CN101824546A - Method for recovering silver from lead-separating liquid of silver-separating residue of copper anode slime - Google Patents
Method for recovering silver from lead-separating liquid of silver-separating residue of copper anode slime Download PDFInfo
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- CN101824546A CN101824546A CN201010184502A CN201010184502A CN101824546A CN 101824546 A CN101824546 A CN 101824546A CN 201010184502 A CN201010184502 A CN 201010184502A CN 201010184502 A CN201010184502 A CN 201010184502A CN 101824546 A CN101824546 A CN 101824546A
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- Y02P10/20—Recycling
Abstract
The invention discloses a method for recovering silver from the lead-separating liquid of the silver-separating residue of copper anode slime, which relates to a method for greenly recovering silver in the lead-separating liquid by adopting a step-by-step precipitation method. The method includes lead-separating process, and also includes the processes that: the lead-separating liquid is poured into a stirring tank, sodium hydroxide is added for neutralization, so that the pH of the lead-separating liquid is regulated to 6 to 8, lead is precipitated in the form of lead hydroxide, lead-containing material and first filtrate are obtained by filtration, and the lead-containing material is washed by water and returns to the lead-separating process to separate lead; sodium sulfate is added in the first filtrate until the solution does not produce precipitate, filter residue and second filtrate are obtained by filtration, and the filter residue is centrally treated; sodium hydroxide is utilized to regulate the pH of the second filtrate to no less than 11, a moderate amount of formaldehyde is added, stirring is carried out for 10 to 30 minutes, silver powder and third filtrate are obtained by filtration, hydrochloric acid is added into the third filtrate to regulate the pH to less than 1, and the third filtrate retunes to the lead-separating process. The method is characterized in that: the technique is simple and easy, the used materials and equipment are common and cheap, the final filtrate is recycled, and no pollution is generated.
Description
Technical field
The invention belongs to the recycling that the silver-colored slag of branch divides plumbous liquid silver, particularly reclaim and divide silver-colored slag to divide silver in the plumbous liquid in the copper anode mud.
Background technology
Silver separating residue of copper anode slime is the recrement after copper anode mud extracts valuable elements such as precious metal gold and silver, platinum, palladium and copper, selenium, tellurium.Copper anode mud is in the electrorefining process, forms than the element and the various materials that are insoluble to electrolytic solution of the corrigendum of copper current potential, and its composition depends primarily on composition, castability and the electrolytic technical qualification of copper anode, and its productive rate is generally 0.2-0.8%; It contains Au, Ag, Cu, Pb, Se, Te, As, Sb, Bi, Ni, Fe, S, Sn, SiO usually
2, Al
2O
3, platinum metals and moisture.Derive from the anode sludge of copper sulfide concentrate, contain more Cu, Se, Ag, Pb, Te and a small amount of Au, Sb, Bi, As and gangue mineral, the platinum metals seldom; And the anode sludge that derives from copper one Ni sulphide mine contains more Cu, Ni, S, Se, and precious metal is mainly the platinum metals, and the content of Au, Ag, Pb is less; The circuit card composition brass anode sludge that electrolysis is produced then contains higher Pb, Sn, and precious metal mainly is Ag, also has a spot of Au and platinum metals.
The output capacity of the silver-colored slag of branch is generally the 50-60% of copper anode mud, a smeltery that produces 100000 t electrolytic coppers per year, and about output anode sludge 750t, output is divided silver-colored slag 350-450t.About gold content 10g/t, about silver-colored 500-5000g/t, the platinum palladium is all about 5-15g/t in the silver-colored slag of branch; Mainly based on plumbous, tin, both account for about the 30-60% of the quantity of slag base metal.When being faced with abundant ore source and exploiting the awkward situation that exhaustion, no ore deposit can adopt gradually, the utilization again in non-ferrous metal secondary ore deposit is seemed very urgent, open a new situation also for country's regeneration mineral resources comprehensive utilization along with domestic many large-scale nonferrous mines.Because this slag ingredient complexity, than the gangue ore deposit, the ore dressing difficulty is bigger, directly returns the ore dressing of ore dressing field and falls flat.Than the anode sludge, divide silver-colored slag bullion content low, reclaim precious metal difficulty more, handle workshop section so reverberatory furnace is put or returned to many copper smelting plants all temporarily to this slag muck, and it is poor to return processing precious metal recovering effect, and gives entire treatment workshop section aggravate the burden.
It is few that domestic slicker solder to minute silver-colored slag is recycled research, each smeltery is many will to divide silver-colored slag to return copper reverberatory furnace workshop section, as the Chinese patent application application of number 200810049459.5 " pyrogenic process separates the smelting process and the device thereof of valuable metal in the anode sludge " by name, increased the furnace charge processing, and slicker solder content but builds up, and might influence the quality of anode copper.So further development and use are waited until dividing silver-colored slag all temporarily to stack on one side by most of now producers.Minority producer sells some special precious metals with it and reclaims the business processes recovery; carry out the extraction of some precious metal element; as number of patent application 90103200.X " a kind of solder anode slime nitric acid slag extracts the method for silver and gold " by name; number of patent application 97105925.X " a kind of method of utilizing the lead in the copper anode mud to produce lead sulfate tribasic " by name; " a kind of method of from minute silver-colored slag, extracting silver " 200710303815.7 by name etc.; the recovery of this extensive style is with some valuable metal in the waste slag; and do not consider environment protection in the technology, not only wasted resource but also caused new environmental pollution.
In Chinese patent application number 200910084613.7 " a kind of silver separating residue of copper anode slime of circuit board reclaims the method for slicker solder " by name and application number 200910089686.5 " a kind of method of recovering lead from lead paste of waste lead-acid battery " by name, disclose method plumbous method of recovery from contain scrap lead (for example waste lead acid battery lead cream and the silver-colored slag of branch) of utilizing pure hydrometallurgy and promptly divided splicer's preface, the plumbous rate of recovery is more than 95%.Utilize NaCl-CaCl
2-HCl system reclaims lead, and the solution after the recovery is called the plumbous liquid of branch, divides plumbous liquid can return branch splicer preface and recycles, have do not produce the economic environmental protection of waste liquid advantage.In minute plumbous process, because chlorine ion concentration is very high, divide the AgCl in the silver-colored slag will be dissolved in the plumbous liquid of branch, the silver content in the lead separated slag finally is reduced to about 40g/t.Therefore,, divide silver in the plumbous liquid, acquire a certain degree and the silver in minute plumbous liquid need be separated, could effectively leach the silver in the silver-colored slag of branch, reach better economical effectiveness enrichment gradually along with recycling of minute plumbous liquid.
Summary of the invention
Purpose of the present invention mainly solves the recovery problem of silver in the plumbous liquid of branch, not only can guarantee efficient recovery silver valuable metal, and processing technological flow is short, equipment simply, does not cause secondary pollution.
The method that a kind of silver separating residue of copper anode slime of the present invention divides plumbous liquid to reclaim silver is as follows, comprises branch splicer preface, also comprises the steps:
To divide plumbous liquid to put into steel basin, and add sodium hydroxide and neutralize, and make the plumbous liquid pH of score be adjusted into 6 ~ 8, lead will filter and obtain the leaded material and first filtrate with the form precipitation of lead hydroxide, and leaded material washing is returned branch splicer preface and carried out branch lead; First filtrate adds sodium sulfate, does not produce precipitation up to solution and stops to add sodium sulfate, filters, and obtains the filter residue and second filtrate, and filter residue focuses on; Utilize sodium hydroxide that second filtrate is regulated pH for being not less than 11, add an amount of formaldehyde, stirred 10-30 minute, filter and obtain silver powder and the 3rd filtrate, the 3rd filtrate adds hydrochloric acid and adjusts the pH value less than 1, returns branch splicer preface.
The formaldehyde that described adding is an amount of, formaldehyde: silver (mass ratio)=1: 3-3: 3.
Compared with prior art, because the present invention has adopted the isolating method of fractional precipitation, obtain highly purified silver powder, silver is reclaimed to greatest extent, and filtrate can be returned branch splicer preface again through subsequent disposal and realize recycling, and reaches the CR production level.
Characteristics such as the present invention has simple for process, and all more common and cheap, the final filtrate cycle of raw materials used and equipment uses, pollution-free.
Description of drawings
Fig. 1 represents branch splicer program flow diagram
Fig. 2 represents that silver separating residue of copper anode slime divides plumbous liquid to reclaim silver-colored schema.
Embodiment
Embodiment 1
Divide plumbous liquid (silver content 2.1g/L) to put into steel basin 1L, add sodium hydroxide and neutralize, make the plumbous liquid pH of score be adjusted into 6, lead will be with the form precipitation of lead hydroxide, filtration obtains the leaded material and first filtrate, and leaded material washing is returned branch splicer preface and carried out branch lead; First filtrate adds sodium sulfate, does not produce precipitation up to solution and stops to add sodium sulfate, filters, and obtains the filter residue and second filtrate, and filter residue focuses on; Utilizing sodium hydroxide that second filtrate is regulated pH is 12, adds 0.7g formaldehyde, stirs 10 minutes, filters and obtains silver powder and the 3rd filtrate, and the 3rd filtrate adds hydrochloric acid and adjusts pH=0.5, returns branch splicer preface.Silver raising recovery rate 98.5%.
Embodiment 2
Divide plumbous liquid (silver content 1.8g/L) to put into steel basin 1L, add sodium hydroxide and neutralize, make the plumbous liquid pH of score be adjusted into 7.5, lead will be with the form precipitation of lead hydroxide, filtration obtains the leaded material and first filtrate, and leaded material washing is returned branch splicer preface and carried out branch lead; First filtrate adds sodium sulfate, does not produce precipitation up to solution and stops to add sodium sulfate, filters, and obtains the filter residue and second filtrate, and filter residue focuses on; Utilizing sodium hydroxide that second filtrate is regulated pH is 11.5, adds 0.9g formaldehyde, stirs 15 minutes, filters and obtains silver powder and the 3rd filtrate, and the 3rd filtrate adds hydrochloric acid and adjusts pH=0.8, returns branch splicer preface.Silver raising recovery rate 99.1%.
Embodiment 3
Divide plumbous liquid (silver content 1.5g/L) to put into steel basin 1L, add sodium hydroxide and neutralize, make the plumbous liquid pH of score be adjusted into 8, lead will be with the form precipitation of lead hydroxide, filtration obtains the leaded material and first filtrate, and leaded material washing is returned branch splicer preface and carried out branch lead; First filtrate adds sodium sulfate, does not produce precipitation up to solution and stops to add sodium sulfate, filters, and obtains the filter residue and second filtrate, and filter residue focuses on; Utilizing sodium hydroxide that second filtrate is regulated pH is 13, adds 1.2g formaldehyde, stirs 30 minutes, filters and obtains silver powder and the 3rd filtrate, and the 3rd filtrate adds hydrochloric acid and adjusts pH=0.2, returns branch splicer preface.Silver raising recovery rate 98.6%.
Embodiment 4
Divide plumbous liquid (silver content 2.5g/L) to put into steel basin 1L, add sodium hydroxide and neutralize, make the plumbous liquid pH of score be adjusted into 7, lead will be with the form precipitation of lead hydroxide, filtration obtains the leaded material and first filtrate, and leaded material washing is returned branch splicer preface and carried out branch lead; First filtrate adds sodium sulfate, does not produce precipitation up to solution and stops to add sodium sulfate, filters, and obtains the filter residue and second filtrate, and filter residue focuses on; Utilizing sodium hydroxide that second filtrate is regulated pH is 13.5, adds 2.5g formaldehyde, stirs 25 minutes, filters and obtains silver powder and the 3rd filtrate, and the 3rd filtrate adds hydrochloric acid and adjusts pH=0, returns branch splicer preface.Silver raising recovery rate 99.2%.
Claims (2)
1. a silver separating residue of copper anode slime divides plumbous liquid to reclaim the method for silver, comprises branch splicer preface, it is characterized in that also comprising the steps:
1.1 the plumbous liquid of the branch that will divide splicer's preface to obtain is put into steel basin, add sodium hydroxide and neutralize, regulating the plumbous liquid pH value of branch is 6-8, and lead will be with the form precipitation of lead hydroxide, filtration obtains the leaded material and first filtrate, and leaded material returns branch splicer preface and carries out branch lead after washing;
1.2 first filtrate adds sodium sulfate, does not produce precipitation up to solution and stops to add sodium sulfate, filters, and obtains the filter residue and second filtrate, filter residue focuses on;
1.3 utilize sodium hydroxide to regulate second pH value of filtrate to being not less than 11, add formaldehyde and stirring, filter and obtain silver powder and the 3rd filtrate;
Adjust the 3rd pH value of filtrate to less than 1 1.4 add hydrochloric acid, return branch splicer preface.
2. a kind of silver separating residue of copper anode slime according to claim 1 divides plumbous liquid to reclaim the method for silver, it is characterized in that: in the described step 1.3, and formaldehyde: silver (mass ratio)=1: 3-3: 3, churning time is 10-30 minute.
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| CN2010101845026A CN101824546B (en) | 2010-05-20 | 2010-05-20 | Method for recovering silver from lead-separating liquid of silver-separating residue of copper anode slime |
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| CN2010101845026A CN101824546B (en) | 2010-05-20 | 2010-05-20 | Method for recovering silver from lead-separating liquid of silver-separating residue of copper anode slime |
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| CN101824546B CN101824546B (en) | 2011-11-16 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318853A (en) * | 2013-06-17 | 2013-09-25 | 山东恒邦冶炼股份有限公司 | Method for recovering selenium from copper anode slime |
| CN103966449A (en) * | 2014-05-23 | 2014-08-06 | 江西理工大学 | Method for preparing lead-tin alloy from copper anode sludge silver separating slag |
| CN103966456A (en) * | 2014-05-23 | 2014-08-06 | 江西理工大学 | Method for comprehensively recovering valuable metals from copper anode sludge silver separating slag |
| CN113528850A (en) * | 2021-07-26 | 2021-10-22 | 中南大学 | Method for purifying gold by controlling potential |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
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- 2010-05-20 CN CN2010101845026A patent/CN101824546B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
Non-Patent Citations (2)
| Title |
|---|
| 《湿法冶金》 20010331 李运刚 《湿法处理铜阳极泥工艺研究（III）-银的分离》 第18页第1.2、2.1部分、第19页第2.1.1部分、第21页第2.2.3部分 1-2 第20卷, 第1期 2 * |
| 《稀有金属与硬质合金》 20091231 张玲玲 《回收铜阳极泥预处理上清夜中银的工艺研究》 32-35 1-2 第37卷, 第4期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318853A (en) * | 2013-06-17 | 2013-09-25 | 山东恒邦冶炼股份有限公司 | Method for recovering selenium from copper anode slime |
| CN103966449A (en) * | 2014-05-23 | 2014-08-06 | 江西理工大学 | Method for preparing lead-tin alloy from copper anode sludge silver separating slag |
| CN103966456A (en) * | 2014-05-23 | 2014-08-06 | 江西理工大学 | Method for comprehensively recovering valuable metals from copper anode sludge silver separating slag |
| CN103966456B (en) * | 2014-05-23 | 2015-12-02 | 江西理工大学 | A kind of method from silver separating residue of copper anode slime comprehensively recovering valuable metal |
| CN103966449B (en) * | 2014-05-23 | 2016-01-13 | 江西理工大学 | A kind of method preparing terne metal from silver separating residue of copper anode slime |
| CN113528850A (en) * | 2021-07-26 | 2021-10-22 | 中南大学 | Method for purifying gold by controlling potential |
| CN113528850B (en) * | 2021-07-26 | 2022-06-07 | 中南大学 | Method for purifying gold by controlling potential |
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Owner name: ZHIYUAN HOLDING GROUP CO., LTD. Effective date: 20130829 |
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Inventor after: Pan Dean Inventor after: Zhang Shengen Inventor after: Li Bin Inventor after: Tian Jianjun Inventor after: Wang Yunlong Inventor after: Xue Kexin Inventor before: Pan Dean Inventor before: Zhang Shengen Inventor before: Li Bin Inventor before: Tian Jianjun |
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Free format text: CORRECT: INVENTOR; FROM: PAN DEAN ZHANG SHENGEN LI BIN TIAN JIANJUN TO: PAN DEAN ZHANG SHENGEN LI BIN TIAN JIANJUN WANG YUNLONG XUE KEXIN |
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Effective date of registration: 20130829 Address after: 100083 Haidian District, Xueyuan Road, No. 30, Patentee after: University of Science and Technology Beijing Patentee after: Zhiyuan Holding Group Co., Ltd. Address before: 100083 Haidian District, Xueyuan Road, No. 30, Patentee before: University of Science and Technology Beijing |