CN104313320B - The strong acid saturated crystallization separation method of zinc-magnesium in a kind of zinc electrolyte - Google Patents
The strong acid saturated crystallization separation method of zinc-magnesium in a kind of zinc electrolyte Download PDFInfo
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- CN104313320B CN104313320B CN201410567990.7A CN201410567990A CN104313320B CN 104313320 B CN104313320 B CN 104313320B CN 201410567990 A CN201410567990 A CN 201410567990A CN 104313320 B CN104313320 B CN 104313320B
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Abstract
The invention discloses in a kind of zinc electrolyte zinc-magnesium strong acid saturated crystallization separation method, including the step such as strong acid allotment, stirring eddy flow, precipitate and separate and separator reuse.The phenomenon that the present invention quickly can be separated out in specific high temperature peracid condition in a large number using zinc sulfate and magnesium sulfate, zinc-magnesium in zinc electrolyte is separated, whole production process does not introduce any impurity, discharge without waste water and dregs, sulphuric acid in flow process can all reclaim use, realize the whole of electrolysis waste solution to recycle without outer row, saved the consumption of waste water, the expenses of environmental protection of Solid state fermentation and additive in traditional neutralization precipitation method, can effectively reduce power consumption.Present invention process simplicity, short, easy to operate flow process, reduced investment, consumption are low, and additive and the electrolysis waste solution after process all can be recycled, and fully achieve the reasonable utilization and maximizing the benefits of ERM, have preferable economic benefit and social benefit.
Description
Technical field
The invention belongs to the electrolytic zinc technical field of hydrometallurgy industry, and in particular in a kind of zinc electrolyte, zinc-magnesium is strong
Sour saturated crystallization separation method.
Background technology
It is in zinc electrolysis production process, inevitably containing foreign metals such as lead, nickel, copper, magnesium in raw material zinc ore, right
Electrolytic zinc quality affects very big, the current efficiency and electrolysis zinc product when wherein the magnesium elements in zinc liquid can have a strong impact on electrolysis
Purity.With constantly carrying out for electrolytic process, the Zn content in electrolyte constantly will be reduced, and sulfuric acid content is continuously increased,
In order to keep stablizing for electrolytic condition, need from a waste liquid extraction part for electrolysis to return in sulphuric leachate, at this moment, contain
The anolyte of magnesium ion and sulphuric acid is used to soak ore deposit together, and in leaching and purification process, the magnesium ion in waste liquid can not be by
Effectively remove, then, in recycling, magnesium ion is progressively enriched with electrolytic zinc anolyte so that electrolytic process energy consumption significantly increases
Plus.For reducing energy consumption, generally opened a way using electrolyte, daily the electrolyte in discharge once electrolytic groove, this part of discharge
In electrolyte, sulphuric acid, zinc, content of magnesium are all higher, to avoid environmental pollution and waste, the typically electrolyte to discharging from first using hydrogen
Then plus sulfide precipitation is filtered calcium oxide is neutralized, and, precipitate returns pyrometallurgical smelting, outer after wastewater treatment to arrange.Although the method
Simply, implement easy, but directly neutralize, however it remains problems with：1., due to acid concentration height in waste liquid, needs add big
Amount calcium hydroxide is neutralized, and can produce a large amount of waste residues, while being also a kind of waste to sour resource；2., precipitation process with the addition of
Sulfide, easily causes secondary pollution after the hydrogen sulfide emission of generation, the emission treatment cost of investment in later stage is higher；3., generate
Slag in zinc recovering using relatively costly, waste water is difficult to direct reuse and needs discharge, and enterprise's production capacity is high, resource circulation utilization
Rate is low.
The content of the invention
In order to solve problem present in background technology, it is an object of the invention to provide one kind can have from zinc electrolyte
Effect separating magnesium sulphate, realizes zero generation of wastewater zero discharge and solid waste while electrolytic zinc power consumption is reduced, and energy-conserving and environment-protective, invests into
The zinc-magnesium strong acid saturated crystallization separation method of this low, achievable resource circulation utilization.
The object of the present invention is achieved like this, and the separation method is comprised the following steps that：
1., strong acid allotment：Pending zinc electrolyte is placed in agitator tank, is slowly added into tank after opening agitating device
Concentration is 98% concentrated sulphuric acid, and zinc electrolyte is 1 with the new volume ratio for adding concentrated sulphuric acid:0.8～0.9；
2., stir eddy flow：Accelerate stirring when mixeding liquid temperature reaches 110～120 DEG C, form eddy flow, speed of agitator is
1000～1200 revs/min, mixing time is 3～5 minutes；
3., precipitate and separate：Mixed liquor is imported after the completion of stirring and staticly settled in sedimentation tank, mixed liquor is separated into and is deposited in
The zinc-magnesium solidfied material of downside and the supernatant for floating over upside；
4., separator reuse：Transparent limpid supernatant pump is returned into wet method electrolysis Zn system reuse, bottom is deposited in
Zinc-magnesium solidfied material send dispensing in pyrometallurgical smelting fuming furnace to smelt to reclaim zinc, magnesium become slag making element water it is broken after be used as cement raw
Material.
The research of Jing lot of experiments finds that the zinc sulfate and magnesium sulfate in zinc electrolyte can be big at specific temperature and acidity
Amount is quick to be separated out, and the present invention formulates technique using the characteristic and the zinc-magnesium in zinc electrolyte is separated, and whole production process does not have
There is introducing any impurity, discharge without waste water and dregs, the sulphuric acid in flow process can all reclaim use, realize the whole of electrolysis waste solution
Recycle without outer row, saved the consumption of waste water, the expenses of environmental protection of Solid state fermentation and additive in traditional neutralization precipitation method, can
Power consumption is reduced effectively.Present invention process simplicity, short, easy to operate flow process, reduced investment, consumption are low, and additive and the electricity after process
Liquid waste solution all can be recycled, and fully achieve the reasonable utilization and maximizing the benefits of ERM, have preferable economy
Benefit and social benefit.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is further illustrated, but never in any form to the present invention in addition
Limit, based on present invention teach that any conversion for being made or replacement, belong to protection scope of the present invention.
Embodiment 1：
It is the zinc electrolyte of 24.5g/L that 1000L Zn contents are taken for 51g/L, content of magnesium, is carried out point by the method for the invention
From.
1., strong acid allotment：Pending zinc electrolyte is placed in agitator tank, is slowly added into tank after opening agitating device
Concentration is 98% concentrated sulphuric acid, and the speed of agitator of agitating device is 800 revs/min, solution mix homogeneously, temperature stabilization is increased,
Do not occur it is quick-fried splash, zinc electrolyte is 1 with the new volume ratio for adding concentrated sulphuric acid:0.8；
2., stir eddy flow：Accelerate stirring when mixeding liquid temperature reaches 110 DEG C, form eddy flow, speed of agitator is 1200
Rev/min, mixing time is 5 minutes；
3., precipitate and separate：Mixed liquor is imported after the completion of stirring and staticly settled in sedimentation tank, the time for staticly settling is 90
Minute, mixed liquor is separated into the zinc-magnesium solidfied material for being deposited in downside and the supernatant for floating over upside；
4., separator reuse：Transparent limpid supernatant pump is returned into wet method electrolysis Zn system reuse, bottom is deposited in
Zinc-magnesium solidfied material send dispensing in pyrometallurgical smelting fuming furnace to smelt to reclaim zinc, magnesium become slag making element water it is broken after be used as cement raw
Material.
In the present embodiment, after testing, in the supernatant after precipitate and separate Zn content be 1.96g/L, content of magnesium be 7.28g/
L, up to 96%, the separation rate of magnesium solves industry conventional difficulties up to 70% to the separation rate of zinc, meets current energy-conserving and environment-protective, resource and follows
Ring such as utilizes at the social development in science and technology theme, with preferable economic benefit and social benefit.
Embodiment 2：
It is the zinc electrolyte of 24.5g/L that 1000L Zn contents are taken for 51g/L, content of magnesium, is carried out point by the method for the invention
From.
1., pretreatment：In pending zinc electrolyte, add the concentration that percent by volume is 1% to be 98% concentrated sulphuric acid and stir
Mix uniform, make the temperature of zinc electrolyte be increased to 36 DEG C；
2., strong acid allotment：Pending zinc electrolyte is placed in agitator tank, is slowly added into tank after opening agitating device
Concentration is 98% concentrated sulphuric acid, and the speed of agitator of agitating device is 900 revs/min, solution mix homogeneously, temperature stabilization is increased,
Do not occur it is quick-fried splash, zinc electrolyte is 1 with the new volume ratio for adding concentrated sulphuric acid:0.85；
3., stir eddy flow：Accelerate stirring when mixeding liquid temperature reaches 115 DEG C, form eddy flow, speed of agitator is 1100
Rev/min, mixing time is 4 minutes；
4., precipitate and separate：Mixed liquor is imported after the completion of stirring and staticly settled in sedimentation tank, the time for staticly settling is 60
Minute, mixed liquor is separated into the zinc-magnesium solidfied material for being deposited in downside and the supernatant for floating over upside；
5., separator reuse：Transparent limpid supernatant pump is returned into wet method electrolysis Zn system reuse, bottom is deposited in
Zinc-magnesium solidfied material send dispensing in pyrometallurgical smelting fuming furnace to smelt to reclaim zinc, magnesium become slag making element water it is broken after be used as cement raw
Material.
In the present embodiment, after testing, in the supernatant after precipitate and separate Zn content be 2g/L, content of magnesium be 4.3g/L, zinc
Separation rate up to 96%, the separation rate of magnesium solves industry conventional difficulties up to 82%, meet current energy-conserving and environment-protective, resources circulation profit
With social development in science and technology theme is waited, with preferable economic benefit and social benefit.
Embodiment 3：
It is the zinc electrolyte of 24.5g/L that 1000L Zn contents are taken for 51g/L, content of magnesium, is carried out point by the method for the invention
From.
1., pretreatment：The concentrated sulphuric acid that the concentration that percent by volume is 0.5% is 98% is added in pending zinc electrolyte simultaneously
Stir, make the temperature of zinc electrolyte be increased to 34 DEG C；
2., strong acid allotment：Pending zinc electrolyte is placed in agitator tank, is slowly added into tank after opening agitating device
Concentration is 98% concentrated sulphuric acid, and the speed of agitator of agitating device is 1000 revs/min, makes solution mix homogeneously, on temperature stabilization
Rise, do not occur it is quick-fried splash, zinc electrolyte is 1 with the new volume ratio for adding concentrated sulphuric acid: 0.9；
3., stir eddy flow：Accelerate stirring when mixeding liquid temperature reaches 120 DEG C, form eddy flow, speed of agitator is 1000
Rev/min, mixing time is 3 minutes；
4., precipitate and separate：Mixed liquor is imported after the completion of stirring and staticly settled in sedimentation tank, the time for staticly settling is 40
Minute, mixed liquor is separated into the zinc-magnesium solidfied material for being deposited in downside and the supernatant for floating over upside；
5., separator reuse：Transparent limpid supernatant pump is returned into wet method electrolysis Zn system reuse, bottom is deposited in
Zinc-magnesium solidfied material send dispensing in pyrometallurgical smelting fuming furnace to smelt to reclaim zinc, magnesium become slag making element water it is broken after be used as cement raw
Material.
In the present embodiment, after testing, in the supernatant after precipitate and separate Zn content be 1.9g/L, content of magnesium be 5.8g/L,
Up to 96%, the separation rate of magnesium solves industry conventional difficulties up to 76% to the separation rate of zinc, meets current energy-conserving and environment-protective, resources circulation
The social development in science and technology theme such as utilize, with preferable economic benefit and social benefit.
Claims (3)
1. in a kind of zinc electrolyte zinc-magnesium strong acid saturated crystallization separation method, it is characterised in that comprise the following steps that：
1., strong acid allotment：Pending zinc electrolyte is placed in agitator tank, first volume basis is added in pending zinc electrolyte
Than concentrated sulphuric acid that the concentration for 0.5～2% is 98% and stir, make the temperature of zinc electrolyte be increased to 34～36 DEG C；Then
The concentrated sulphuric acid that concentration is 98%, zinc electrolyte and the new volume for adding concentrated sulphuric acid are slowly added after agitating device is opened into tank
Than for 1:0.8～0.9；
2., stir eddy flow：Accelerate stirring when mixeding liquid temperature reaches 110～120 DEG C, form eddy flow, speed of agitator is 1000
～1200 revs/min, mixing time is 3～5 minutes；
3., precipitate and separate：Mixed liquor is imported after the completion of stirring and staticly settled in sedimentation tank, mixed liquor is separated into and is deposited in downside
Zinc-magnesium solidfied material and float over upside supernatant；
4., separator reuse：Transparent limpid supernatant pump is returned into wet method electrolysis Zn system reuse, the zinc of bottom is deposited in
During magnesium hardener thing send pyrometallurgical smelting fuming furnace, dispensing smelts recovery zinc, and magnesium is used as cement raw material after becoming slag making element water quenching.
2. according to claim 1 in a kind of zinc electrolyte zinc-magnesium strong acid saturated crystallization separation method, it is characterised in that：Step
The speed of agitator of rapid 1. middle agitating device is 800～1000 revs/min.
3. according to claim 1 in a kind of zinc electrolyte zinc-magnesium strong acid saturated crystallization separation method, it is characterised in that：Step
It is rapid 3. in time for staticly settling be 40～90 minutes.
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| CN201410567990.7A CN104313320B (en) | 2014-10-23 | 2014-10-23 | The strong acid saturated crystallization separation method of zinc-magnesium in a kind of zinc electrolyte |
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| CN201410567990.7A CN104313320B (en) | 2014-10-23 | 2014-10-23 | The strong acid saturated crystallization separation method of zinc-magnesium in a kind of zinc electrolyte |
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| CN104313320B true CN104313320B (en) | 2017-04-05 |
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| CN104630471B (en) * | 2015-03-01 | 2017-06-27 | 云南驰宏锌锗股份有限公司 | A kind of method and its device of the removing solution of zinc sulfate magnesium ion that pressurizes |
| CN104630469B (en) * | 2015-03-01 | 2017-03-08 | 云南驰宏锌锗股份有限公司 | A kind of combine the method for Organic substance and magnesium ion and its device in removing solution of zinc sulfate |
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| RU2075524C1 (en) * | 1993-03-10 | 1997-03-20 | Научно-производственный кооператив "Доминион" | Method of processing of zinc-containing solutions |
| JP3273901B2 (en) * | 1997-04-24 | 2002-04-15 | 日鉄鉱業株式会社 | Treatment method of hydrochloric acid waste liquid in which iron and zinc are dissolved |
| AU2006326862A1 (en) * | 2005-12-22 | 2007-06-28 | Bhp Billiton Ssm Development Pty Ltd | Recovery of solid magnesium sulfate hydrate |
| WO2009039579A1 (en) * | 2007-09-26 | 2009-04-02 | Bhp Billiton Ssm Development Pty Ltd | Acid recovery from metal sulfates |
| CN103539302B (en) * | 2013-10-31 | 2015-04-22 | 惠州市斯瑞尔环境化工有限公司 | Treatment method of zinc-containing and iron-containing waste acid |
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