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Method for separating and extracting silver, palladium, copper and germanium in silver separation residues

A technology for separating silver slag and silver, which is applied in the field of separation and extraction of silver, palladium, copper and germanium in silver slag, can solve the problems of complex impurity components, low germanium grade, and long process flow, and achieve simple operation, low equipment investment, and simple process flow Effect

Inactive Publication Date: 2021-09-03
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main sources of germanium in the industry are the by-products of lead-zinc mines and coal mines. The grade of germanium in such raw materials is low, the impurities are complex, the process is long, and the recovery cost is high.

Method used

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  • Method for separating and extracting silver, palladium, copper and germanium in silver separation residues
  • Method for separating and extracting silver, palladium, copper and germanium in silver separation residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Add 100 g of silver-separating slag to slurry, stir evenly, add 5mol / L hydrochloric acid and distill and purify at 90°C to obtain germanium chloride liquid, wherein, feed chlorine gas while heating (the feed amount of chlorine gas is a theoretical amount 1.5 times of 1.5 times); germanium chloride is hydrolyzed and post-treated to obtain germanium oxide; (2) the silver-separating slag that is reacted through step (1) is filtered to obtain leaching slag and filtrate, and the leaching slag and sodium carbonate are mixed uniformly at 1100 Smelting under ℃, obtain silver ingot, after measuring, the recovery rate of silver is 98.3%; (3) in the filtrate that step (2) obtains, add organic extract (wherein organic extract comprises 10% extraction agent LIX63 and 2 % modified preparation MIBK) to simultaneously extract palladium and copper elements, the volume ratio of the formed organic phase to the aqueous phase is 1:1, and the extraction time is 3min; Obtain copper-rich s...

Embodiment 2

[0042] (1) Add 100 g of silver-separating slag to water slurry, stir evenly, add 5mol / L hydrochloric acid and distill and purify at 100° C. to obtain germanium chloride liquid, wherein, feed chlorine gas while heating (the feed amount of chlorine gas is a theoretical amount 1.2 times of 1.2 times); germanium chloride is hydrolyzed and post-treated to obtain germanium oxide; (2) the silver-separating slag through step (1) reaction is filtered to obtain leaching slag and filtrate, and the leaching slag and sodium carbonate are mixed uniformly at 1100 Smelting under ℃, obtain silver ingot, after measuring, the rate of recovery of silver is 98.3%; (3) add organic extract (wherein organic extract comprises 20% extraction agent N235 and 5% in the filtrate that step (2) obtains) % modified preparation TBP) to extract the palladium element, the volume ratio of the formed organic phase to the aqueous phase is 1:1, and the extraction time is 3min; (4) the raffinate obtained in step (3) i...

Embodiment 3

[0044] (1) 100g of silver slag is added with water to adjust the slurry, stir evenly, add 7mol / L hydrochloric acid and distill and purify at 95°C to obtain germanium chloride liquid, wherein, feed chlorine gas while heating (the feed amount of chlorine gas is a theoretical amount 1.2 times of 1.2 times); germanium chloride is hydrolyzed and post-treated to obtain germanium oxide; (2) the silver-separating slag through step (1) reaction is filtered to obtain leaching slag and filtrate, and the leaching slag and sodium carbonate are mixed uniformly at 1100 Smelting under ℃, obtain silver ingot, after measuring, the recovery rate of silver is 98.3%; (3) add organic extraction liquid (wherein the extraction agent LIX63 that comprises 30% in the organic extraction liquid) in the filtrate that step (2) obtains, Extract palladium and copper elements at the same time, the volume ratio of the formed organic phase to the aqueous phase is 1:1, and the extraction time is 3 minutes; (4) fir...

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Abstract

The invention provides a method for separating and extracting silver, palladium, copper and germanium in silver separation residues. The method comprises the steps that S1, water is added into the silver separation residues for size mixing, after uniform stirring, an acid solution and a chlorine-containing oxidant are added, a system is heated and distilled, germanium chloride liquid is obtained, and the germanium chloride liquid is subjected to hydrolyzing and post-treatment to obtain germanium oxide; S2, the silver separation residues obtained after the reaction in the step S1 are filtered, leaching residues and filtrate are obtained, the leaching residues and sodium carbonate are smelted after being uniformly mixed, and metal silver is obtained; S3, organic extraction liquid is added into the filtrate obtained in the step S2, element palladium element and element copper are extracted and separated, and the organic extraction liquid comprises an extraction agent and an organic diluent; S4, a mixed liquid loaded organic phase obtained in the step S3 is subjected to reverse extraction and separation on the element palladium and the element copper, and copper reverse extraction liquid and palladium reverse extraction liquid are obtained; S5, the copper reverse extraction liquid is concentrated and crystallized to obtain copper salt, and a precipitator is added into the palladium reverse extraction liquid to prepare ammonium chloropalladate precipitate; and S6, ammonium chloropalladate is subjected to calcining and reduction to obtain metal palladium.

Description

technical field [0001] The disclosure relates to the field of enrichment and recovery of rare and precious metals, in particular to a method for separating and extracting silver, palladium, copper and germanium in silver-separating slag. Background technique [0002] As a rare and precious metal material, silver palladium germanium has irreplaceable applications in infrared optics, electronics, medicine and other fields. At present, the main sources of germanium in the industry are the by-products of lead-zinc mines and coal mines. The grade of germanium in such raw materials is low, the impurities are complex, the process is long, and the recovery cost is high. However, some secondary resources such as waste or waste devices produced in the production process of electronics, optics and semiconductor materials are rich in rare and precious metals such as silver, germanium and palladium, which have good economic benefits and social significance. At the same time, the recycli...

Claims

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Application Information

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IPC IPC(8): C22B7/04C22B41/00C22B11/02C22B11/00C22B15/00C22B1/02C22B3/26C22B3/28C22B3/30
CPCC22B7/04C22B7/007C22B41/00C22B11/042C22B11/021C22B15/0071C22B15/0069C22B1/02C22B7/001Y02P10/20
Inventor 行卫东朱刘
Owner FIRST RARE MATERIALS CO LTD
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