CN103088218B - Silver, plumbous method is extracted from the smelting slag that copper anode mud pyrogenic attack produces - Google Patents
Silver, plumbous method is extracted from the smelting slag that copper anode mud pyrogenic attack produces Download PDFInfo
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- CN103088218B CN103088218B CN201310015731.9A CN201310015731A CN103088218B CN 103088218 B CN103088218 B CN 103088218B CN 201310015731 A CN201310015731 A CN 201310015731A CN 103088218 B CN103088218 B CN 103088218B
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Abstract
The invention provides a kind of method that extraction is silver-colored, plumbous from the smelting slag that copper anode mud pyrogenic attack produces, belong to metallurgical technology field.The method is that the smelting slag that copper anode mud pyrogenic attack produces is carried out fragmentation, first adopts Sulfothiorine, copper sulfate, S-WAT and ammoniacal liquor to leach as leach liquor and extracts silver; Leach after filtrate adopts SODIUM HYDROSULPHITE sodium reduction and can return continuation Leaching of Silver; Adopt hydrochloric acid-Leaching of sodium chloride to extract to the leached mud after Leaching of Silver plumbous, return continuation after leaching plumbous filtrate precipitation separation of lead and leach plumbous.Present invention process is simple, easy to operate, process, and silver-colored, plumbous extraction yield is high, and (leaching yield of silver is 75 ~ 87%, plumbous extraction yield is more than 90%) final filtrate cycle use, cost is low, strong adaptability, environmental friendliness, is applicable to large-scale commercial production, has good application prospect.
Description
Technical field
The invention belongs to metallurgical technology field, relate to the recycling of the solid slag produced in copper anode mud pyrogenic attack process, particularly relate to a kind of method that extraction is silver-colored, plumbous from the smelting slag that copper anode mud pyrogenic attack produces.
Background technology
Copper anode mud is in the electrorefining processes of copper ore concentrates, is made up of the element corrected than copper current potential and the various materials that are insoluble to electrolytic solution, and its composition depends primarily on the technical qualification etc. of the composition of copper anode, castability and electrolysis.Point silver-colored slag is the recrement of copper anode mud after extracting the valuable elements such as precious metal gold and silver, platinum, palladium and copper, selenium, tellurium, and smelting slag be copper anode mud after pressurization Strengthen education nickel, copper, tellurium drier, pyrometallurgical smelting obtain the residue that produces in the thick alloy process of gold and silver.Main containing sodium, silicon, barium, lead and other elements in smelting slag, separately also containing certain Determination of Rare-Expensive Elements, as gold and silver, selenium, tellurium, bismuth, platinum metals etc., be also the important source material extracting precious metal.In smelting slag, chemical composition and phase composite are all very complicated, and be mostly the metal acid-salt of complicated silicate, arsenate, vitriol, oxide compound and sodium, wherein lead content is in 10 ~ 20%(mass percent), the mass percentage of silver is 0.1 ~ 1.0%.The smelting slag that copper anode mud pyrogenic attack produces is the very good material of the valuable metals such as Comprehensive Recovery of Ag, gold, lead, carries out recycling to it, has important meaning for the serious scarcity solving Precious Metals Resources.
Due to smelting slag complicated component, than gangue ore deposit, carry out independently precious metal to it and extract and reclaim, ore dressing difficulty is larger, if it is directly returned dressing-works ore dressing, falls flat; And than the anode sludge, in slag, bullion content is low, process more difficult.At present, be that not only gold and silver yield is lower by its direct Returning smelting stove to extract gold and silver to the processing mode of smelting slag both at home and abroad, the harm such as lead, antimony and impurity element also can be caused to leach, thus affect the quality of follow-up cathode copper.In addition, fire reduction melting extraction is carried out only to the single metallic element of certain in smelting slag, owing to containing dystectic silicate and vitriol in smelting slag, fire reduction melting is extracted single metallic element and is not only brought high energy consumption, inefficient detrimentally affect, thus some valuable metal both wasted in slag, cause again new environmental pollution.Adopt wet method to carry out comprehensive reutilization to smelting slag, the smelting slag composition produced due to copper anode mud pyrogenic attack is quite complicated, and the most of valuable metal cycles in comprehensive reutilization smelting slag are long, complex process is heavy, efficiency is low.
Summary of the invention
The object of the invention is for problems of the prior art, provide a kind of and extract silver, plumbous method from the smelting slag that copper anode mud pyrogenic attack produces.
The present invention extracts silver, plumbous method from the smelting slag that copper anode mud pyrogenic attack produces, and comprises following processing step:
(1) leach desilver: after the smelting slag that copper anode mud pyrogenic attack produces is carried out fragmentation, adopt the mixed solution of Sulfothiorine-copper sulfate-sodium sulfite solution as leach liquor, control solid-to-liquid ratio at 1:6 ~ 1:10g/ml; Adjust pH=8 ~ 11 with ammoniacal liquor, agitation leach 0.5 ~ 5h at the temperature of 20 ~ 45 DEG C, solid-liquid separation obtains leaching filter residue and leach liquor; Leach filter residue and carry lead for leaching; Add V-Brite B in leach liquor, stir reduction 0.5 ~ 2h, solid-liquid separation at 50 ~ 70 DEG C, separation slag is raw Ag powder, returns continuation Leaching of Silver after adding Sulfothiorine (add-on is 0.01 ~ 0.1 g/ml) adjustment in parting liquid.
In described mixing leach liquor, Sulfothiorine can form more stable complexing ion with silver ions, has good leaching effect to the compound of silver, and leaching rate is fast, and Selectively leaching efficiency is high; Cupric ion in copper sulfate has the effect of oxygenant, and ammoniacal liquor both can adjust ph, can form complexing ion again with cupric ion, is conducive to the leaching of silver.
In described mixing leach liquor, the quality of Sulfothiorine is 20 ~ 50% of smelting slag quality; The quality of copper sulfate is 2 ~ 6% of smelting slag quality, and the quality of S-WAT is 4 ~ 12% of smelting slag quality; The add-on of described V-Brite B is 1 ~ 5% of smelting slag quality.The leaching yield of silver is 75 ~ 87%.
(2) lead is carried in leaching: adopt the mixed solution of concentrated hydrochloric acid-sodium-chlor as leach liquor the leaching filter residue of step (1), and control solid-to-liquid ratio at 1:6 ~ 1:10g/ml, agitation leach 1 ~ 6h at 90 ~ 100 DEG C, solid-liquid separation obtains leached mud and leach liquor; Leached mud can continue on for extracting its use such as other metals after inspection chemical composition; Leach liquor thin up 1 ~ 10 times separates out rich plumbous thing, then carries out solid-liquid separation and must be separated slag and parting liquid; Being separated slag is the lead chloride of high-content, can be used for producing plumbous product; Return after (addition of hydrochloric acid is 0.05 ~ 0.2 g/ml, and the addition of sodium-chlor is 0.1 ~ 0.3 g/ml) after adding hydrochloric acid and sodium-chlor adjustment in parting liquid and continue to leach lead.
In the mixed solution of concentrated hydrochloric acid-sodium-chlor, copper anode mud pyrogenic process can divide the oxide compound in the residue after silver, sulfide etc. to change into the hydrochloride of solubility by concentrated hydrochloric acid, is conducive to plumbous leaching; Sodium-chlor mainly improves the chlorine ion concentration in solution, can be plumbous muriate by simple substance lead and plumbous converting compounds again, for the leaching of lead.
In the mixed solution of concentrated hydrochloric acid-sodium-chlor, the final concentration of described concentrated hydrochloric acid is 50 ~ 200g/L, and the final concentration of sodium-chlor is 100 ~ 300g/L.Plumbous extraction yield is up to more than 95%.
Hinge structure of the present invention has the following advantages:
1, after the smelting slag that copper anode mud pyrogenic attack produces is carried out fragmentation by the present invention, first adopt Sulfothiorine-copper sulfate-S-WAT-ammoniacal liquor to leach as leach liquor and extract silver, leach after filtrate adopts SODIUM HYDROSULPHITE sodium reduction silver and can return continuation Leaching of Silver; Adopt hydrochloric acid-Leaching of sodium chloride to extract to the leached mud after Leaching of Silver plumbous, return continuation after leaching plumbous filtrate precipitation separation of lead and leach plumbous, silver is high with the extraction yield of lead, achieves the recycling of the solid slag produced in copper anode mud pyrogenic attack process.
2, present invention process is simple, easy to operate, and final filtrate cycle uses, and has saved cost, has decreased environmental pollution.
3, present device is simple, process, environmental friendliness, strong adaptability, is applicable to large-scale commercial production, has good application prospect.
Embodiment
Below by specific embodiment, silver is extracted from the smelting slag that copper anode mud pyrogenic attack produces to the present invention, plumbous method elaborates.
Embodiment 1
(1) desilver is leached: after the smelting slag that copper anode mud pyrogenic attack produces is carried out mechanical disintegration, precise residue powder 100g, put into 1000ml beaker, add 600ml water (solid-to-liquid ratio is 1:6 g/ml), add 4g copper sulfate, 10g S-WAT, 50g Sulfothiorine and 20ml ammoniacal liquor (system pH=10.8), be heated to 35 DEG C, and holder ties up to 33 ~ 37 DEG C, Keep agitation soaks silver-colored 2h; Then carry out solid-liquor separation, obtain leaching filter residue (91.8g) and leach liquor; Leach filter residue to enter next step and carry out leaching and carry lead; Add 3g V-Brite B in leach liquor, be warmed up to 60 DEG C, and holder ties up to 55 ~ 65 DEG C, Keep agitation reduces silver-colored 30min, solid-liquid separation, and separation slag is raw Ag powder; Can add again in parting liquid 20g Sulfothiorine continue to return carry out leaching silver.In the smelting slag that copper anode mud pyrogenic attack produces, the leaching yield of silver is 87.0%.
(2) lead is carried in leaching: above-mentioned desilver is leached filter residue and puts into 1000ml beaker, add 700ml water (solid-to-liquid ratio is 1:8 g/ml), add concentrated hydrochloric acid, sodium-chlor respectively, stir, the final concentration of concentrated hydrochloric acid is 80g/L, and sodium chloride concentration is 250g/L; Be warmed up to 95 DEG C, and holder ties up to more than 90 DEG C, agitation leach 2h; Filter solid-liquid separation and obtain leached mud and leach liquor; Leached mud can continue on for extracting its use such as other metals after inspection chemical composition; In leach liquor, thin up 2 times separates out rich plumbous thing, then carries out solid-liquid separation and must be separated slag and parting liquid, and being separated slag is the lead chloride of high-content, can be used for producing plumbous product; Returning continuation after being separated rear liquid interpolation 80g hydrochloric acid and 200g sodium-chlor leaches plumbous.Leaching yield plumbous in the smelting slag that copper anode mud pyrogenic attack produces is 95.3%.
Embodiment 2
(1) desilver is leached: the smelting slag that copper anode mud pyrogenic attack produces is carried out mechanical disintegration, precise residue powder 100g, put into 1000ml beaker, add 800ml water (solid-to-liquid ratio is 1:8 g/ml), add 4g copper sulfate, 8g S-WAT, 40g Sulfothiorine and 15ml ammoniacal liquor (system pH=10.3), be heated to 35 DEG C, and holder ties up to 33 ~ 37 DEG C, Keep agitation soaks silver-colored 2h.Then carry out solid-liquor separation to obtain leaching filter residue (92.1g) and leach liquor; Leach filter residue to enter next step and carry out leaching and carry lead; Add 3g V-Brite B in leach liquor, be warmed up to 60 DEG C, and holder ties up to 55 ~ 65 DEG C, Keep agitation reduces silver-colored 30min, solid-liquid separation, and separation slag is raw Ag powder; Can add again in parting liquid 25g Sulfothiorine continue to return carry out leaching silver.In the smelting slag that copper anode mud pyrogenic attack produces, the leaching yield of silver is 81.9%.
(2) lead is carried in leaching: above-mentioned desilver is leached filter residue and puts into 1000ml beaker, add 700ml water (solid-to-liquid ratio is 1:8 g/ml), add concentrated hydrochloric acid, sodium-chlor respectively, stir, the final concentration of concentrated hydrochloric acid is 64g/L, and sodium chloride concentration is 250g/L, be warmed up to 95 DEG C, and holder ties up to more than 90 DEG C, agitation leach 2h, filters solid-liquid separation and obtains leached mud and leach liquor; Can continue on for extracting its use such as other metals after inspection chemical composition; Leach liquor thin up 2 times separates out rich plumbous thing, then carries out solid-liquid separation and must be separated slag and parting liquid, and being separated slag is the lead chloride of high-content, can be used for producing plumbous product; Parting liquid returns after adding 100g hydrochloric acid and 250g sodium-chlor and continues to leach lead.In the smelting slag produce copper anode mud pyrogenic attack, plumbous leaching yield is 98.3%.
Embodiment 3
(1) desilver is leached: the smelting slag that copper anode mud pyrogenic attack produces is carried out mechanical disintegration, precise residue powder 500g, put into 5000ml beaker, add 3000ml water (solid-to-liquid ratio is 1:6 g/ml), add 20g copper sulfate, 45g S-WAT, 200g Sulfothiorine and 70ml ammoniacal liquor (system pH=10.5), be heated to 35 DEG C, and holder ties up to 32 ~ 39 DEG C, Keep agitation soaks silver-colored 1h.Then carry out solid-liquor separation to obtain leaching filter residue (461.8 g) and leach liquor; Leach filter residue to enter next step and carry out leaching and carry lead; Add 15g V-Brite B in leach liquor, be warmed up to 60 DEG C, and holder ties up to 52 ~ 68 DEG C, Keep agitation reduces silver-colored 45min, solid-liquid separation, and separation slag is raw Ag powder, can add 125g Sulfothiorine again and continue to return and carry out leaching silver in parting liquid.In the smelting slag that copper anode mud pyrogenic attack produces, the leaching yield of silver is 83.7%.
(2) lead is carried in leaching: above-mentioned desilver is leached filter residue and puts into 5000ml beaker, add 3600ml water (solid-to-liquid ratio is 1:8 g/ml), add concentrated hydrochloric acid, sodium-chlor respectively, stir, the final concentration of concentrated hydrochloric acid is 80g/L, and sodium chloride concentration is 250g/L, be warmed up to 95 DEG C, and holder ties up to more than 90 DEG C, agitation leach 2h, filters solid-liquid separation and obtains leached mud and leach liquor; Leached mud can continue on for extracting its use such as other metals after inspection chemical composition; Leach liquor thin up 2 times separates out rich plumbous thing, then carries out solid-liquid separation, and being separated slag is the lead chloride of high-content, can be used for producing plumbous product; Parting liquid returns after adding 300g hydrochloric acid and 650g sodium-chlor and continues to leach lead.Leaching yield plumbous in the smelting slag that copper anode mud pyrogenic attack produces is 98.6%.
Claims (1)
1. from the smelting slag that copper anode mud pyrogenic attack produces, extract silver, plumbous method, comprise following processing step: (1) leaches desilver: after the smelting slag that copper anode mud pyrogenic attack produces is carried out fragmentation, adopt the mixed solution of Sulfothiorine-copper sulfate-sodium sulfite solution as leach liquor, control solid-to-liquid ratio at 1:6 ~ 1:10g/ml; Adjust pH=8 ~ 11 with ammoniacal liquor, agitation leach 0.5 ~ 5h at the temperature of 20 ~ 45 DEG C, solid-liquid separation obtains leaching filter residue and leach liquor; Leach filter residue and carry lead for leaching, add V-Brite B in leach liquor, stir reduction 0.5 ~ 2h, solid-liquid separation at 50 ~ 70 DEG C, separation slag is raw Ag powder, and parting liquid returns continuation Leaching of Silver after adjustment; In described mixing leach liquor, the quality of Sulfothiorine is 20 ~ 50% of smelting slag quality; The quality of copper sulfate is 2 ~ 6% of smelting slag quality; The quality of S-WAT is 4 ~ 12% of smelting slag quality; The add-on of V-Brite B is 1 ~ 5% of smelting slag quality; Being adjusted to of described parting liquid: add Sulfothiorine in parting liquid, the addition of Sulfothiorine is 0.01 ~ 0.1 g/ml;
(2) lead is carried in leaching: adopt the mixed solution of hydrochloric acid-sodium-chlor as leach liquor above-mentioned leaching filter residue, and control solid-to-liquid ratio at 1:6 ~ 1:10g/ml, agitation leach 1 ~ 6h at 90 ~ 100 DEG C, solid-liquid separation obtains leached mud and leach liquor; Leach liquor thin up 1 ~ 10 times separates out rich plumbous thing, then carries out solid-liquid separation and must be separated slag and parting liquid; Being separated slag is the lead chloride of high-content; Parting liquid returns and continues to leach lead after adjustment; The final concentration of described hydrochloric acid is 50 ~ 200g/L; The final concentration of described sodium-chlor is 100 ~ 300g/L; The adjustment of described parting liquid is: in parting liquid, add hydrochloric acid and sodium-chlor, and the addition of hydrochloric acid is 0.05 ~ 0.2 g/ml; The addition of sodium-chlor is 0.1 ~ 0.3 g/ml.
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| CN111650192A (en) * | 2020-06-16 | 2020-09-11 | 中国原子能科学研究院 | Method for removing lead in lead-bismuth alloy and method for measuring tellurium in lead-bismuth alloy |
| CN115323187B (en) * | 2022-08-19 | 2023-08-22 | 中南大学 | Method for removing SnPbFe impurities in platinum group metal-rich copper anode slime |
| CN115504439B (en) * | 2022-09-07 | 2023-09-29 | 金川集团股份有限公司 | Method for removing lead from high-lead tellurium powder |
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| CN1067271A (en) * | 1992-03-31 | 1992-12-23 | 西安冶金建筑学院 | Extract the method for gold and silver with lime sulfur mixture |
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