CN107400904A - The preparation method of copper electrolyte removing impurities agent and the method for copper electrolyte removing impurities - Google Patents

The preparation method of copper electrolyte removing impurities agent and the method for copper electrolyte removing impurities Download PDF

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Publication number
CN107400904A
CN107400904A CN201710681460.9A CN201710681460A CN107400904A CN 107400904 A CN107400904 A CN 107400904A CN 201710681460 A CN201710681460 A CN 201710681460A CN 107400904 A CN107400904 A CN 107400904A
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removing impurities
agent
electrolyte
preparation
copper electrolyte
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CN107400904B (en
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宁万涛
谢祥添
余华清
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Yanggu Xiangguang Copper Co Ltd
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Yanggu Xiangguang Copper Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06Operating or servicing
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00Obtaining copper
    • C22B15/0063Hydrometallurgy
    • C22B15/0084Treating solutions
    • C22B15/0089Treating solutions by chemical methods
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/12Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention provides a kind of preparation method of copper electrolyte removing impurities agent, comprise the following steps:Dynamic wave mud and stibium trioxide are used into sulfuric acid washing, obtain mixture;The mixture is aoxidized in the presence of oxidant, obtains copper electrolyte removing impurities agent.Present invention also provides a kind of method that removing impurities agent prepared by carries out copper electrolyte removing impurities.Electrolyte removing impurities method provided by the invention, the removal efficiency of antimony are up to 91.34%, and the removal efficiency of bismuth is up to 95.48%.The present invention takes full advantage of intermediate material dynamic wave mud and adds stibium trioxide to be configured to the removing impurities that removing impurities agent carries out electrolyte, increase small investment, positive effect, antimony bismuth can be reclaimed by carrying out processing after the removing impurities agent removing impurities of gained, whole process technique is simple, easily realizes industrialization, and impurity-removing rate is high, the composition of electrolyte is not limited, strong applicability.

Description

The preparation method of copper electrolyte removing impurities agent and the method for copper electrolyte removing impurities
Technical field
The present invention relates to cleaning copper electrolyte technical field, more particularly to the preparation method of copper electrolyte removing impurities agent and copper electricity The method for solving liquid removing impurities.
Background technology
Arsenic antimony bismuth in electrolyte influences very big, arsenic antimony bismuth because chemical potential is close with copper, therefore on the quality of electrolytic copper Open circuit turn into inevitable, mainly have electrodeposition removing impurities, extraction or ion exchange and three kinds of impurity-removing methods of chemical precipitation at present.
The country generally uses electrodeposition purification and impurity removal, wherein being divided into the continuous removing impurities of continuous removing impurities, parallel circulating, eddy flow again Removing impurities etc., but this method power consumption is high, cycle length, equipment investment is big, and factory building takes up an area big;Ion exchange is because the dense and high arsenic of peracid It is selectively all poor, although domestic also have the document that antimony bismuth is taken off using ion exchange, still there is no an enterprise in industry Industrialization, wherein problem is well imagined;The tail washings of extraction is difficult, influences environment.More than being based on, a kind of suitable method is found Antimony bismuth impurity in inexpensive, efficient removing electrolyte can give following cleaning copper electrolyte to expand direction.
The content of the invention
Present invention solves the technical problem that being the preparation method for providing copper electrolyte removing impurities agent, copper prepared by the application is electric The agent of solution liquid removing impurities is used to remove antimony, the bismuth in copper electrolyte, and cost is low and removal efficiency is high.
In view of this, this application provides a kind of preparation method of copper electrolyte removing impurities agent, comprise the following steps:
Dynamic wave mud and stibium trioxide are used into sulfuric acid washing, obtain mixture;
The mixture is aoxidized in the presence of oxidant, obtains copper electrolyte removing impurities agent.
Preferably, the concentration of sulfuric acid is 200~250g/L, and the liquid-solid ratio of the sulfuric acid and before processing material is 3:1, it is described Before processing material is dynamic wave mud and stibium trioxide.
Preferably, the mass ratio of the stibium trioxide and the dynamic wave mud is 1:(1~5).
Preferably, the oxidant is hydrogen peroxide, and the addition of the hydrogen peroxide is the dynamic wave mud and the stibium trioxide 1~2 times of gross mass.
Preferably, the temperature of the pickling is 70~80 DEG C, and the time is 0.5~1h;The time of the oxidation is 1~2h.
Present invention also provides a kind of method of copper electrolyte removing impurities, including:
Electrolyte is mixed with removing impurities agent and carries out removing impurities, obtains removing impurities electrolyte;The removing impurities agent is described in such scheme Preparation method prepared by removing impurities agent.
Preferably, the electrolyte and the liquid-solid ratio of removing impurities agent are (10~15):1.
Preferably, the temperature of the removing impurities is 60~70 DEG C, and the time is 1.5~2h.
This application provides a kind of preparation method of copper electrolyte removing impurities agent, and it uses dynamic wave mud with stibium trioxide as removing impurities The primary raw material of agent, above two raw material obtain removing impurities agent after overpickling, oxidation;In dynamic wave mud during pickling The generation such as lead oxide, bismuth oxide and antimonial lead sulfate, bismuth sulfate, alkali formula antimony sulfate and alkali formula bismuth sulfate etc., in addition Some soluble impurities, which are dissolved into acid, to be removed, and stibium trioxide part is oxidized to antimony pentavalent compound;In copper electrolyte removing impurities, Extremely tiny antimony, the bismuth in electrolyte of the particle of lead sulfate in cleaner has a suction-operated, and the hydrate of quinquevalence antimony with Trivalent antimony, bismuth reaction in electrolyte, the complex of the different valence state of bismuth antimonate and antimony is generated, so as to which antimony, bismuth are removed;Alkali formula The self cleaning of antimony sulfate and alkali formula bismuth sulfate further removes the impurity in electrolyte;Dynamic wave mud belongs to waste simultaneously Recycling, therefore, the cost of the copper electrolyte removing impurities agent of the application is relatively low, and antimony, bismuth removal efficiency are high.
Brief description of the drawings
Fig. 1 is the preparation method and removing impurities method flow schematic diagram of copper electrolyte removing impurities agent of the present invention.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still It should be appreciated that these descriptions are simply further explanation the features and advantages of the present invention, rather than to the claims in the present invention Limitation.
It is high for antimony bismuth impurity removal cost in copper electrolyte in the prior art, it is difficult to the problem of effectively removing, the application A kind of preparation method of copper electrolyte removing impurities agent is provided, the removing impurities agent that this method is prepared is applied to the de- of copper electrolyte Miscellaneous, achievable cost is low, and the purpose that removal efficiency is high, specifically, the invention discloses a kind of preparation of copper electrolyte removing impurities agent Method, comprise the following steps:
Dynamic wave mud and stibium trioxide are used into sulfuric acid washing, obtain mixture;
The mixture is aoxidized in the presence of oxidant, obtains copper electrolyte removing impurities agent.
In the preparation process of copper electrolyte removing impurities agent, the application is first configured raw material, in a particular embodiment, The dynamic wave mud is with the stibium trioxide according to mass ratio (1~5):1 proportioning adds;Wherein dynamic wave mud is copper anode mud melting Dynamic wave mud during Slag treatment, composition is mainly leaded, antimony, the material of bismuth oxidation state, and the content of general lead is more than 30wt%, the content of bismuth are more than 1wt%, and the content of antimony is more than 1wt%, and its quality refers to the quality of the dynamic wave mud after drying; The stibium trioxide is antimony oxide.
Then dynamic wave mud and stibium trioxide are used sulfuric acid washing, in the process, be preferably added to liquid-solid ratio 3 by the application:1 200~250g/L sulfuric acid is acidified, and the temperature in acidization is 70~80 DEG C, and the time is 0.5~1h.In the mistake of pickling Cheng Zhong, lead oxide, bismuth oxide, antimonial in dynamic wave mud etc. in presence of an acid, generation lead sulfate, bismuth sulfate, alkali formula sulphur Sour antimony (Sb4SO9·H2) and alkali formula bismuth sulfate (Bi O2S2O9·3H2O) etc., other soluble impurity, which is dissolved into acid, to be removed Go.
After pickling, the application is aoxidized the mixture after pickling, obtains removing impurities agent.In the process, stibium trioxide With oxidant reaction, the part pentavalent hydrate for generating antimony has suction-operated and chemical precipitation.During oxidation, The oxidant of the oxidation can be common oxidant, such as the oxidant such as sodium chlorate, hydrogen peroxide, chlorine and oxygen, but It is to introduce new impurity to also need to further handle, therefore, in the application, the oxidant of the oxidation is selected from hydrogen peroxide;It is described The addition of hydrogen peroxide is 1~2 times of dynamic wave mud and stibium trioxide gross mass;The time of the oxidation is 1~2h.
The preparation method of copper electrolyte removing impurities agent described herein is specially:
With stibium trioxide according to mass ratio 1~5 after dynamic wave mud is dried:1 proportioning, adds liquid-solid ratio 3:1 200~250g/L Dilute sulfuric acid stir and evenly mix, be warming up to 70~80 DEG C, react 0.5h, after being acidified removal filtration;Keeping temperature is constant, is slowly added to For hydrogen peroxide untill when Slurry bubble is seldom, hydrogen peroxide addition now is 1~2 times of addition amount of solid, reacts 1~2h, Washing and filtering, removing impurities agent configuration successful.
According to the present invention, after the completion of copper electrolyte removing impurities agent preparation, the removing impurities of copper electrolyte, the copper electricity are used it for Solution liquid removing impurities method be:
Electrolyte is mixed with removing impurities agent and carries out removing impurities, obtains removing impurities electrolyte;The removing impurities agent is described in such scheme Preparation method prepare removing impurities agent.
During above-mentioned removing impurities, the electrolyte and the liquid-solid ratio of the removing impurities agent are (10~15):1;It is described de- Miscellaneous temperature is 60~70 DEG C, and the time is 1.5~2h.
In the application, the process of the copper electrolyte removing impurities is specially:
By removing impurities agent and electrolyte according to solid-to-liquid ratio 1:10~15 proportionings, are warming up to 60~70 DEG C, and the reaction time is 1.5~ 2h, reaction are cooled to 30 DEG C of filterings after terminating, and obtain the scavenging solution after removing impurities purification and removing impurities agent.
During above-mentioned removing impurities, after copper electrolyte removing impurities, removing impurities agent is also obtained, the removing impurities agent is in copper electricity Solve to repeat in liquid and utilize, i.e., described removing impurities agent can be recycled, and the condition of recycling is identical with use for the first time.Removing impurities Afterwards, several materials in removing impurities agent do not change in acid solution, except it is a small amount of to electrolyte in impurity removal loss in addition to, Major part can reuse, and removing impurities agent can be taken out to part plus hydrogen peroxide when using the removal efficiency of antimony bismuth substantially to reduce Activate and add a part of new removing impurities agent, so recycle, the effect of removing impurities can effectively ensure that.
During the application copper electrolyte utilizes removing impurities agent removing impurities, the particle of the lead sulfate in removing impurities agent is extremely tiny, There can be suction-operated to the antimony bismuth in electrolyte, and the trivalent antimony bismuth in the hydrate and electrolyte of quinquevalence antimony reacts, and generates antimony The complex of the different valence state of sour bismuth and antimony, so as to which antimony bismuth is removed;Alkali formula antimony sulfate (Sb4SO9·H2) and alkali formula bismuth sulfate O (Bi2S2O9·3H2O self cleaning) further removes the impurity in electrolyte.Herein described copper electrolyte removing impurities agent Preparation and application it is specifically as shown in Figure 1.
Therefore, it is based on considered below that the application, which prepares removing impurities agent,:The lead of oxidation state, bismuth and others in dynamic wave mud Some impurity, by the washing of the impurity such as sulfuric acid reaction selenium, tellurium, copper into electrolyte, lead becomes lead sulfate precipitation, dynamic wave mud lead Content be higher than 30%, be advantageous to aggregation of the lead sulfate in removing impurities agent, after adding stibium trioxide, through peroxidating, antimony becomes five valence states, And the impurity in dynamic wave mud is further processed.Antimony in electrolyte, bismuth situation after removing impurities agent is made into, form metaantimmonic acid The compound of bismuth, bismuthic acid antimony and antimony bismuth oxide is collectively forming precipitation, is finally reached the mesh of antimony bismuth impurity in removing electrolyte 's.
Present invention process flow is short, and treating capacity is big, and equipment and raw material input are cheap, only need to be i.e. operable at ambient pressure, and Whole flow process Whote-wet method is metallurgical, non-environmental-pollution problem, and organic efficiency is higher.The removing impurities liquid of gained can further arsenic removal, take off Miscellaneous dose can reuse, and can outside be sold after saturation and can further reclaim antimony bismuth.Test result indicates that the application preparation is de- The removal efficiency of miscellaneous dose of antimony reaches as high as 91.34%, and the removal efficiency of bismuth reaches as high as 95.48%.
The present invention is not particularly limited to the sources of all raw materials, to be commercially available or passed through by specialty chemical personnel suitable When method is produced;The purity of added medicament is not particularly limited, preferably industrial top grade product.
For a further understanding of the present invention, with reference to preparation of the embodiment to copper electrolyte removing impurities agent provided by the invention The method of method and copper electrolyte removing impurities, protection scope of the present invention are not limited by the following examples.
Embodiment 1
First by dynamic wave mud and stibium trioxide according to mass ratio 3:50g after 1 proportioning, add 220g/L dilute sulfuric acid 150ml, add double Oxygen water 60ml, 1~2h is reacted in 70~80 DEG C, obtains removing impurities agent;Removing impurities agent composition is as shown in table 1:
The removing impurities agent compositional data table (wt%) of table 1
Removing impurities agent will be obtained it is added in the electrolyte that need to be purified to carry out a removing impurities, the temperature of removing impurities is 60~70 DEG C, Time is 1.5~2h;Bath composition and acquired results are as Table 2,3:
The bath composition table of table 2
3 1~3 removing impurities liquid component lists of table
Result above can be seen that antimony, the removal efficiency highest of bismuth respectively reach 79.9% and 89.6%, reach target.
Embodiment 2
First by dynamic wave mud and stibium trioxide according to mass ratio 2:50g after 1 proportioning, add 200g/L dilute sulfuric acid 150ml, add double Oxygen water 50ml, 1~2h is reacted in 70~80 DEG C, obtains removing impurities agent;Removing impurities agent composition is as shown in table 4:
The removing impurities agent component list (wt%) of table 4
Removing impurities agent will be obtained to be added in the electrolyte that need to be purified, carry out a removing impurities, the temperature of removing impurities is 60~70 DEG C, Time is 1.5~2h;Bath composition and acquired results are as shown in Table 5,6:
The bath composition table of table 5
6 1~3 removing impurities liquid component lists of table
Result above can be seen that antimony, the removal efficiency highest of bismuth respectively reach 91.34% and 95.48%, reach expected mesh Mark.
Embodiment 3
First by dynamic wave mud and stibium trioxide according to mass ratio 2:50g after 1 proportioning, add 250g/L dilute sulfuric acid 150ml, add double Oxygen water 80ml, 1~2h is reacted in 70~80 DEG C, obtains removing impurities agent;Removing impurities agent composition is as shown in table 7:
The removing impurities agent component list (wt%) of table 7
Removing impurities agent will be obtained again to be added in the electrolyte that need to be purified, and carries out a removing impurities, the temperature of removing impurities is 60~70 DEG C, the time is 1.5~2h;Bath composition and acquired results are as shown in table 8,9:
The bath composition table of table 8
9 1~3 removing impurities liquid component lists of table
Result above can be seen that antimony, the removal efficiency highest of bismuth respectively reach 81.57% and 86.56%, reach expected mesh Mark.
The explanation of above example is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that pair For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention. A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one The most wide scope caused.

Claims (8)

1. a kind of preparation method of copper electrolyte removing impurities agent, comprises the following steps:
Dynamic wave mud and stibium trioxide are used into sulfuric acid washing, obtain mixture;
The mixture is aoxidized in the presence of oxidant, obtains copper electrolyte removing impurities agent.
2. preparation method according to claim 1, it is characterised in that the concentration of sulfuric acid is 200~250g/L, the sulfuric acid Liquid-solid ratio with before processing material is 3:1, the before processing material is dynamic wave mud and stibium trioxide.
3. preparation method according to claim 1, it is characterised in that the mass ratio of the stibium trioxide and the dynamic wave mud is 1:(1~5).
4. preparation method according to claim 1, it is characterised in that the oxidant is hydrogen peroxide, the hydrogen peroxide Addition is 1~2 times of the dynamic wave mud and the stibium trioxide gross mass.
5. preparation method according to claim 1, it is characterised in that the temperature of the pickling is 70~80 DEG C, and the time is 0.5~1h;The time of the oxidation is 1~2h.
6. a kind of method of copper electrolyte removing impurities, including:
Electrolyte is mixed with removing impurities agent and carries out removing impurities, obtains removing impurities electrolyte;The removing impurities agent is that Claims 1 to 5 is any The removing impurities agent prepared by preparation method described in.
7. according to the method for claim 6, it is characterised in that the liquid-solid ratio of the electrolyte and removing impurities agent for (10~ 15):1.
8. according to the method for claim 6, it is characterised in that the temperature of the removing impurities be 60~70 DEG C, the time be 1.5~ 2h。
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109022785A (en) * 2018-10-10 2018-12-18 江西理工大学 A method of bismuth is removed from copper electrolyte
CN109022784A (en) * 2018-10-10 2018-12-18 江西理工大学 A method of bismuth, arsenic, antimony are removed from copper electrolyte
CN109628953A (en) * 2018-12-26 2019-04-16 浙江工业大学 The method of arsenic removal antimony bismuth is gone in a kind of copper electrolyte
CN113308606A (en) * 2021-06-04 2021-08-27 昆明理工大学 Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag

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CN104060295A (en) * 2014-07-14 2014-09-24 中南大学 Copper electrolyte adsorption, impurity removal and purification method
CN104962738A (en) * 2015-07-17 2015-10-07 中南大学 Copper electrolyte purifying technology
CN106086935A (en) * 2016-08-29 2016-11-09 江西理工大学 A kind of from copper electrolyte removing arsenic, antimony, the method for bismuth

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JPH1088382A (en) * 1996-09-19 1998-04-07 Sumitomo Metal Mining Co Ltd Method for electrolytically refining copper
CN102181882A (en) * 2011-04-09 2011-09-14 中南大学 Method for purifying copper electrolyte by regulating valence state
CN102433568A (en) * 2011-11-29 2012-05-02 东营方圆有色金属有限公司 Technology for removing bismuth from copper electrolyte with low cost
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CN109022785A (en) * 2018-10-10 2018-12-18 江西理工大学 A method of bismuth is removed from copper electrolyte
CN109022784A (en) * 2018-10-10 2018-12-18 江西理工大学 A method of bismuth, arsenic, antimony are removed from copper electrolyte
CN109022785B (en) * 2018-10-10 2020-05-01 江西理工大学 Method for removing bismuth from copper electrolyte
CN109022784B (en) * 2018-10-10 2020-05-08 江西理工大学 Method for removing bismuth, arsenic and antimony from copper electrolyte
CN109628953A (en) * 2018-12-26 2019-04-16 浙江工业大学 The method of arsenic removal antimony bismuth is gone in a kind of copper electrolyte
CN109628953B (en) * 2018-12-26 2020-10-23 浙江工业大学 Method for removing arsenic, antimony and bismuth in copper electrolyte
CN113308606A (en) * 2021-06-04 2021-08-27 昆明理工大学 Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag
CN113308606B (en) * 2021-06-04 2022-10-18 昆明理工大学 Method for leaching and separating valuable metals from silver-gold-rich selenium steaming slag

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