CN106011930B - A kind of continuous preparation method of cupric electrolysis refining electrolyte - Google Patents

A kind of continuous preparation method of cupric electrolysis refining electrolyte Download PDF

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Publication number
CN106011930B
CN106011930B CN201610601643.0A CN201610601643A CN106011930B CN 106011930 B CN106011930 B CN 106011930B CN 201610601643 A CN201610601643 A CN 201610601643A CN 106011930 B CN106011930 B CN 106011930B
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electrolytic cell
electrolyte
earth
positive pole
circulating slot
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CN106011930A (en
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高轩
高一轩
王拥军
赵体茂
刘素红
宗迎军
许向波
卫向平
冯瑞康
曹军超
李丕强
丁鹏
孙鹏
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Henan Yuguang Gold and Lead 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
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

The present invention relates to a kind of cupric electrolysis continuous preparation method of refining electrolyte, specific preparation process is:Life water is filled into earth of positive pole storage tank, it is filtered through earth of positive pole filter press, into supernatant liquid bath, enter circulating slot by microfroc filter, enter electrolytic cell through head tank, then cupric sulfate pentahydrate is added into electrolytic cell, the concentrated sulfuric acid is added using sulfuric acid gauge tank, the earth of positive pole then pulled out in electrolytic cell is stifled, electrolyte enters earth of positive pole storage tank, it is filtered through filter press, into supernatant liquid bath, enter head tank through microfroc filter filtering, entering the stifled electrolytic cell blocked with supernatant of the earth of positive pole through liquid separation packet, start normal circulation, gelatine is added into circulating slot before being powered for electrolytic cell, hydrochloric acid, gelatine is added after energization into circulating slot, hydrochloric acid, thiocarbamide, obtain electrolyte;Have the advantages that easy to operate, cycle production, preparation efficiency is high and electrolyte impurity content is low with the continuous preparation method of refining electrolyte using the cupric electrolysis of above-mentioned technique.

Description

A kind of continuous preparation method of cupric electrolysis refining electrolyte
Technical field
The invention belongs to the continuous preparations of cupric electrolysis technology field more particularly to a kind of cupric electrolysis refining electrolyte Method.
Background technology
Currently, before newly-built copper electrolyzing refining workshop is gone into operation, general be dissolved in water using cupric sulfate pentahydrate prepares electrolyte, or Person uses the old electrolyte in other copper electrolyzing refining workshops.Be dissolved in water using cupric sulfate pentahydrate, concentrator, earth of positive pole tank or When being prepared in net liquid process weight fluid bowl, because the volume for preparing electrolyte is larger, above-mentioned tank body narrow space is inconvenient, Heating, stirring are very limited when preparation, and electrolyte preparation efficiency is relatively low.Use the old electricity in other copper electrolyzing refining workshops Liquid is solved, because territory restriction and electrolyte long-distance transportation are there are certain danger, there is also significant limitations.
Invention content
It is an object of the invention to solve prior art copper electrolyte prepare when it is inconvenient, electrolyte preparation efficiency is low, The problem of being unable to continuous production, and a kind of cupric electrolysis for having easy to operate, recyclable continuous production, impurity content low is provided and is used Refine the continuous preparation method of electrolyte.
The technical solution adopted in the present invention is:
A kind of cupric electrolysis continuous preparation method of refining electrolyte, includes the following steps:
Step 1), into earth of positive pole storage tank fill into life water, filtered through filter press, filter out filter residue, filtrate enters supernatant Slot;
Step 2), life water filtered through microfroc filter after entering supernatant liquid bath, filter residue return earth of positive pole storage tank, filtrate into Enter circulating slot, filtrate enters head tank from circulating slot;
Step 3), into the filtrate from head tank enter electrolytic cell through liquid separation packet, life water is filled into electrolytic cell so that Liquid volume reaches the volume that plan prepares electrolyte in electrolytic cell, into before head tank, liter of the liquid in electrolytic cell defined Warm curve ranges inner edge enters side heating;
Step 4), at interval of one hour cupric sulfate pentahydrate was added portionwise into electrolytic cell, it is stirring while adding, until electrolytic cell Middle copper ion concentration reaches 38 ~ 42 g/L;
Step 5), using sulfuric acid gauge tank the concentrated sulfuric acid is slowly added into circulating slot, until the acidity of electrolysis tank liquid Reach 160 ~ 200g/L;
Step 6), pull out that the earth of positive pole in electrolytic cell is stifled, and the liquid in electrolytic cell enters earth of positive pole storage tank, through filter press mistake Filter enters circulating slot into supernatant liquid bath, then through microfroc filter filtering, enters liquid separation packet through head tank, finally enter anode The stifled electrolytic cell blocked with supernatant of mud, starts normal circulation;
Step 7), after normal circulation, gelatine, hydrochloric acid are added into circulating slot before being powered for electrolytic cell, control chlorine in electrolytic cell Ion concentration is 0.03 ~ 0.06g/L, and gelatine, hydrochloric acid, thiocarbamide is added after energization into circulating slot, obtains electrolyte.
Further, the heating device heated to liquid is equipped between the circulating slot and head tank.
Further, the heating device is tray heater.
Further, 60 DEG C -70 DEG C are finally heated into the liquid in circulating slot.
Further, step 7)The additive amount that hydrochloric acid needed for copper per ton is electrolysed after middle energization is the addition of 150 ~ 200g, thiocarbamide Amount is 20 ~ 80g, the additive amount of gelatine is 20 ~ 60g, and wherein hydrochloric acid and thiocarbamide cannot be added simultaneously.
Further, step 4)Compressed gas is passed through into electrolytic cell during cupric sulfate pentahydrate is added to electrolytic cell, Enhancing stirring.
Further, the compressed gas is compressed air or compressed nitrogen.
The beneficial effects of the present invention are:
1. in electrolyte preparation process, electrolyte directly prepares completion in a cell, and electrolyzer surface place is larger, duty Work is easy to operate, and preparation process is carried out continuously, and electrolyte preparation efficiency is high;
2. in electrolyte preparation process, can be heated to electrolyte, stirring, electrolyte continuously recycles, and improves efficiency;
3. electrolyte and with water by being filtered for multiple times, prepared electrolyte impurity content is low.
A kind of cupric electrolysis provided by the invention continuous preparation method of refining electrolyte has easy to operate, cycle life Production, the advantage that preparation efficiency is high and electrolyte impurity content is low.
Description of the drawings
Fig. 1 is the process flow chart for the continuous preparation method that a kind of cupric electrolysis provided by the invention refines electrolyte.
Specific implementation mode
The invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1, a kind of continuous preparation method of cupric electrolysis refining electrolyte, as shown in Figure 1, including the following steps:
Step 1), into earth of positive pole storage tank fill into life water, filtered through filter press, filter out filter residue, filtrate enters supernatant Slot;
Step 2), life water filtered through microfroc filter after entering supernatant liquid bath, filter residue return earth of positive pole storage tank, filtrate into Enter circulating slot, filtrate enters head tank from circulating slot;
Step 3), into the filtrate of head tank enter electrolytic cell through liquid separation packet, life water is filled into electrolytic cell so that electricity Solution tank liquid volume reaches the volume that plan prepares electrolyte, into before head tank, heating of the liquid in electrolytic cell defined Curve ranges inner edge enters side heating;
Step 4), at interval of one hour cupric sulfate pentahydrate was added portionwise into electrolytic cell, it is stirring while adding, front end band is used in combination The airbag of stainless steel pipes introduces compressed air or compressed nitrogen into electrolytic cell, and enhancing stirring is up to copper ion in electrolytic cell Concentration reaches 38 ~ 42 g/L;
Step 5), using sulfuric acid gauge tank the concentrated sulfuric acid is slowly added into circulating slot, until the acidity of electrolysis tank liquid Reach 160 ~ 200g/L;
Step 6), pull out that the earth of positive pole in electrolytic cell is stifled, and the liquid in electrolytic cell enters earth of positive pole storage tank, through filter press mistake Filter enters circulating slot into supernatant liquid bath, then through microfroc filter filtering, enters liquid separation packet through head tank, finally enter anode The stifled electrolytic cell blocked with supernatant of mud, starts normal circulation;
Step 7), after normal circulation, gelatine, hydrochloric acid are added into circulating slot before being powered for electrolytic cell, control chlorine in electrolytic cell Ion concentration is 0.03 ~ 0.06g/L, and gelatine, hydrochloric acid, thiocarbamide is added after energization into circulating slot, copper institute per ton is electrolysed after energization It is 150 ~ 200g to need the additive amount of hydrochloric acid, the additive amount of thiocarbamide is 20 ~ 80g, the additive amount of gelatine is 20 ~ 60g, wherein hydrochloric acid and Thiocarbamide cannot be added simultaneously, obtain electrolyte.
The continuous preparation method of 2 a kind of cupric electrolysis of embodiment refining electrolyte, as shown in Figure 1, including the following steps:
Step 1), into earth of positive pole storage tank fill into life water, filtered through filter press, filter out filter residue, filtrate enters supernatant Slot;
Step 2), life water filtered through microfroc filter after entering supernatant liquid bath, filter residue return earth of positive pole storage tank, filtrate into Enter circulating slot, filtrate enters head tank from circulating slot;
Step 3), into the filtrate of head tank enter electrolytic cell through liquid separation packet, life water is filled into electrolytic cell so that electricity Solution tank liquid volume reaches the volume that plan prepares electrolyte, into before head tank, heating of the liquid in electrolytic cell defined Curve ranges inner edge enters side heating;
Step 4), at interval of one hour cupric sulfate pentahydrate was added portionwise into electrolytic cell, it is stirring while adding, front end band is used in combination The airbag of stainless steel pipes introduces compressed air or compressed nitrogen into electrolytic cell, and enhancing stirring is up to copper ion in electrolytic cell Concentration reaches 38g/L;
Step 5), using sulfuric acid gauge tank the concentrated sulfuric acid is slowly added into circulating slot, until the acidity of electrolysis tank liquid Reach 160 ~ 200g/L;
Step 6), pull out that the earth of positive pole in electrolytic cell is stifled, and the liquid in electrolytic cell enters earth of positive pole storage tank, through filter press mistake Filter enters circulating slot into supernatant liquid bath, then through microfroc filter filtering, enters liquid separation packet through head tank, finally enter anode The stifled electrolytic cell blocked with supernatant of mud, starts normal circulation;
Step 7), after normal circulation, gelatine, hydrochloric acid are added into circulating slot before being powered for electrolytic cell, control chlorine in electrolytic cell Ion concentration is 0.06g/L, and gelatine, hydrochloric acid, thiocarbamide is added after energization into circulating slot, hydrochloric acid needed for copper per ton is electrolysed after energization Additive amount be 200g, the additive amount of thiocarbamide is 80g, the additive amount of gelatine is 60g, wherein hydrochloric acid and thiocarbamide to add simultaneously Enter, obtains electrolyte.
The continuous preparation method of 3 a kind of cupric electrolysis of embodiment refining electrolyte, as shown in Figure 1, including the following steps:
Step 1), into earth of positive pole storage tank fill into life water, filtered through filter press, filter out filter residue, filtrate enters supernatant Slot;
Step 2), life water filtered through microfroc filter after entering supernatant liquid bath, filter residue return earth of positive pole storage tank, filtrate into Enter circulating slot, filtrate enters head tank from circulating slot;
Step 3), into the filtrate of head tank enter electrolytic cell through liquid separation packet, life water is filled into electrolytic cell so that electricity Solution tank liquid volume reaches the volume that plan prepares electrolyte, into before head tank, heating of the liquid in electrolytic cell defined Curve ranges inner edge enters side heating;
Step 4), at interval of one hour cupric sulfate pentahydrate was added portionwise into electrolytic cell, it is stirring while adding, front end band is used in combination The airbag of stainless steel pipes introduces compressed air or compressed nitrogen into electrolytic cell, and enhancing stirring is up to copper ion in electrolytic cell Concentration reaches 38 g/L;
Step 5), using sulfuric acid gauge tank the concentrated sulfuric acid is slowly added into circulating slot, until the acidity of electrolysis tank liquid Reach 160 ~ 200g/L;
Step 6), pull out that the earth of positive pole in electrolytic cell is stifled, and the liquid in electrolytic cell enters earth of positive pole storage tank, through filter press mistake Filter enters circulating slot into supernatant liquid bath, then through microfroc filter filtering, enters liquid separation packet through head tank, finally enter anode The stifled electrolytic cell blocked with supernatant of mud, starts normal circulation;
Step 7), after normal circulation, gelatine, hydrochloric acid are added into circulating slot before being powered for electrolytic cell, control chlorine in electrolytic cell Ion concentration is 0.03g/L, and gelatine, hydrochloric acid, thiocarbamide is added after energization into circulating slot, hydrochloric acid needed for copper per ton is electrolysed after energization Additive amount be 150g, the additive amount of thiocarbamide is 20g, the additive amount of gelatine is 20g, wherein hydrochloric acid and thiocarbamide to add simultaneously Enter, obtains electrolyte.
The continuous preparation method of 4 a kind of cupric electrolysis of embodiment refining electrolyte, as shown in Figure 1, including the following steps:
Step 1), into earth of positive pole storage tank fill into life water, filtered through filter press, filter out filter residue, filtrate enters supernatant Slot;
Step 2), life water filtered through microfroc filter after entering supernatant liquid bath, filter residue return earth of positive pole storage tank, filtrate into Enter circulating slot, filtrate enters head tank from circulating slot;
Step 3), into the filtrate of head tank enter electrolytic cell through liquid separation packet, life water is filled into electrolytic cell so that electricity Solution tank liquid volume reaches the volume that plan prepares electrolyte, into before head tank, heating of the liquid in electrolytic cell defined Curve ranges inner edge enters side heating;
Step 4), at interval of one hour cupric sulfate pentahydrate was added portionwise into electrolytic cell, it is stirring while adding, front end band is used in combination The airbag of stainless steel pipes introduces compressed air or compressed nitrogen into electrolytic cell, and enhancing stirring is up to copper ion in electrolytic cell Concentration reaches 40 g/L;
Step 5), using sulfuric acid gauge tank the concentrated sulfuric acid is slowly added into circulating slot, until the acidity of electrolysis tank liquid Reach 170g/L;
Step 6), pull out that the earth of positive pole in electrolytic cell is stifled, and the liquid in electrolytic cell enters earth of positive pole storage tank, through filter press mistake Filter enters circulating slot into supernatant liquid bath, then through microfroc filter filtering, enters liquid separation packet through head tank, finally enter anode The stifled electrolytic cell blocked with supernatant of mud, starts normal circulation;
Step 7), after normal circulation, gelatine, hydrochloric acid are added into circulating slot before being powered for electrolytic cell, control chlorine in electrolytic cell Ion concentration is 0.05g/L, and gelatine, hydrochloric acid, thiocarbamide is added after energization into circulating slot, hydrochloric acid needed for copper per ton is electrolysed after energization Additive amount be 180g, the additive amount of thiocarbamide is 50g, the additive amount of gelatine is 40g, wherein hydrochloric acid and thiocarbamide to add simultaneously Enter, obtains electrolyte.
The continuous preparation side of a kind of cupric electrolysis of present invention refining electrolyte it can be seen from above specific implementation mode Method has the advantages that easy to operate, cycle production, preparation efficiency is high and electrolyte impurity content is low.

Claims (8)

1. a kind of cupric electrolysis continuous preparation method of refining electrolyte, which is characterized in that include the following steps:
Step 1), into earth of positive pole storage tank fill into life water, filtered through filter press, filter out filter residue, filtrate enters supernatant liquid bath;
Step 2), life water filtered through microfroc filter after entering supernatant liquid bath, filter residue return earth of positive pole storage tank, filtrate enter follows Annular groove, filtrate enter head tank from circulating slot;
Step 3), into the filtrate of head tank enter electrolytic cell through liquid separation packet, life water is filled into electrolytic cell so that electrolytic cell Interior liquid volume reaches the volume that plan prepares electrolyte, into before head tank, heating curve of the liquid in electrolytic cell defined Range inner edge enters side heating;
Step 4), at interval of one hour cupric sulfate pentahydrate was added portionwise into electrolytic cell, it is stirring while adding, until electrolysis buried copper Ion concentration reaches 38 ~ 42 g/L;
Step 5), using sulfuric acid gauge tank the concentrated sulfuric acid is slowly added into circulating slot, until the acidity of electrolysis tank liquid reaches 160~200g/L;
Step 6), pull out that the earth of positive pole in electrolytic cell is stifled, and the liquid in electrolytic cell enters earth of positive pole storage tank, is filtered through filter press, Enter circulating slot into supernatant liquid bath, then through microfroc filter filtering, enters liquid separation packet through head tank, it is stifled to finally enter the earth of positive pole The electrolytic cell blocked with supernatant starts normal circulation;
Step 7), after normal circulation, gelatine, hydrochloric acid are added into circulating slot before being powered for electrolytic cell, control chlorion in electrolytic cell Gelatine, hydrochloric acid, thiocarbamide are added into circulating slot, obtains electrolyte by a concentration of 0.03 ~ 0.06g/L after energization.
2. a kind of continuous preparation method of cupric electrolysis according to claim 1 refining electrolyte, it is characterised in that:Institute State the heating device for being equipped between circulating slot and head tank and being heated to liquid.
3. a kind of continuous preparation method of cupric electrolysis according to claim 2 refining electrolyte, which is characterized in that described Heating device be tray heater.
4. a kind of continuous preparation method of cupric electrolysis according to claim 3 refining electrolyte, which is characterized in that enter Liquid in circulating slot is finally heated to 60 DEG C -70 DEG C.
5. according to a kind of continuous preparation method of cupric electrolysis refining electrolyte described in claim 1, which is characterized in that step 4) In electrolyte configuration process, cupric sulfate pentahydrate is directly added into electrolytic cell.
6. a kind of continuous preparation method of cupric electrolysis according to claim 1 refining electrolyte, which is characterized in that step 7)The additive amount that hydrochloric acid needed for copper per ton is electrolysed after middle energization is 150 ~ 200g, the additive amount of thiocarbamide is 20 ~ 80g, gelatine adds Dosage is 20 ~ 60g, and wherein hydrochloric acid and thiocarbamide cannot be added simultaneously.
7. a kind of continuous preparation method of cupric electrolysis according to claim 1 refining electrolyte, which is characterized in that step 4)Compressed gas, enhancing stirring are passed through into electrolytic cell during cupric sulfate pentahydrate is added to electrolytic cell.
8. a kind of continuous preparation method of cupric electrolysis according to claim 7 refining electrolyte, which is characterized in that described Compressed gas is compressed air or compressed nitrogen.
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CN106498440B (en) * 2016-12-13 2018-04-03 云南锡业股份有限公司铜业分公司 A kind of copper electrolysis system fluid balance control method
CN106637305A (en) * 2016-12-28 2017-05-10 阳谷祥光铜业有限公司 Electrolyte treatment method and system in copper electrolysis process
CN110144604B (en) * 2019-06-17 2020-06-09 阳谷祥光铜业有限公司 Preparation process of electrodeposited copper powder
CN113463138A (en) * 2021-07-16 2021-10-01 兰溪自立环保科技有限公司 Copper anode slime regenerated acid recycling equipment and recycling method thereof

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