CN103966456A - Method for comprehensively recovering valuable metals from copper anode sludge silver separating slag - Google Patents

Method for comprehensively recovering valuable metals from copper anode sludge silver separating slag Download PDF

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CN103966456A
CN103966456A CN201410221705.6A CN201410221705A CN103966456A CN 103966456 A CN103966456 A CN 103966456A CN 201410221705 A CN201410221705 A CN 201410221705A CN 103966456 A CN103966456 A CN 103966456A
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silver
solution
hot acid
slag
copper anode
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CN103966456B (en
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汪金良
卢宏
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Jiangxi University of Science and Technology
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Abstract

The invention relates to a copper anode sludge silver separating slag reutilization technique, particularly a method for comprehensively recovering valuable metals from copper anode sludge silver separating slag. The method comprises the following steps: carrying out hot acid leaching on silver separating slag, filtering to obtain a hot acid leaching solution containing silver and barium and hot acid leaching slag containing tin and lead; diluting the hot acid leaching solution with water, filtering to obtain a precipitate, dissolving the precipitate with nitric acid, and filtering to obtain a barium sulfate precipitate and a silver nitrate solution; reducing the solution to obtain silver powder; leaching the hot acid leaching slag with acidic chlorine salt, filtering to obtain a chlorine salt leaching solution and chlorine salt leaching slag; cooling the chlorine salt leaching solution to crystallize and precipitate lead chloride; and carrying out alkali fusion, water immersion and evaporation crystallization on the chlorine salt leaching slag to obtain sodium stannate. The method can effectively recover all the valuable metals with higher content in the silver separating slag, and the recovery rates of the lead, silver, tin and barium are respectively up to higher than 97%, 92%, 90% and 95%. The method has the characteristics of simple technique, no emission of three wastes, high metal recovery rate and the like, and is suitable for large-scale industrial production.

Description

A kind of method from silver separating residue of copper anode slime comprehensively recovering valuable metal
Technical field
The present invention relates to silver separating residue of copper anode slime reutilization technology, particularly a kind of method from silver separating residue of copper anode slime comprehensively recovering valuable metal.
Background technology
Dividing silver-colored slag is the recrement of copper anode mud after extracting the valuable metals such as precious metal gold and silver, platinum, palladium and copper, selenium, tellurium, and main component is tin, lead, barium, silver and a small amount of gold and micro-platinum, palladium, has very high comprehensive reutilization and is worth.
Current, few to valuable metal recovery utilization research in minute silver-colored slag, how each smeltery will divide silver-colored slag to return to pyrometallurgical smelting stove (application number: 200810049459.5), increased Charge Treatment, and tin, lead is failed to open a way and is reclaimed, constantly accumulation, likely affect cupric electrolysis operation, minority is sold precious metal returned enterprise, but also only focus on gold in minute silver-colored slag, recovery (the patent application 90103200.X of silver, 97105925.X, 200710303815.7, 201010184502.6, 201110092626.6, 201210475308.2, 201310245462.5, 201310144214.1), cause the waste of other valuable metals.Patent application 200910084613.7 discloses a kind of method that silver separating residue of copper anode slime of circuit board reclaims slicker solder, patent application 201110292654.2 discloses a kind of method of producing Babbitt metal from silver separating residue of copper anode slime, these methods relate to the recovery of plumbous in minute silver-colored slag and tin, but mainly for silver separating residue of copper anode slime of circuit board.Different from silver separating residue of copper anode slime of circuit board, the anode sludge obtaining from copper-sulphide ores or composition brass smelting process divides silver-colored slag except containing more lead, silver and tin, the barium that contains 30% left and right, these barium exist with barium sulfate form, be wrapped in the valuable metals such as a large amount of tin, silver, bring very large difficulty to comprehensively recovering valuable metal from minute silver-colored slag.
Summary of the invention
The object of this invention is to provide a kind of method from silver separating residue of copper anode slime comprehensively recovering valuable metal, can be by the higher whole efficient recovery of valuable metal of content in silver separating residue of copper anode slime.
For achieving the above object, the present invention will divide silver-colored slag first to carry out hot acid leaching, and silver and barium leaching are entered to hot acid leach liquor, and tin and lead are stayed in hot acid leached mud; After hot acid leach liquor dilute with water, barium precipitates with Sulfuric acid disilver salt form with barium sulfate form, silver; Precipitation is after nitric acid dissolve, and barium is stayed in precipitation, and silver enters solution with Silver Nitrate form, after reduction, obtains silver powder; Hot acid leached mud is after acid villaumite leaches, and lead enters chloride leaching solution with lead chloride form, after crystallisation by cooling, separates out lead chloride crystallization, and mother liquor returns to villaumite and leaches; Villaumite leached mud, after alkali fusion, water logging, evaporative crystallization, obtains sodium stannate crystallization, and crystalline mother solution returns to alkali fusion.
Technological process and processing parameter that the present invention is concrete are as follows:
A, silver separating residue of copper anode slime is put into steel basin, adds the vitriol oil to carry out hot acid leaching, after filtration hot acid leached mud and hot acid leach liquor; Extract technology condition is: liquid-solid mass ratio is 2:1~10:1, and temperature is 200~500 ℃, and the time is 5~60 minutes;
B, by A step hot acid leach liquor dilute with water, water consumption is 10%~50% of hot acid leach liquor volume, after filtration diluent and precipitation, diluent returns copper anode mud pretreatment process;
C, the precipitation that the water logging of B step is obtained are put into steel basin, add 16mol/L nitric acid dissolve, and liquid-solid mass ratio is 1:1~3:1, obtain after filtration barium sulfate precipitate and silver nitrate solution;
D, the hydrazine hydrate (N for silver nitrate solution that C step is obtained 2h 4h 2o) reduce at normal temperatures and obtain silver powder, hydrazine hydrate consumption is theoretical value 1.5~3.0 times;
E, A step hot acid leached mud is leached under acid chlorine salt system, after filtration villaumite leached mud and chloride leaching solution; Extract technology condition is: liquid-solid mass ratio is 7:1~11:1, and sodium chloride concentration is 200~300g/l, and calcium chloride concentration is 4~40g/l, and concentration of hydrochloric acid is 0.5~1.5mol/l, and temperature is 60~90 ℃, and the time is 0.5~2.0 hour;
F, E step chloride leaching solution is carried out to crystallisation by cooling, temperature is normal temperature, 6~12 hours time, after filtration lead chloride crystallization and crystalline mother solution, crystalline mother solution returns to villaumite and leaches operation;
G, E step villaumite leached mud is mixed with sodium hydroxide, carry out alkali fusion and obtain calcining; Alkali fusion processing condition are: temperature is 600~850 ℃, and the time is 1~3 hour, and sodium hydroxide concentration is 0.6~1.2 times of villaumite leached mud quality;
H, the calcining water that G step alkali fusion is obtained leach, and obtain after filtration sodium stannate solution and water logging slag, and water logging slag returns copper anode mud pretreatment process; Water logging processing condition are: liquid-solid mass ratio is 3:1~6:1, and temperature is 30~60 ℃, and the time is 1~3 hour;
I, the sodium stannate solution that H step is obtained carry out evaporative crystallization, and controlling sodium stannate solution proportion is 1.2~1.3, obtain sodium stannate product, and crystalline mother solution returns to alkali fusion procedure.
Described all ingredients is technical grade reagent.
With the existing method comparison of reclaiming valuable metal from silver separating residue of copper anode slime, the present invention has following advantage: by the high barium of content in minute silver-colored slag, by hot acid leaching and tin, plumbous separated, and then separated with silver by nitric acid dissolve, the valuable metals such as the tin that makes to be wrapped up by barium, silver, lead are released, thereby realized the high efficiente callback of the valuable metals such as tin, silver, lead, barium, the rate of recovery of lead, silver, tin and barium reaches respectively more than 97%, 92%, 90% and 95%; Have technique simple, without " three wastes " discharge, metal recovery rate advantages of higher, be applicable to large-scale commercial production.
Accompanying drawing explanation
Accompanying drawing is process flow sheet of the present invention.
Embodiment
As shown in drawings, the present invention can be widely used in comprehensively recovering valuable metal from all kinds of minutes silver-colored slags, be particularly suitable for processing the high silver separating residue of copper anode slime of baric from copper-sulphide ores or useless composition brass production process output, its main component scope is (%) by weight percentage: Pb5.0~20.0, Ag1.0~10.0, Sn2.0~20.0, Ba10.0~40.0.
Embodiment 1:
Dividing silver-colored slag main component is (%): Pb16.0, Ag1.86, Sn7.5, Ba31.97 by weight percentage.
Toward 500g, divide silver-colored slag to add vitriol oil 750ml, at 350 ℃, leach 15 minutes, obtain hot acid leach liquor and hot acid leached mud.
150ml water dilution for hot acid leach liquor, obtains diluent and precipitation after filtration; Diluent returns copper anode mud pretreatment process, and precipitation is dissolved with 16mol/L nitric acid 350ml, obtains after filtration barium sulfate precipitate and silver nitrate solution, barium sulfate precipitate dry weight 263.4g, the barium sulfate containing 98.5%, the barium rate of recovery 95.5%; The hydrazine hydrate reduction of 3 times of theoretical values for silver nitrate solution, obtains silver powder 8.63g, and purity reaches 99.5%, silver raising recovery rate 92.3%.
Hot acid leached mud adds water 1400ml, sodium-chlor 475g, 6mol/L hydrochloric acid 170ml, calcium chloride 13.5g, stirs 2 hours at 60 ℃, filters to obtain chloride leaching solution and villaumite leached mud; Chloride leaching solution normal temperature crystallisation by cooling 6 hours, filters to obtain lead chloride crystallization 106.6g, and purity reaches 98%, and lead recovery is 97.3%, and crystalline mother solution returns to villaumite and leaches operation; Villaumite leached mud adds sodium hydroxide 50g, after mixing at 700 ℃ alkali fusion 2 hours, the calcining obtaining is placed and is cooled to room temperature, add water 300ml, at 60 ℃, stir 1.5 hours, filter to obtain sodium stannate solution and water logging slag, water logging slag returns copper anode mud pretreatment process; Sodium stannate solution is carried out to evaporative crystallization, and controlling sodium stannate solution proportion is 1.2, filters, dryly obtains sodium stannate product 81.45g, and purity reaches GB/T26040-2010 one-level, and the tin rate of recovery is 91.2%.
Embodiment 2:
Dividing silver-colored slag main component is (%): Pb11.5, Ag5.55, Sn8.5, Ba28.85 by weight percentage.
Toward 500g, divide silver-colored slag to add vitriol oil 1000ml, at 250 ℃, leach 25 minutes, obtain hot acid leach liquor and hot acid leached mud.
350ml water dilution for hot acid leach liquor, obtains diluent and precipitation after filtration; Diluent returns copper anode mud pretreatment process, and precipitation is dissolved with 16mol/L nitric acid 500ml, obtains after filtration barium sulfate precipitate and silver nitrate solution, barium sulfate precipitate dry weight 240.5g, the barium sulfate containing 98.9%, the barium rate of recovery 97.0%; The hydrazine hydrate reduction of 1.5 times of theoretical values for silver nitrate solution, obtains silver powder 26.54g, and purity reaches 99.1%, silver raising recovery rate 94.8%.
In hot acid leached mud, add water 1200ml, sodium-chlor 450g, 6mol/L hydrochloric acid 150ml, calcium chloride 12.5g, at 80 ℃, stir 1 hour, filter to obtain chloride leaching solution and villaumite leached mud; Chloride leaching solution normal temperature crystallisation by cooling 8 hours, filters to obtain lead chloride crystallization 76.2g, and purity reaches 98.5%, and lead recovery is 97.3%, and crystalline mother solution returns to villaumite and leaches operation.Villaumite leached mud adds sodium hydroxide 40g, after mixing at 600 ℃ alkali fusion 3 hours, the calcining obtaining is placed and is cooled to room temperature, add water 280ml, at 30 ℃, stir 2.5 hours, filter to obtain sodium stannate solution and water logging slag, water logging slag returns copper anode mud pretreatment process; Sodium stannate solution is carried out to evaporative crystallization, and the proportion of controlling sodium stannate solution is 1.25, filters, dryly obtains sodium stannate product 95.58g, and purity reaches GB/T26040-2010 one-level, and the tin rate of recovery is 94.5%.
Embodiment 3:
Dividing silver-colored slag main component is (%): Pb9.78, Ag7.13, Sn10.5, Ba24.95 by weight percentage.
Toward 500g, divide silver-colored slag to add vitriol oil 900ml, at 400 ℃, leach 10 minutes, obtain hot acid leach liquor and hot acid leached mud.
300ml water dilution for hot acid leach liquor, obtains diluent and precipitation after filtration; Diluent returns copper anode mud pretreatment process, and precipitation is dissolved with 16mol/L nitric acid 300ml, obtains after filtration barium sulfate precipitate and silver nitrate solution, barium sulfate precipitate dry weight 210.9g, the barium sulfate containing 98.7%, the barium rate of recovery 98.2%; The hydrazine hydrate reduction of 2 times of theoretical values for silver nitrate solution, obtains silver powder 34.18g, and purity reaches 99.2%, silver raising recovery rate 95.1%.
Hot acid leached mud adds water 1000ml, sodium-chlor 650g, 6mol/L hydrochloric acid 350ml, calcium chloride 45.5g, stirs 0.5 hour at 90 ℃, filters to obtain chloride leaching solution and villaumite leached mud; Chloride leaching solution normal temperature crystallisation by cooling 12 hours, filters to obtain lead chloride crystallization 64.5g, and purity reaches 98.9%, and lead recovery is 97.2%, and crystalline mother solution returns to villaumite and leaches operation; Villaumite leached mud adds sodium hydroxide 60g, after mixing at 850 ℃ alkali fusion 1 hour, the calcining obtaining is placed and is cooled to room temperature, add water 350ml, at 40 ℃, stir 2 hours, filter to obtain sodium stannate solution and water logging slag, water logging slag returns copper anode mud pretreatment process; Sodium stannate solution is carried out to evaporative crystallization, and controlling sodium stannate solution proportion is 1.3, filters, dryly obtains sodium stannate product 115.55g, and purity reaches GB/T26040-2010 one-level, and the tin rate of recovery is 92.4%.

Claims (2)

1. from a method for silver separating residue of copper anode slime comprehensively recovering valuable metal, it is characterized in that: comprise the following steps:
A, silver separating residue of copper anode slime is put into steel basin, adds the vitriol oil to carry out hot acid leaching, after filtration hot acid leached mud and hot acid leach liquor; Extract technology condition is: liquid-solid mass ratio is 2:1~10:1, and temperature is 200~500 ℃, and the time is 5~60 minutes;
B, by A step hot acid leach liquor dilute with water, water consumption is 10%~50% of hot acid leach liquor volume, after filtration diluent and precipitation, diluent returns copper anode mud pretreatment process;
C, the precipitation that the water logging of B step is obtained are put into steel basin, add 16mol/L nitric acid dissolve, and liquid-solid mass ratio is 1:1~3:1, obtain after filtration barium sulfate precipitate and silver nitrate solution;
D, the silver nitrate solution that C step is obtained reduce at normal temperatures and obtain silver powder with hydrazine hydrate, hydrazine hydrate consumption is theoretical value 1.5~3.0 times;
E, A step hot acid leached mud is leached under acid chlorine salt system, after filtration villaumite leached mud and chloride leaching solution; Extract technology condition is: liquid-solid mass ratio is 7:1~11:1, and sodium chloride concentration is 200~300g/l, and calcium chloride concentration is 4~40g/l, and concentration of hydrochloric acid is 0.5~1.5mol/l, and temperature is 60~90 ℃, and the time is 0.5~2.0 hour;
F, E step chloride leaching solution is carried out to crystallisation by cooling, temperature is normal temperature, 6~12 hours time, after filtration lead chloride crystallization and crystalline mother solution, crystalline mother solution returns to villaumite and leaches operation;
G, E step villaumite leached mud is mixed with sodium hydroxide, carry out alkali fusion and obtain calcining; Alkali fusion processing condition are: temperature is 600~850 ℃, and the time is 1~3 hour, and sodium hydroxide concentration is 0.6~1.2 times of villaumite leached mud quality;
H, the calcining water that G step alkali fusion is obtained leach, and obtain after filtration sodium stannate solution and water logging slag, and water logging slag returns copper anode mud pretreatment process; Water logging processing condition are: liquid-solid mass ratio is 3:1~6:1, and temperature is 30~60 ℃, and the time is 1~3 hour;
I, the sodium stannate solution that H step is obtained carry out evaporative crystallization, and controlling sodium stannate solution proportion is 1.2~1.3, obtain sodium stannate product, and crystalline mother solution returns to alkali fusion procedure.
2. a kind of method from silver separating residue of copper anode slime comprehensively recovering valuable metal according to claim 1, it is characterized in that: Best Applying Condition: by 500g, divide silver-colored slag to add vitriol oil 1000ml, at 250 ℃, leach 25 minutes, obtain hot acid leach liquor and hot acid leached mud;
350ml water dilution for hot acid leach liquor, obtains diluent and precipitation after filtration; Diluent returns copper anode mud pretreatment process, and precipitation is dissolved with 16mol/L nitric acid 500ml, obtains after filtration barium sulfate precipitate and silver nitrate solution, barium sulfate precipitate dry weight 240.5g, the barium sulfate containing 98.9%, the barium rate of recovery 97.0%; The hydrazine hydrate reduction of 1.5 times of theoretical values for silver nitrate solution, obtains silver powder 26.54g, and purity reaches 99.1%, silver raising recovery rate 94.8%;
In hot acid leached mud, add water 1200ml, sodium-chlor 450g, 6mol/L hydrochloric acid 150ml, calcium chloride 12.5g, at 80 ℃, stir 1 hour, filter to obtain chloride leaching solution and villaumite leached mud; Chloride leaching solution normal temperature crystallisation by cooling 8 hours, filters to obtain lead chloride crystallization 76.2g, and purity reaches 98.5%, and lead recovery is 97.3%, and crystalline mother solution returns to villaumite and leaches operation; Villaumite leached mud adds sodium hydroxide 40g, after mixing at 600 ℃ alkali fusion 3 hours, the calcining obtaining is placed and is cooled to normal temperature, add water 280ml, at 30 ℃, stir 2.5 hours, filter to obtain sodium stannate solution and water logging slag, water logging slag returns copper anode mud pretreatment process; Sodium stannate solution is carried out to evaporative crystallization, and the proportion of controlling sodium stannate solution is 1.25, filters, dryly obtains sodium stannate product 95.58g, and purity reaches GB/T26040-2010 one-level, and the tin rate of recovery is 94.5%.
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CN104841564A (en) * 2015-05-15 2015-08-19 西北矿冶研究院 Lead-silver residue flotation combined collecting agent and application process thereof
CN105886782A (en) * 2016-06-29 2016-08-24 江西铜业集团公司 Method for recycling valuable metal in silver residue by using full-wet method
CN106702166A (en) * 2017-02-06 2017-05-24 温州中希电工合金有限公司 Method for recycling silver in high oil-bearing sludge
CN106756039A (en) * 2016-12-14 2017-05-31 江西自立环保科技有限公司 A kind of wet processing process of Treatment of Copper nickel tin antimony complex materials
CN106939377A (en) * 2017-04-27 2017-07-11 中南大学 A kind of chlorination of sulfur acid lead materials takes off the method that lead liquid is recycled
CN107502744A (en) * 2017-08-04 2017-12-22 江西铜业集团公司 A kind of processing method of high lead barium silver separating residues
CN108034825A (en) * 2017-12-22 2018-05-15 中国科学院过程工程研究所 The method that wet method extracts gold and silver from the earth of positive pole
CN108913912A (en) * 2018-08-01 2018-11-30 济源职业技术学院 A kind of device of the waste recycling copper generated from Copper making
CN113604672A (en) * 2021-08-09 2021-11-05 四川省乐山锐丰冶金有限公司 Method for recovering lead chloride and rare earth from lead-barium slag

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Cited By (13)

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Publication number Priority date Publication date Assignee Title
CN104841564A (en) * 2015-05-15 2015-08-19 西北矿冶研究院 Lead-silver residue flotation combined collecting agent and application process thereof
CN105886782A (en) * 2016-06-29 2016-08-24 江西铜业集团公司 Method for recycling valuable metal in silver residue by using full-wet method
CN105886782B (en) * 2016-06-29 2018-01-23 江西铜业集团公司 A kind of method of valuable metal in Whote-wet method recovery silver separating residues
CN106756039A (en) * 2016-12-14 2017-05-31 江西自立环保科技有限公司 A kind of wet processing process of Treatment of Copper nickel tin antimony complex materials
CN106702166A (en) * 2017-02-06 2017-05-24 温州中希电工合金有限公司 Method for recycling silver in high oil-bearing sludge
CN106939377A (en) * 2017-04-27 2017-07-11 中南大学 A kind of chlorination of sulfur acid lead materials takes off the method that lead liquid is recycled
CN107502744A (en) * 2017-08-04 2017-12-22 江西铜业集团公司 A kind of processing method of high lead barium silver separating residues
CN108034825A (en) * 2017-12-22 2018-05-15 中国科学院过程工程研究所 The method that wet method extracts gold and silver from the earth of positive pole
CN108034825B (en) * 2017-12-22 2019-07-19 中国科学院过程工程研究所 The method that wet process extracts gold and silver from the earth of positive pole
CN108913912A (en) * 2018-08-01 2018-11-30 济源职业技术学院 A kind of device of the waste recycling copper generated from Copper making
CN108913912B (en) * 2018-08-01 2020-11-13 济源职业技术学院 Device for recovering copper from waste slag generated in copper smelting
CN113604672A (en) * 2021-08-09 2021-11-05 四川省乐山锐丰冶金有限公司 Method for recovering lead chloride and rare earth from lead-barium slag
CN113604672B (en) * 2021-08-09 2022-10-04 四川省乐山锐丰冶金有限公司 Method for recovering lead chloride and rare earth from lead-barium slag

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