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Method for separating and recycling selenium and tellurium from copper anode mud

A copper anode slime, separation and recovery technology, applied in metallurgy and chemical industry, can solve the problems of high reagent consumption, low tellurium recovery rate, less than 50%, etc.

Inactive Publication Date: 2017-03-08
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the recovery process route of selenium and tellurium in the traditional process is very long, not only the consumption of reagents is large, the processing cost is high, and the recovery rate of tellurium is low, the recovery rate of tellurium is usually less than 50%, and almost no one uses it now
Another reason for this result is that most of the lead sulfate in the copper anode slime reacts with sodium carbonate in the sintering and leaching process into lead carbonate and sodium sulfate, so that the process has to increase the concentration of the leachate to dry and dry residue. Add carbon reduction and other processes to separate and recover selenium and sodium carbonate

Method used

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  • Method for separating and recycling selenium and tellurium from copper anode mud
  • Method for separating and recycling selenium and tellurium from copper anode mud

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Take 100g of copper anode slime, add 35g of anhydrous sodium carbonate, grind and mix well, and then sinter in a muffle furnace at 600°C for 3.5h. After the sintered slag is finely ground, add water at a solid-to-liquid ratio of 1:3g / ml, stir and leaching at 95°C for 1.5 h, filtered to obtain leaching solution and leaching residue. The leaching solution was acidified with sulfuric acid to pH 5.1, and the precipitated TeO was separated by filtration. 2 After that, continue to add sulfuric acid to acidify to H + The concentration is 1mol / L, slowly add sodium sulfite to reduce the Se in it according to twice the theoretical amount, stir at 85°C for 2.5h to precipitate the selenium in it, and filter to obtain coarse selenium powder and selenium-precipitated liquid; the coarse selenium powder contains Se up to 98.7 %, the selenium-precipitated solution contains Se of 0.02g / L. Add 100g / L H 2 SO 4 solution, stirred and leached at 95°C for 1.5h, filtered to obtain acid leac...

Embodiment 2

[0052] Take 10kg of decoppered anode slime, add 2kg of anhydrous sodium carbonate and 0.2kg of sodium nitrate, mix well and granulate, sinter in a multi-tang furnace at 550-630°C for 3.5h, add water to the sintered slag at a solid-to-liquid ratio of 1:1.5g / ml , Stirring and leaching at 85°C for 2.5h, and filtering to obtain leaching solution and leaching residue. CO 2 Acidify to pH 5.5, filter and separate the TeO precipitated therein 2 Finally, according to the sulfate in the solution precipitates out in the form of gypsum twice the theoretical amount, add CaCO 3 , stirred at room temperature for 2.5 hours, filtered to obtain filtrate and filter residue; filter residue was added 1mol / L sulfuric acid solution at a solid-to-liquid ratio of 1:2g / ml, stirred and washed at room temperature for 1h, filtered to obtain gypsum and washing water; after adding 4kg of sodium chloride to the filtrate Repass CO 2 to 0.3MPa, cooled and crystallized at 15°C, and filtered to obtain NaHCO ...

Embodiment 3

[0055] Take 100kg of decoppered anode slime, add 25kg of anhydrous sodium carbonate, grind and mix well, then sinter in a rotary kiln at 450-650°C for 2.5h, add water to the sintered slag at a solid-to-liquid ratio of 1:2g / ml, stir and leach at 100°C for 2h, Filter to obtain leaching solution and leaching residue. Add sodium chloride to the leaching solution to adjust the NaCl concentration to 150g / L, then cool to 0°C to crystallize, filter to obtain mixed crystals of sodium carbonate and sodium sulfate and its crystallization mother liquor; add sulfuric acid to acidify the crystallization mother liquor to pH 5.1, and filter to separate it Precipitated TeO 2 After that, add sulfuric acid to acidify to the solution acidity [H + ] is 0.1mol / L, then pass SO 2 Reduction to the Se concentration in the solution drops to 0.02g / L, and the coarse selenium powder is obtained by filtration. After the coarse selenium powder is refined by sodium sulfite dissolution-precipitation method, ...

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Abstract

Disclosed is a method for separating and recycling selenium and tellurium from copper anode mud. The method includes: performing soda sintering on the copper anode mud or copper-removed anode mud obtained after copper removing is performed on the copper anode mud, adding water into the sintered material for leaching, and filtering to obtain selenium-rich leachate and tellurium-rich leach residues; subjecting the selenium-rich leachate to sodium carbonate separating and recycling, using sodium sulfite or SO2 to revivify and recycle selenium in the selenium-rich leachate or filtrate, filtering to obtain rough selenium powder, and further refining the rough selenium powder to obtain metal selenium; leaching the tellurium-rich leach residues via a sulfuric acid solution, filtering to obtain acid leachate and acid leach residues; subjecting the acid leachate to silver separating through chlorination, using sodium sulfite or SO2 to revivify and precipitate tellurium in the chlorinated acid leachate, filtering to obtain rough tellurium powder, and further refining the rough tellurium powder to obtain metal tellurium. The method has the advantages that by the integral redesign of the process and the mutual cooperation of the steps, the process route for separating and recycling the selenium and the tellurium from the copper anode mud is simplified greatly, environmental protection pressure during a copper anode mud processing process is alleviated greatly, and the method conforms to the development tendency of energy saving and emission reduction technical transformation; the method is simple in process, simple to operate, low in production cost, high in selenium and tellurium recycling rate, good in working environment, suitable for industrialized application, and the like.

Description

technical field [0001] The invention discloses a method for separating and recovering selenium and tellurium from copper anode slime, which belongs to the technical field of metallurgy and chemical industry. Background technique [0002] Both selenium and tellurium are typical scattered elements, which are mainly enriched in the anode slime of electrolytic refining of heavy non-ferrous metals, among which copper anode slime is the main raw material for the production of selenium and tellurium. Copper anode slime usually contains Cu 10-30%, Pb 5-20%, Se1-10%, Te0.2-6%. Cu in copper anode slime mainly exists in the form of metallic copper, and almost all Pb is in the form of lead sulfate form, while selenium and tellurium mainly exist as selenides and tellurides of copper and silver. The methods for separation and recovery of selenium and tellurium from copper anode slime mainly include sulfuration roasting, distilling selenium-water leaching for copper-alkali leaching for te...

Claims

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Application Information

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IPC IPC(8): C01B19/02
CPCC01B19/02C01P2006/80
Inventor 王学文王明玉葛奇
Owner CENT SOUTH UNIV
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