CN110484736A - A method of copper removal is purified for zinc sulfate leaching liquid - Google Patents

A method of copper removal is purified for zinc sulfate leaching liquid Download PDF

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Publication number
CN110484736A
CN110484736A CN201910932712.XA CN201910932712A CN110484736A CN 110484736 A CN110484736 A CN 110484736A CN 201910932712 A CN201910932712 A CN 201910932712A CN 110484736 A CN110484736 A CN 110484736A
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copper
zinc sulfate
leachate
liquid
tin
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CN201910932712.XA
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CN110484736B (en
Inventor
肖驰名
肖之晔
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Hunan Renfa Material Technology Co Ltd
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Hunan Renfa Material Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0084—Treating solutions
    • C22B15/0089—Treating solutions by chemical methods
    • C22B15/0091—Treating solutions by chemical methods by cementation
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/32—Refining zinc
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

A method of copper removal being purified for zinc sulfate leaching liquid, tin-coated copper waste garrulous material is added in zinc sulfate leaching liquid, after completion of the reaction, is separated by solid-liquid separation, obtains leached mud, leachate and replacement slag；Air or oxygen is blasted into leachate, so that Sn2+It is oxidized to Sn4+；The pH value of leachate is adjusted again to 4.5-5, so that the Sn in leachate4+It is converted into sediment, is then separated by solid-liquid separation, liquid and stanniferous filter residue after copper removal are obtained.Tin-coated copper waste garrulous material is derived from the solid wastes such as " city mineral products " or electronic waste in the present invention, it is directly used in zinc sulfate leaching liquid purification copper removal, antimony, iron, arsenic, products therefrom (filter residue) first is that copper sponge, it can be directly used for pyrometallurgy of the cupric electrolysis with liquid or copper, resource, benefits of environment and economy are obvious.

Description

A method of copper removal is purified for zinc sulfate leaching liquid
Technical field
The present invention relates to a kind of methods more particularly to non-ferrous metal hydrometallurgy for zinc sulfate leaching liquid purification copper removal The method of middle zinc sulfate leaching liquid purification copper removal and tin-coated copper waste garrulous material resource utilization.
Background technique
In non-ferrous extractive metallurgy, zinc calcine or other material containing zincs (such as containing the flue dust of zinc oxide) after middle leaching, Neutral leachate is generated, there are many impurity, such as Cu, As, Fe, Sb, Cd, Co, Ni for the leachate, these impurity are to sulfuric acid The production of zinc or zinc electrolysis deposition process have high risks, it is necessary to by solution purification, the harmful impurity of institute be removed, output is closed Lattice scavenging solution can just be sent to zinc electrolysis bath, or for producing sulfuric acid zinc chemical product.
Currently, both at home and abroad purifying zinc sulfate solution remove wherein copper, iron, arsenic, stilba matter method, the process generallyd use It is:
1. control terminal acidity makes Fe in leaching process3+Complete hydrolysis precipitating, while removing arsenic, antimony and partial impurities；
2. hydrogen peroxide (H is added into leachate in advance2O2), by Fe2+It is completely oxidized to Fe3+, then PH is adjusted with lime white Value, makes Fe3+Complete hydrolysis precipitating, while removing arsenic, antimony and partial impurities；
3. after removing arsenic, iron, antimony and partial impurities, removing the copper in solution of zinc sulfate with zinc dust precipitation.
But the above method, first is that method 1. in, it is understood that there may be Fe2+It is converted to Fe3+Not exclusively, thus de-ferrous effect not It is ideal；Second is that process flow is long, uneconomical except iron, arsenic, antimony and copper removal substep carry out；Third is that simple substance zinc produces using zinc powder copper removal Product need to be rationalized in terms of being converted into the intermediate product of zinc, cost and benefit.Therefore, a kind of short route, low cost, resource are established The purification method of circular form, necessitates.
The modern industries such as electronics, communication, photoelectricity, audio-visual largely use tinned wird, tin plating copper material and tin plating copper piece, are plating In the production and use process of tin product, it is inevitably generated a large amount of tin-coated copper waste garrulous material, including useless tinned wire, electronics Foot, hot tinning production can also generate hot dip scruff.Stanniferous about 1~3wt% or so in tin plating waste garrulous material, copper content is on the left side 98wt% The right side, the stanniferous about 30~90wt% of hot dip scruff have very high recycling value.But the physical and chemical individual character based on tin element is extracted In metallurgical process, copper and tin is difficult to separate.
Currently, mainly useless using pyrogenic process, pyrogenic process electrolysis method, electrochemical process and leaching and displacement method recycling tin-coated copper both at home and abroad Particle.But above method energy consumption height, high production cost, process route are long, because adding other reagents, can also cause to copper centainly Loss, method process is relatively isolated, can not generate Synergy.
Summary of the invention
It is an object of the invention to based on prior art technology there are the problem of, a kind of purification of zinc sulfate leaching liquid is provided and is removed Copper and tin-coated copper waste garrulous material copper and tin are located away from one, mutually beneficial promotion, while realizing that copper and tin separation is removed with zinc sulfate leaching liquid purification The method of copper, to further realize, short technique, small investment, equipment is simple, resources circulation and extraction of economic circulation, green low-carbon Metallurgical production mode.
A method of copper removal being purified for zinc sulfate leaching liquid, is included the following steps:
S1, tin-coated copper waste garrulous material is added in zinc sulfate leaching liquid, after completion of the reaction, is separated by solid-liquid separation, acquisition leached mud, Leachate and replacement slag；
Wherein, the surface of tin-coated copper waste garrulous material is without covering；The leached mud is mainly made of detin copper waste garrulous material, the displacement Slag is mainly made of copper sponge；
Air or oxygen is blasted in S2, the leachate obtained into S1, so that Sn2+It is oxidized to Sn4+；Leachate is adjusted again PH value is to 4.5-5, so that the Sn in leachate4+It is converted into sediment, is then separated by solid-liquid separation, liquid and stanniferous after copper removal is obtained Filter residue.
Further, in S1, first by zinc sulfate leaching liquid inject purification leaching tanks in, be then added portionwise tin-coated copper give up it is broken Material is separated by solid-liquid separation after completion of the reaction, obtains leached mud, leachate and replacement slag.Generally, the Leach reaction time is 35- 40min。
In S1, zinc sulfate leaching liquid includes Zn50-500g/L, Cu0.5-5g/L, Fe0-5g/L, As0-5g/L, Sb0-5g/ L。
In S1, in the tin-coated copper waste garrulous material, Theil indices are 1~3wt%.The additive amount of tin-coated copper waste garrulous material can be according to sulphur Cu in sour zinc solution2+Theil indices COMPREHENSIVE CALCULATING obtains in content and solution of zinc sulfate total amount, tin-coated copper waste garrulous material.
In the present invention, surface can be understood as the wireless skin in surface or the covering of other surfaces without the tin-coated copper waste garrulous material of covering The exposed tin-coated copper waste garrulous material of object, further, in tin-coated copper waste garrulous material, simple substance tin is distributed in the surface layer of tin-coated copper waste garrulous material.
Further, the tin-coated copper waste garrulous material includes in tinned wird, tin plating copper material, tin plating copper piece and hot dip scruff One or more, the tin plating copper piece include tin-coated copper electronic foot.
In general, the precipitate granularity of copper is minimum, and size is smaller than tin-coated copper waste garrulous material or detin copper waste garrulous material when leaching Several orders of magnitude, thus the precipitate of copper and the copper waste garrulous material after detin can be easily separated, so be easy in the separation of solid and liquid of S1 Separation obtains two kinds of solid formations of leached mud and replacement slag.
In S1, the temperature for controlling zinc sulfate leaching liquid is 50-60 DEG C.
In S1, zinc sulfate leaching liquid is that zinc sulfate leaches stoste, alternatively, the solution that dilution obtains.
In S1, when zinc sulfate leaching liquid blue is taken off, end of reaction is indicated；Alternatively, zinc sulfate leaching liquid is taken to stand, detect Cu in supernatant2+Concentration, work as Cu2+Concentration be lower than preset value when, indicate end of reaction.
Further, the preset value is 0.01-0.05 g/L, specifically can be true according to the purification demand of zinc sulfate leaching liquid It is fixed.
In S2, the time for blasting air is 55-65min.
In S2, the pH value of leachate is adjusted by the way that lime is added.Preferably, it is directly added into white lime.
In S2, when being separated by solid-liquid separation to leachate, realized by sheet frame diaphragm filter press.
After S2, the stanniferous filter residue is washed, obtains purification slag.
Further, directly use water as cleansing medium the washing of leached mud, filter residue, and wash water can mutual circulation It uses, insufficient section can additional supplement water.
In the present invention, replacement slag is mainly newly-generated copper sponge, and copper sponge granularity therein is small, and activity is high, mainly by Cu and O is constituted, and can send metallurgy of copper system, and copper sponge is integrally in pureed, is easy and relatively large sized detin copper waste garrulous material point From；Leached mud is mainly detin copper waste garrulous material, can return to copper metallurgy industry and carries out copper recovery processing；Liquid impurity content after copper removal It is low, next work flow can be sent；Filter residue and purification slag are tin, arsenic, antimony, the scum based on tin element, can send tin metallurgical system It carries out valuable element and carries out valuable element synthetical recovery.
Key reaction principle of the invention is as follows: leaching in process, the metallic tin displacement zinc sulfate in tin-coated copper waste garrulous material Cu in leachate2+, generate Sn2+With copper sponge (granularity is minimum)；In neutralization precipitation process, air is blasted, so that Sn2+By oxygen It is melted into Sn4+, there are Fe2+When, Fe2+It is oxidized to Fe3+, when adjustment pH value is to 4.5~5, Sn in solution4+Hydrolysis generates α- SnO2·H2O is then changed into the β-(SnO with rock-steady structure2·H2O)5Colloid, β-(SnO2·H2O)5Colloid trapping solution The ion or hydrolysate that the elements such as middle As, Sb, Fe are formed generate co-precipitation, meanwhile, the addition of lime can improve precipitating The performance of object filters convenient for solid-liquor separation.
Compared with prior art, the present invention has the advantage that
1) tin-coated copper waste garrulous material is derived from the solid wastes such as " city mineral products " or electronic waste, is directly used in zinc sulfate leaching liquid purification and removes Copper, antimony, iron, arsenic, products therefrom (filter residue) first is that copper sponge, can be directly used for pyrometallurgy of the cupric electrolysis with liquid or copper, money Source, benefits of environment and economy are obvious.
2) technical process closed water circuit, filter residue return metallurgy of copper and tin smelting system respectively, non-wastewater discharge, without waste It generates, impurity component is as valuable element synthetical recovery.
3) same process, zinc sulfate leaching liquid purify the impurity such as copper removal and purification arsenic removal, iron, antimony and complete together, technique stream Journey is simple, consumes low.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the invention.
Fig. 2 is the photo in kind of leached mud in embodiment 1.
Specific embodiment
Following description describe optional embodiment of the invention with instruct those of ordinary skill in the art how to implement and It is bright to reproduce this.
Embodiment 1
It is the zinc sulfate of Zn150.70g/L, Cu0.95g/L, Fe0.15g/L, As0.25g/L, Sb0.71g/L by chemical component Leachate after being purified with excessive tin-coated copper waste garrulous material by Fig. 1 process flow, obtains copper removal zinc sulfate leaching liquid (Cu0.32g/ L, As0.05 g/L, Sb0.03g/L, Fe0.04g/L).Detin copper waste garrulous material is apparently without residual tin, the stanniferous < 0.3% of copper sponge, only Slugging contains Sn18.72%, As1.57%, Fe1.4%, and Cu content is lower than 0.2% in purification slag；
Wherein, each percentage indicates mass percentage.
Embodiment 2
The zinc sulfate that chemical component is Zn140.57g/L, Cu1.17g/L, As1.8g/L, Sb1.27g/L, Fe1.3g/L is taken to leach Liquid after purifying by Fig. 1 process flow, obtains copper removal zinc sulfate leaching liquid (Cu0.08 g/ with excessive tin plating copper scrap electronic foot L, As0.07g/L, Sb0.03g/L, Fe0.01g/L).Detin copper scrap electronic foot detin is thorough, the stanniferous < 0.3% of copper sponge, purification Slag contains Sn13.77%, As1.0%, Sb0.83%, and purification slag Cu content is lower than 0.2%；
Wherein, each percentage indicates mass percentage.
Embodiment 3
Taking chemical component is the zinc sulfate of Zn137.07g/L, Cu1.03g/L, Sb0.97g/L, As1.12g/L, Fe1.12 g/L Leachate after purifying by Fig. 1 process flow, obtains copper removal zinc sulfate leaching liquid (Cu0.11g/ with excessive tin plating copper scrap line L, As0.009 g/L, Sb0.27g/L, Fe0.51g/L), detin copper scrap line is without apparent residual tin, the stanniferous < 0.3% of copper sponge, purification Slag contains Sn17.78%, As0.98%, Sb0.57%, Fe1.7%, and purification slag Cu content is lower than 0.3%；
Wherein, each percentage indicates mass percentage.
The content that above-described embodiment illustrates should be understood as that these embodiments are only used for being illustrated more clearly that the present invention, without For limiting the scope of the invention, after the present invention has been read, those skilled in the art are to various equivalent forms of the invention Modification each fall within the application range as defined in the appended claims.

Claims (9)

1. a kind of method for zinc sulfate leaching liquid purification copper removal, which comprises the steps of:
S1, tin-coated copper waste garrulous material is added in zinc sulfate leaching liquid, after completion of the reaction, is separated by solid-liquid separation, acquisition leached mud, Leachate and replacement slag；
Wherein, the surface of tin-coated copper waste garrulous material is without covering；The leached mud is mainly made of detin copper waste garrulous material, the displacement Slag is mainly made of copper sponge；
Air or oxygen is blasted in S2, the leachate obtained into S1, so that Sn2+It is oxidized to Sn4+；The pH of leachate is adjusted again Value is to 4.5-5, so that the Sn in leachate4+It is converted into sediment, is then separated by solid-liquid separation, liquid and stanniferous filter after copper removal are obtained Slag.
2. the method according to claim 1, wherein in S1, zinc sulfate leaching liquid include Zn50-500g/L, Cu0.5-5g/L、Fe0-5g/L、As0 -5g/L、Sb0-5g/L。
3. the method according to claim 1, wherein in S1, in the tin-coated copper waste garrulous material, Theil indices are 1~ 3wt%。
4. the method according to claim 1, wherein the temperature for controlling zinc sulfate leaching liquid is 50-60 in S1 ℃。
5. the method according to claim 1, wherein when zinc sulfate leaching liquid blue is taken off, indicating reaction in S1 It finishes；Alternatively, zinc sulfate leaching liquid is taken to stand, Cu in supernatant is detected2+Concentration, work as Cu2+Concentration be lower than preset value when, Indicate end of reaction.
6. the method according to claim 1, wherein the time for blasting air is 55-65min in S2.
7. method according to claim 1-6, which is characterized in that in S2, adjust leachate by the way that lime is added PH value.
8. method according to claim 1-6, which is characterized in that in S2, when being separated by solid-liquid separation to leachate, It is realized by sheet frame diaphragm filter press.
9. method according to claim 1-6, which is characterized in that after S2, washed to the stanniferous filter residue It washs, obtains purification slag.
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CN1530452A (en) * 2003-03-14 2004-09-22 中国有色工程设计研究总院 Method and apparatus for removing copper, cadmium and cobalt from zinc sulfate solution
CN102002594A (en) * 2010-12-17 2011-04-06 赖小洪 Method for recycling tin
CN102409180A (en) * 2011-11-02 2012-04-11 郴州丰越环保科技有限公司 Metallurgical process for recovering metal copper, lead, zinc and tin from copper refining waste slag
WO2012089840A2 (en) * 2010-12-31 2012-07-05 University Of Tartu THE METHOD OF PREPARATION OF NANOCOLLOIDAL SnO2 WATERSOL AND ITS USES
CN102676820A (en) * 2012-06-08 2012-09-19 大兴安岭云冶矿业开发有限公司 Treatment method of zinc sulfate leach solution
CN103014355A (en) * 2012-12-13 2013-04-03 马永涛 Multi-metal comprehensive recycling process for copper smelting ash
CN107779599A (en) * 2017-11-07 2018-03-09 安徽工业大学 A kind of preparation of new rare precious metal complex reducing agent and its application method
CN108165751A (en) * 2017-12-29 2018-06-15 中国葛洲坝集团绿园科技有限公司 The method and system of recycling valuable metal are smelted in a kind of collaboration from waste printed circuit board, copper scap and copper-containing residue
CN110241308A (en) * 2019-04-08 2019-09-17 无锡市安盛再生资源有限公司 The recovery method and system of tin metal in a kind of nitric acid type tin-stripping wastewater

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5399336A (en) * 1990-06-29 1995-03-21 Rhone-Poulenc Chimie Stannozeosilite/zirconozeosilite zeolites and catalytic hydroxylation of phenolics therewith
US20030073385A1 (en) * 2001-10-12 2003-04-17 International Business Machines Corporation Self-cleaning colloidal slurry composition and process for finishing a surface of a substrate
CN1530452A (en) * 2003-03-14 2004-09-22 中国有色工程设计研究总院 Method and apparatus for removing copper, cadmium and cobalt from zinc sulfate solution
CN102002594A (en) * 2010-12-17 2011-04-06 赖小洪 Method for recycling tin
WO2012089840A2 (en) * 2010-12-31 2012-07-05 University Of Tartu THE METHOD OF PREPARATION OF NANOCOLLOIDAL SnO2 WATERSOL AND ITS USES
CN102409180A (en) * 2011-11-02 2012-04-11 郴州丰越环保科技有限公司 Metallurgical process for recovering metal copper, lead, zinc and tin from copper refining waste slag
CN102676820A (en) * 2012-06-08 2012-09-19 大兴安岭云冶矿业开发有限公司 Treatment method of zinc sulfate leach solution
CN103014355A (en) * 2012-12-13 2013-04-03 马永涛 Multi-metal comprehensive recycling process for copper smelting ash
CN107779599A (en) * 2017-11-07 2018-03-09 安徽工业大学 A kind of preparation of new rare precious metal complex reducing agent and its application method
CN108165751A (en) * 2017-12-29 2018-06-15 中国葛洲坝集团绿园科技有限公司 The method and system of recycling valuable metal are smelted in a kind of collaboration from waste printed circuit board, copper scap and copper-containing residue
CN110241308A (en) * 2019-04-08 2019-09-17 无锡市安盛再生资源有限公司 The recovery method and system of tin metal in a kind of nitric acid type tin-stripping wastewater

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