical industry and hydrogen peroxide industry, etc. [0003] Coal-to-ethylene glycol is to replace petroleum ethylene with coal to produce ethylene glycol. This technical route is in line with the resource characteristics of my country's lack of oil, less gas, and relatively rich coal resources. At present, the production capacity of coal-to-ethylene glycol that has been put into production in China exceeds 2 million tons , The palladium catalyst loaded in the device is about 1000 tons. By 2020, the national coal-to-ethylene glycol industry will have more than 5,000 tons of palladium cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B11/00C22B11/02
CPCC22B11/026C22B11/048Y02P10/20
Inventor 贺小塘王欢吴喜龙赵雨李勇刘文张选冬李子璇王金营
Owner GUIYAN RESOURCE YIMEN