CN101555550A - Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board - Google Patents

Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board Download PDF

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Publication number
CN101555550A
CN101555550A CNA2009100846137A CN200910084613A CN101555550A CN 101555550 A CN101555550 A CN 101555550A CN A2009100846137 A CNA2009100846137 A CN A2009100846137A CN 200910084613 A CN200910084613 A CN 200910084613A CN 101555550 A CN101555550 A CN 101555550A
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lead
silver
liquid
sodium
water
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CN101555550B (en
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张深根
潘德安
田建军
李彬
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ZHIYUAN HOLDING GROUP CO Ltd
University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses a method for recycling lead-tin in silver separating residue of copper anode slime of a circuit board and relates to a method for recycling silver separating residue of copper anode slime of the circuit board by a wetting method. The method comprises the following steps of: stirring silver separating residue, water, hydrochloric acid, calcium chloride and sodium chloride for 0.5 to 2.0h under proper temperature according to requirements, filtering and obtaining lead separating liquid and lead separating residue; carrying out displacement to the lead separating liquid by using excess iron powder, filtering and obtaining spongy lead and displaced liquid; using sodium hydroxide to adjust pH value of the displaced liquid till the precipitate is not generated; and returning lead separating procedure after the iron is precipitated. The lead separating residue, the sodium hydroxide and sodium nitrate are mixed evenly to carry out roasting with the temperature of 350 to 500 DEG C, and then are added with water and filtered, thus obtaining the sodium stannate. Compared with the prior art, due to the adoption of a full-wetting process, the method reduces a large amount of waste gas and dusts in the process of pyrometallurgical treatment; the liquid after the iron is precipitated contains the main compositions of hydrochloric acid and sodium chloride; and the method can return acid pickling procedure, reduce discharge of waste water and lower cost, and is characterized by simple technique, no pollution and the like.

Description

A kind of silver separating residue of copper anode slime of circuit board reclaims the method for slicker solder
Technical field
The present invention relates to the method for hydrometallurgic recovery anode sludge slicker solder, particularly relate to the method for hydrometallurgic recovery silver separating residue of copper anode slime of circuit board slicker solder.
Background technology
The silver-colored slag of branch 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 with the various materials that are insoluble to electrolytic solution than the element that copper current potential is higher, 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-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, Au and platinum metals, and the silver-colored slag of branch that precious metal obtains after extracting contains Pb, Sn is higher, has very high recovery value.
It is few that domestic slicker solder to minute silver-colored slag is recycled research, and each smeltery is many will to divide silver-colored slag to return copper reverberatory furnace workshop section (application number: 200810049459.5), increased the furnace charge processing, and slicker solder content builds up but, 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 (patent application 90103200.X, 97105925.X, 200710303815.7) of some precious metal element; 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.
Lead mainly is with PbSO in the silver-colored slag of branch 4, PbCl 2, PbS, PbO and Pb form exist, wherein lead sulfate accounts for more than 95%.And tin is mainly with SnO 2Form exists, and accounts for more than 95% of tin total amount.Soak plumbous theory, PbSO according to chlorination process 4, PbCl 2Solubleness in water is very little, but two kinds of precipitations are dissolved in the dense NaCl solution of heat, so under the hot conditions, with the aqueous hydrochloric acid is medium, add sodium-chlor, lead sulfate is dissolved in the salt solution, and lead sulfide, metallic lead and plumbous oxide also are converted into lead chloride accordingly and extract from minute gold and silver slag under hydrochloric acid and sodium chloride medium condition.Tindioxide is stable tetravalence structure, is insoluble to bronsted lowry acids and bases bronsted lowry.Therefore, tindioxide must be made the transition the form that can be dissolved in acid, could realize that the wet method of tin is extracted.In the compound of tin, sodium stannate can be water-soluble, can obtain by alkali fusion.
Summary of the invention
Purpose of the present invention mainly solves the anode sludge and divides slicker solder recovery problem in the silver-colored slag, not only can guarantee that efficient recovery divides the valuable metal of the slicker solder in the silver-colored slag, and processing technological flow is short, equipment is simple.
The anode sludge of the present invention divides silver-colored slag slicker solder recovery method as follows:
To divide silver-colored slag to dissolve by design requirements water, hydrochloric acid, calcium chloride and sodium-chlor, water wherein: divide silver-colored slag=5: 1~10: 1, concentration of hydrochloric acid is 50~100g/L, calcium chloride concentration is 100~300g/L, sodium chloride concentration is 150~300g/L, 75~95 ℃ are stirred 0.5~2.0h down, filter and obtain plumbous liquid of branch and lead separated slag; Divide plumbous liquid to replace, filter and obtain spongy lead and displaced liquid with excess iron powder; Displaced liquid is regulated the pH value up to not producing precipitation with sodium hydroxide, and liquid returns branch splicer preface behind the heavy iron; Lead separated slag adds sodium hydroxide and SODIUMNITRATE mixes, and forms the lead separated slag mixture, wherein sodium hydroxide: divide silver-colored slag=1: 10~3: 10, SODIUMNITRATE: divide silver-colored slag=1: 100~5: 100; The lead separated slag mixture is carried out 350~500 ℃ of roasting 1.0~3.0h, roasting sand is placed 24~48h in air, add entry and carry out water logging, stir 0.5~1.0h, water: divide silver-colored slag=3: 1~5: 1, filter and obtain sodium stannate.
Compared with prior art, because the present invention has adopted wet processing process, reduce the large quantity of exhaust gas and the dust that produce in the pyrogenic attack process; Liquid and evaporation back liquid can return the plumbous and water logging operation recycle of branch respectively behind the heavy iron, reduce discharge of wastewater, reduce cost.
Characteristics such as the present invention has simple for process, and raw materials used and equipment is all more common and cheap, pollution-free.
Description of drawings
Fig. 1 represents that the anode sludge divides silver-colored slag slicker solder recovery process figure
Embodiment
Embodiment 1
50g divides silver-colored slag to add entry 250g, hydrochloric acid 20g, and calcium chloride 50g, sodium-chlor 30g, 80 ℃ are stirred 0.5h down; Filtration obtains plumbous liquid of branch and lead separated slag, divides plumbous liquid to replace with excess iron powder, filters to obtain spongy lead and displaced liquid, and displaced liquid is regulated the pH value up to not producing precipitation with sodium hydroxide, and liquid returns branch splicer preface behind the heavy iron; Lead separated slag adds sodium hydroxide 5g and SODIUMNITRATE 1g, mixes; 350 ℃ of roasting 1.5h; Roasting sand is placed 24h in air, add entry 150g, stir 0.5h, filter and obtain sodium stannate.Lead recovery 95.3%, the tin rate of recovery 98.2%.
Embodiment 2
100g divides silver-colored slag to add liquid 200g behind the embodiment 1 heavy iron, water 500g, and hydrochloric acid 25g, calcium chloride 70g, sodium-chlor 100g, 75 ℃ are stirred 1h down; Filtration obtains plumbous liquid of branch and lead separated slag, divides plumbous liquid to replace with excess iron powder, filters to obtain spongy lead and displaced liquid, and displaced liquid is regulated the pH value up to not producing precipitation with sodium hydroxide, and liquid can return branch splicer preface behind the heavy iron; Lead separated slag adds sodium hydroxide 20g and SODIUMNITRATE 4g, mixes; 420 ℃ of roasting 1h; Roasting sand is placed 30h in air, add entry 400g, stir 1h, filter and obtain sodium stannate.Lead recovery 93.7%, the tin rate of recovery 99.1%.
Embodiment 3
50g divides silver-colored slag to add liquid 200g behind the embodiment 2 heavy iron, water 50g, and hydrochloric acid 5g, calcium chloride 30g and sodium-chlor 20g, 95 ℃ are stirred 2h down; Filtration obtains plumbous liquid of branch and lead separated slag, divides plumbous liquid to replace with excess iron powder, filters to obtain spongy lead and displaced liquid, and displaced liquid is regulated the pH value up to not producing precipitation with sodium hydroxide, and liquid can return branch splicer preface behind the heavy iron; Lead separated slag adds sodium hydroxide 7g and SODIUMNITRATE 2g, mixes; 450 ℃ of roasting 2h; Roasting sand is placed 48h in air, add entry 250g, stir 0.5h, filter and obtain sodium stannate.Lead recovery 94.1%, the tin rate of recovery 97.8%.
Embodiment 4
150g divides silver-colored slag to add liquid 250g behind the embodiment 3 heavy iron, water 750g, and hydrochloric acid 60g, calcium chloride 120g and sodium-chlor 170g, 90 ℃ are stirred 1h down; Filtration obtains plumbous liquid of branch and lead separated slag, divides plumbous liquid to replace with excess iron powder, filters to obtain spongy lead and displaced liquid, and displaced liquid is regulated the pH value up to not producing precipitation with sodium hydroxide, and liquid can return branch splicer preface behind the heavy iron; Lead separated slag adds sodium hydroxide 45g and SODIUMNITRATE 7.5g, mixes; 500 ℃ of roasting 1h; Roasting sand is placed 36h in air, add entry 500g and stir 1h, filter and obtain sodium stannate.Lead recovery 92.5%, the tin rate of recovery 97.1%.

Claims (2)

1, a kind of silver separating residue of copper anode slime of circuit board reclaims the method for slicker solder, it is characterized in that: divide silver-colored slag, water, hydrochloric acid, calcium chloride and sodium-chlor to stir 0.5~2.0h down in 75~95 ℃, wherein the amount of water, hydrochloric acid, calcium chloride and sodium-chlor is respectively: water: divide silver-colored slag=5: 1~10: 1, concentration of hydrochloric acid is 50~100g/L, calcium chloride concentration is 100~300g/L, and sodium chloride concentration is 150~300g/L; Filtration obtains plumbous liquid of branch and lead separated slag, divides plumbous liquid to replace with excess iron powder, filters to obtain spongy lead and displaced liquid, and displaced liquid is regulated the pH value up to not producing precipitation with sodium hydroxide, and liquid returns branch splicer preface behind the heavy iron; Lead separated slag adds sodium hydroxide and SODIUMNITRATE mixes sodium hydroxide: divide silver-colored slag=1: 10~3: 10, SODIUMNITRATE: divide silver-colored slag=1: 100~5: 100; In 350~500 ℃ of roasting 1.0~3.0h; Roasting sand is placed 24~48h in air, add entry and carry out water logging, stir 0.5~1.0h, filter and obtain sodium stannate.
2, silver separating residue of copper anode slime of circuit board as claimed in claim 1 reclaims the method for slicker solder, it is characterized in that the amount that adds entry in the water logging process is: water: divide silver-colored slag=3: 1~5: 1.
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CN101824546A (en) * 2010-05-20 2010-09-08 北京科技大学 Method for recovering silver from lead-separating liquid of silver-separating residue of copper anode slime
CN101831553A (en) * 2010-05-28 2010-09-15 北京科技大学 Method for green recovery of waste circuit boards by cyanide-free full-wet whole set process
CN101928958A (en) * 2010-07-21 2010-12-29 北京科技大学 Method and device for recovering metal tin from lead separated slag of copper anode slime
CN101768668B (en) * 2010-01-07 2011-07-20 株洲冶炼集团股份有限公司 Method for comprehensive recovery of lead and tin from alkaline refining slag of lead
CN102674437A (en) * 2012-05-25 2012-09-19 中南大学 Method for deeply purifying sodium stannate liquor
CN102776386A (en) * 2012-07-20 2012-11-14 北京科技大学 Method for recycling stannic oxide from tin-containing lead slag
CN102943180A (en) * 2012-07-20 2013-02-27 北京科技大学 Method for recycling gold and silver from silver separating residues of copper anode slime
CN103088218A (en) * 2013-01-16 2013-05-08 西北师范大学 Method for extracting silver and lead from smelting slag generated by pyrogenic process treatment of copper anode mud
CN103305699A (en) * 2013-06-20 2013-09-18 山东恒邦冶炼股份有限公司 Method for extracting platinum-palladium out of copper anode mud
CN103757439A (en) * 2014-01-20 2014-04-30 北京矿冶研究总院 Method for recovering antimony and lead from antimony-lead-containing complex sulfide ore
CN103937982A (en) * 2014-03-25 2014-07-23 陕西锌业有限公司 Method for extracting lead and silver from zinc oxide leached residues through wet method technology
CN103966451A (en) * 2014-05-23 2014-08-06 江西理工大学 Method for preparing sodium stannate from copper anode mud silver separation residue
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
CN105132676A (en) * 2015-09-11 2015-12-09 吕志芳 Hydrometallurgy matched equipment capable of cyclically using water
CN106566931A (en) * 2016-11-03 2017-04-19 贵州宏达环保科技有限公司 Wet process lead smelting method with iron as circulation substance
CN106967884A (en) * 2017-03-20 2017-07-21 北矿力澜科技咨询(北京)有限公司 A kind of method of silver separating residue of copper anode slime step by step arithmetic
CN107345274A (en) * 2017-06-06 2017-11-14 云南云铜锌业股份有限公司 It is a kind of that lead, silver, the method for indium are reclaimed from lead smelting gas
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CN110453073A (en) * 2019-08-14 2019-11-15 河南中原黄金冶炼厂有限责任公司 A method of recycling lead from copper pyrometallurgy flue dust acid leaching residue
CN110904338A (en) * 2019-12-10 2020-03-24 暨南大学 Method for selectively recovering tin or lead from waste circuit board
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CN111733327A (en) * 2020-07-07 2020-10-02 中国恩菲工程技术有限公司 Recovery method and recovery device for valuable metals in scrap copper electrolysis anode mud
CN112981132A (en) * 2019-12-15 2021-06-18 湖南省桂阳银星有色冶炼有限公司 Lead bullion electrolytic refining method beneficial to cadmium removal
CN114807623A (en) * 2022-03-10 2022-07-29 金川集团股份有限公司 Method for removing tellurium from copper anode mud leaching slag
CN114990338A (en) * 2022-05-07 2022-09-02 江西铜业技术研究院有限公司 Method for efficiently extracting tin from silver separating residues of copper anode slime
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CN101824546A (en) * 2010-05-20 2010-09-08 北京科技大学 Method for recovering silver from lead-separating liquid of silver-separating residue of copper anode slime
US9689055B2 (en) 2010-05-28 2017-06-27 University Of Science And Technology Beijing Complete non-cyanogens wet process for green recycling of waste printed circuit board
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CN114807623A (en) * 2022-03-10 2022-07-29 金川集团股份有限公司 Method for removing tellurium from copper anode mud leaching slag
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