CN1062930A - The recovery method of copper in the spent etching solution - Google Patents

The recovery method of copper in the spent etching solution Download PDF

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Publication number
CN1062930A
CN1062930A CN91100122A CN91100122A CN1062930A CN 1062930 A CN1062930 A CN 1062930A CN 91100122 A CN91100122 A CN 91100122A CN 91100122 A CN91100122 A CN 91100122A CN 1062930 A CN1062930 A CN 1062930A
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China
Prior art keywords
copper
solution
iron filings
metathesis
reaction
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Pending
Application number
CN91100122A
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Chinese (zh)
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景焕德
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Individual
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Individual
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Priority to CN91100122A priority Critical patent/CN1062930A/en
Publication of CN1062930A publication Critical patent/CN1062930A/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

A kind of method that the copper in alkaline spent etching solution and the acidic waste etching liquid can be reclaimed simultaneously.Method of the present invention is, after two kinds of spent etching solutions are mixed, with hydrochloric acid the pH value of mixed solution is adjusted into 1~4, dilute with water makes cupric chloride concentration be controlled at 30~100 grams per liters again, carries out replacement(metathesis)reaction with iron filings, can obtain copper content is more than 95%, the copper powder of granularity more than 320 orders.This copper powder can directly be used for producing Red copper oxide.

Description

The recovery method of copper in the spent etching solution
Involved in the present invention is the method that the copper in alkaline spent etching solution and the acidic waste etching liquid is reclaimed simultaneously with replacement(metathesis)reaction.
Alkalescence and acidic waste etching liquid all are the waste liquids of making printed-wiring board (PWB) in the electronic industry.Mainly contain ammoniacal liquor, ammonia chloride and cupric chloride in the alkalescence spent etching solution, copper content is 120~150 grams per liters, mainly is cupric chloride in the acidic waste etching liquid, and copper content is 90~130 grams per liters.At present, the method for industrial processing waste cuprous chloride solution is: through twice neutralization reaction, cupric chloride is become copper sulfate.The application Chinese patent of having found, application number are 86108929 invention, adopt redox reaction, and cupric chloride is reduced to the blister copper powder, carry out melting again and smelt that to make copper content be 97~98% copper ingot.Above-mentioned two kinds of methods only relate to the processing of acid copper chloride waste fluid, and first kind can only obtain a kind of mantoquita, and second kind also needs pyrotic smelting, just can obtain purer copper ingot.
Purpose of the present invention just provides a kind of method, the copper in alkalescence and the acidic waste etching liquid can be reclaimed simultaneously, the gained copper powder do not need pyrotic smelting can be directly as the raw material of Red copper oxide.
Method of the present invention is: saturated acidic waste etching liquid is added in the corrosion-resistant container, more undersaturated acidic waste etching liquid is added, stir, the precipitation in the saturated spent etching solution is dissolved fully.Thin up stirs then, adds alkaline spent etching solution more while stirring, add-on be two kinds of acidic waste etching liquid weight 1/3rd to half.Add, measure the acid alkalescence of solution, if alkalescence or neutral need add hydrochloric acid adjustment, make whole mixed solution be acid, the pH value of general mixed solution will be adjusted into 1~4, if with the pH value of mixed solution be adjusted into 2~3 the most desirable.Add water again in solution, the concentration of cupric chloride drops to 30~100 grams per liters in mixed solution, preferably till 50~75 grams per liters.After mixed solution configures, add iron filings in mixed solution, the iron filings of adding should be excessive, and the zone of oxidation on iron filings surface will be removed in advance.After iron filings entered solution, replacement(metathesis)reaction began immediately, every 10~15 seconds, took out iron filings and beat, and will shake attached to its surperficial copper powder.When solution temperature rose to 25~30 ℃, speed of response was accelerated, and every 5~10 seconds, took out iron filings and beat once.When solution temperature rose to 50~55 ℃, 80% copper had been displaced in the solution, and speed of response slows down, and at this moment attached to the copper show bubble on iron filings surface, needn't take out iron filings and beat, and only needed every 5~10 minutes, iron filings was stirred several following.When whole solution became clear, reaction finished, and the copper in the solution 98% or more has been displaced, and sank to container bottom with the form of copper powder.Take out remaining iron filings, solution can be recycled or discharges with in the unslaked lime and back.The copper powder copper content that copper powder is cleaned, dries, obtained with clear water is more than 95%, and granularity can directly be used for producing Red copper oxide more than 320 orders.
Principal reaction of the present invention is:
Embodiment:
In corrosion-resistant groove, add 200 kilograms of saturated acidic waste etching liquids, add 500 kilograms of undersaturated acidic waste etching liquids again, stir, after the precipitation in the saturated spent etching solution is dissolved fully, after adding 1 ton in water and stirring, add 400 kilograms of alkaline spent etching solutions, stir, survey Property of Acid and Alkali of Solution, add small amount of hydrochloric acid the pH value of solution is transferred between 2~3 near neutral, in solution, add water again, measure the concentration of cupric chloride in the solution, drop to about 60 grams per liters, stop to add water up to its concentration.Solution allocation finishes, and adds 220 kilograms of iron filings in solution.Beginning, every 10~15 seconds, taking stainless steel fork that iron filings are chosen liquid level beats with wooden stick, when solution temperature is raised to more than 25 ℃,, iron filings is chosen beat every 5~10 seconds, copper powder attached to the iron filings surface all falls into bottom land, when solution temperature is raised to 50~55 ℃, at this moment needn't chooses iron filings and beat, every 5~10 minutes, stir several iron filings down with steel fork, foamed copper and iron filings are separated, and when entire reaction was carried out about 90 minutes, solution was the clear shape, solution is discharged in another corrosion-resistant groove, the copper powder taking-up water of bottom land is washed down, and oven dry obtains 180 kilograms of the thin copper powder of granularity more than 320 orders.

Claims (3)

1, a kind of method that the copper in alkaline spent etching solution and the acidic waste etching liquid can be reclaimed simultaneously, make raw material with iron filings, it is characterized in that, elder generation's dilute with water acidic waste etching liquid adds alkaline spent etching solution again, with hydrochloric acid the pH value of mixed solution is adjusted to 1~4, thin up again, make that cupric chloride concentration is controlled at 30~100 grams per liters in the solution, add iron filings, obtain copper content at the copper powder more than 95% through replacement(metathesis)reaction.
2, method according to claim 1 is characterized in that, earlier the pH value of mixed solution is adjusted to 2~3, adds water then with cupric chloride concentration dilution to 50 in the solution~75 grams per liters, carries out replacement(metathesis)reaction again.
3, method according to claim 1 is characterized in that, in the replacement(metathesis)reaction process, every 5~15 seconds, the iron filings taking-up is beaten, and copper powder attached thereto is come off.
CN91100122A 1991-01-04 1991-01-04 The recovery method of copper in the spent etching solution Pending CN1062930A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN91100122A CN1062930A (en) 1991-01-04 1991-01-04 The recovery method of copper in the spent etching solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN91100122A CN1062930A (en) 1991-01-04 1991-01-04 The recovery method of copper in the spent etching solution

Publications (1)

Publication Number Publication Date
CN1062930A true CN1062930A (en) 1992-07-22

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Application Number Title Priority Date Filing Date
CN91100122A Pending CN1062930A (en) 1991-01-04 1991-01-04 The recovery method of copper in the spent etching solution

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CN (1) CN1062930A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102240814A (en) * 2010-05-12 2011-11-16 陈卓贤 Method for preparing superfine copper powder by utilizing environmentally-friendly recycled circuit board etching waste liquor
CN102887536A (en) * 2012-10-12 2013-01-23 金川集团股份有限公司 Method for comprehensively utilizing high-acid low-copper solution
CN102899493A (en) * 2011-07-26 2013-01-30 新疆新鑫矿业股份有限公司阜康冶炼厂 Method for recovering valuable metals from chlorine leaching displacement tailing solution in production of precious metals
CN104499003A (en) * 2014-11-13 2015-04-08 黄石市英柯有色金属有限公司 Method for extracting metal in aqueous solution
CN107354461A (en) * 2017-09-13 2017-11-17 田成 A kind of printed circuit board acidic etching waste liquor process for regenerating, recovering and reutilizing
CN108746602A (en) * 2018-05-26 2018-11-06 烟台大学 A method of preparing copper-clad iron powder using copper-containing wastewater

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102240814A (en) * 2010-05-12 2011-11-16 陈卓贤 Method for preparing superfine copper powder by utilizing environmentally-friendly recycled circuit board etching waste liquor
CN102899493A (en) * 2011-07-26 2013-01-30 新疆新鑫矿业股份有限公司阜康冶炼厂 Method for recovering valuable metals from chlorine leaching displacement tailing solution in production of precious metals
CN102887536A (en) * 2012-10-12 2013-01-23 金川集团股份有限公司 Method for comprehensively utilizing high-acid low-copper solution
CN102887536B (en) * 2012-10-12 2014-06-25 金川集团股份有限公司 Method for comprehensively utilizing high-acid low-copper solution
CN104499003A (en) * 2014-11-13 2015-04-08 黄石市英柯有色金属有限公司 Method for extracting metal in aqueous solution
CN107354461A (en) * 2017-09-13 2017-11-17 田成 A kind of printed circuit board acidic etching waste liquor process for regenerating, recovering and reutilizing
CN108746602A (en) * 2018-05-26 2018-11-06 烟台大学 A method of preparing copper-clad iron powder using copper-containing wastewater

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