CN106367594A - Low-energy-consumption, quick and recyclable lead paste desulfurization mother liquid desalinating process - Google Patents

Low-energy-consumption, quick and recyclable lead paste desulfurization mother liquid desalinating process Download PDF

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Publication number
CN106367594A
CN106367594A CN201610725560.2A CN201610725560A CN106367594A CN 106367594 A CN106367594 A CN 106367594A CN 201610725560 A CN201610725560 A CN 201610725560A CN 106367594 A CN106367594 A CN 106367594A
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CN
China
Prior art keywords
mother solution
lead
desulfurization
mother liquid
lead paste
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610725560.2A
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Chinese (zh)
Inventor
吴国庆
朱保义
任永刚
陈华勇
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Anhui Huabo Renewable Resources Technology Co Ltd
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Anhui Huabo Renewable Resources Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Anhui Huabo Renewable Resources Technology Co Ltd filed Critical Anhui Huabo Renewable Resources Technology Co Ltd
Priority to CN201610725560.2A priority Critical patent/CN106367594A/en
Publication of CN106367594A publication Critical patent/CN106367594A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00Obtaining lead
    • C22B13/04Obtaining lead by wet processes
    • C22B13/045Recovery from waste materials

Abstract

A low-energy-consumption, quick and recyclable lead paste desulfurization mother liquid desalinating process includes the steps of: 1) collecting the waste lead paste from detachment of waste and used lead acid batteries, and according to difference of sulfur content of the waste lead paste, adding water to the waste lead paste in a reaction kettle, in which strong convection can be formed, to prepare ore slurry being 50% in solid content; 2) adding Na2CO3 to the ore slurry with addition quantity of the Na2CO3 being 1.3-1.4 times as theoretical quantity, wherein the addition process is free of heating; 3) starting the reaction kettle to continuously stir the ore slurry for 30 min, and feeding the ore slurry into a device having strong collision, extrusion and friction effects to perform a reaction, wherein a PbCO3 layer coating the surface of PbSO4 during a desulfurization process is broken, so that the PbSO4 is fully contact with the Na2CO3 in the solution; and 4) after the reaction for 20 min, performing solid liquid separation to the reaction product to obtain desulfurization mother liquid and desulfurization lead paste; and 5) pumping the desulfurization mother liquid into a crystallizer, adding a certain amount of a crystallization accelerant, discharging the mother liquid after 30 min and performing solid liquid separation so as to removal by-product salt from the desulfurization mother liquid.

Description

A kind of low energy consumption, lead plaster desulphurization mother solution desalinating process quick, capable of circulation
Technical field
The present invention relates to reviver technical field is and in particular to a kind of low energy consumption, quick, lead plaster desulphurization mother solution capable of circulation take off Salt technique.
Background technology
Although various battery new techniques are evolving now, have the lead-acid battery of 150 years development history still with By means of its excellent cost performance, stable chemical property, ripe production technology and its higher recycling of waste product etc. Advantage occupies first place in secondary cell market.The sustainable growth of annual production had both represented the importance to the mankind for the lead-acid battery, Mean have substantial amounts of lead to be consumed on lead-acid accumulator product every year.
Lead-acid accumulator, as the main consumer products in the whole world, also becomes topmost lead regenerated resources simultaneously.China The primary raw material of reviver has more than 80% to be derived from waste and old lead acid accumulator.Lead as a kind of highly toxic heavy metal, from environmental protection From the point of view of, the recycling to lead in waste and old lead acid accumulator is significant.
The recovery process of lead-acid battery scrap lead cream at this stage is broadly divided into: pyrometallurgical smelting technique and wet recycling process. Pyrometallurgical smelting technique can produce the secondary pollutions such as lead dust and sulfur dioxide in heating process, and high energy consumption, utilization rate are low.Wet Method recovery process useless diachylon desulphurization method the most frequently used at present is with na2co3Or nahco3For desulfurizing agent, stirring reaction makes it take off Sulfur, by pbso4It is converted into pbco3, then Hydrocerussitum (Ceruse) is obtained to its roasting or electrolysis.Desulphurization mother solution after desulfurization needs to carry out at desalination Reason, and desalinating process of the prior art is complex, inefficient.
Content of the invention
The technical problem to be solved is to provide a kind of method simple, the low energy consumption of cycle is short, quick, can follow Ring lead plaster desulphurization mother solution desalinating process.
The technical problem to be solved employs the following technical solutions to realize:
A kind of low energy consumption, lead plaster desulphurization mother solution desalinating process quick, capable of circulation, comprise the following steps that:
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, according to the difference of scrap lead cream sulfur content, can formed Add water in the reactor of strong convection the ore pulp being configured to that solid content is 50% by scrap lead cream;
(2) to addition na interior in the ore pulp of step (1)2co3, wherein na2co3Addition be theoretical amount 1.3-1.4 Times, process does not need to heat;
(3) start reactor continuous stirring after 30 minutes, ore pulp is put into one and carries strong impaction, extruding, rubbing action Equipment in reacted, will apply in pbso in sweetening process4The pbco on surface3Layer open, makes pbso4In the solution with na2co3 Being fully contacted, thus improving desulfuration efficiency, reaching the purpose forcing desulfurization;
(4), after reacting 20 minutes, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster;
(5) desulphurization mother solution is squeezed into crystallizer, and add a certain amount of crystallization promoter, release after 30 minutes and carry out solid-liquid Separate, the secondary salt in desulphurization mother solution is removed, salt rejection rate is more than 93%.
Separating liquid after above-mentioned crystallization uses low-pressure distillation technology to reclaim crystallization promoter, recycles, after low-pressure distillation Water return to step (1) in be continuing with.
The addition of above-mentioned crystallization promoter is the 0.5-5% of separating liquid weight.
Above-mentioned crystallization promoter selects organic crystallization promoter.
The invention has the beneficial effects as follows: the present invention carries out crystallization treatment to desulphurization mother solution, and desalination speed is fast, efficiency high, no By-product produces, and equipment and Factory Building expense are low, and capital expenditure saves, and reaches green high-efficient and reclaims.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention realizes are easy to understand, tie below Close specific embodiment, the present invention is expanded on further.
Embodiment 1
A kind of low energy consumption, lead plaster desulphurization mother solution desalinating process quick, capable of circulation, comprise the following steps that:
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, according to the difference of scrap lead cream sulfur content, can formed Add water in the reactor of strong convection the ore pulp being configured to that solid content is 50% by scrap lead cream;
(2) to addition na interior in the ore pulp of step (1)2co3, wherein na2co3Addition be theoretical amount 1.3-1.4 Times, process does not need to heat;
(3) start reactor continuous stirring after 30 minutes, ore pulp is put into one and carries strong impaction, extruding, rubbing action Equipment in reacted, will apply in pbso in sweetening process4The pbco on surface3Layer open, makes pbso4In the solution with na2co3 Being fully contacted, thus improving desulfuration efficiency, reaching the purpose forcing desulfurization;
(4), after reacting 20 minutes, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster;
(5) desulphurization mother solution is squeezed into crystallizer, and add a certain amount of crystallization promoter, release after 30 minutes and carry out solid-liquid Separate, the secondary salt in desulphurization mother solution is removed, salt rejection rate is more than 93%.
Separating liquid after above-mentioned crystallization uses low-pressure distillation technology to reclaim crystallization promoter, recycles, after low-pressure distillation Water return to step (1) in be continuing with.
Embodiment 2
A kind of low energy consumption, lead plaster desulphurization mother solution desalinating process quick, capable of circulation, comprise the following steps that:
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, according to the difference of scrap lead cream sulfur content, can formed Add water in the reactor of strong convection the ore pulp being configured to that solid content is 50% by scrap lead cream;
(2) to addition na interior in the ore pulp of step (1)2co3, wherein na2co3Addition be theoretical amount 1.3-1.4 Times, process does not need to heat;
(3) start reactor continuous stirring after 30 minutes, ore pulp is put into one and carries strong impaction, extruding, rubbing action Equipment in reacted, will apply in pbso in sweetening process4The pbco on surface3Layer open, makes pbso4In the solution with na2co3 Being fully contacted, thus improving desulfuration efficiency, reaching the purpose forcing desulfurization;
(4), after reacting 20 minutes, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster;
(5) desulphurization mother solution is squeezed into crystallizer, and add a certain amount of crystallization promoter, release after 30 minutes and carry out solid-liquid Separate, the secondary salt in desulphurization mother solution is removed, salt rejection rate is more than 93%.
Separating liquid after above-mentioned crystallization uses low-pressure distillation technology to reclaim crystallization promoter, recycles, after low-pressure distillation Water return to step (1) in be continuing with.The addition of above-mentioned crystallization promoter is the 0.5-5% of separating liquid weight.
It should be understood by those skilled in the art that, the present invention is not restricted to the described embodiments, above-described embodiment and explanation Merely illustrating the principles of the invention described in book, without departing from the spirit and scope of the present invention, the present invention also has Various changes and modifications, these changes and improvements both fall within scope of the claimed invention.Claimed scope By appending claims and its equivalent thereof.

Claims (4)

1. a kind of low energy consumption, lead plaster desulphurization mother solution desalinating process quick, capable of circulation are it is characterised in that comprise the following steps that:
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, according to the difference of scrap lead cream sulfur content, right by force being formed Add water in the reactor of stream the ore pulp being configured to that solid content is 50% by scrap lead cream;
(2) to addition na interior in the ore pulp of step (1)2co3, wherein na2co3Addition be 1.3-1.4 times of theoretical amount, mistake Journey does not need to heat;
(3) start reactor continuous stirring after 30 minutes, ore pulp is put into one and carries strong impaction, extruding, the setting of rubbing action Reacted in standby, will be applied in pbso in sweetening process4The pbco on surface3Layer open, makes pbso4In the solution with na2co3Fully Contact;
(4), after reacting 20 minutes, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster;
(5) desulphurization mother solution is squeezed into crystallizer, and add a certain amount of crystallization promoter, release after 30 minutes and carry out solid-liquid and divide From removing to the secondary salt in desulphurization mother solution.
2. a kind of low energy consumption according to claim 1, lead plaster desulphurization mother solution desalinating process quick, capable of circulation, its feature exists In the separating liquid after above-mentioned crystallization uses low-pressure distillation technology to reclaim crystallization promoter, recycles, and the water after low-pressure distillation returns Return in step (1) and be continuing with.
3. a kind of low energy consumption according to claim 1, lead plaster desulphurization mother solution desalinating process quick, capable of circulation, its feature exists In the addition of above-mentioned crystallization promoter is the 0.5-5% of separating liquid weight.
4. a kind of low energy consumption according to claim 1, lead plaster desulphurization mother solution desalinating process quick, capable of circulation, its feature exists In above-mentioned crystallization promoter selects organic crystallization promoter.
CN201610725560.2A 2016-08-25 2016-08-25 Low-energy-consumption, quick and recyclable lead paste desulfurization mother liquid desalinating process Pending CN106367594A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950235A (en) * 2018-07-19 2018-12-07 芜湖青悠静谧环保科技有限公司 A kind of recovery method of the pre- desulphurization mother solution of lead plaster
CN110042247A (en) * 2019-04-26 2019-07-23 南京工程学院 The recycle device and method of scrap lead cream in a kind of lead-acid accumulator

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US20060018819A1 (en) * 2004-07-20 2006-01-26 Engitech S.R.I. Desulfurization process of pastel and grids of lead accumulators
CN103540741A (en) * 2013-11-05 2014-01-29 湖南江冶机电科技股份有限公司 Forcible wet desulphurization process for lead plaster
CN104140115A (en) * 2014-08-25 2014-11-12 湖南江冶机电科技股份有限公司 Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters
CN104263944A (en) * 2014-09-29 2015-01-07 湖南江冶机电科技股份有限公司 Lead paste desulfurization method based on grinding mechanism
CN105420489A (en) * 2015-11-28 2016-03-23 湘潭大学 Diachylon desulphurization method based on throttling self-collision

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US20060018819A1 (en) * 2004-07-20 2006-01-26 Engitech S.R.I. Desulfurization process of pastel and grids of lead accumulators
CN103540741A (en) * 2013-11-05 2014-01-29 湖南江冶机电科技股份有限公司 Forcible wet desulphurization process for lead plaster
CN104140115A (en) * 2014-08-25 2014-11-12 湖南江冶机电科技股份有限公司 Method and device for recovering anhydrous sodium sulfate from filtrate after purification treatment of desulfurated lead plasters
CN104263944A (en) * 2014-09-29 2015-01-07 湖南江冶机电科技股份有限公司 Lead paste desulfurization method based on grinding mechanism
CN105420489A (en) * 2015-11-28 2016-03-23 湘潭大学 Diachylon desulphurization method based on throttling self-collision

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108950235A (en) * 2018-07-19 2018-12-07 芜湖青悠静谧环保科技有限公司 A kind of recovery method of the pre- desulphurization mother solution of lead plaster
CN110042247A (en) * 2019-04-26 2019-07-23 南京工程学院 The recycle device and method of scrap lead cream in a kind of lead-acid accumulator
CN110042247B (en) * 2019-04-26 2020-08-04 南京工程学院 Recycling device and method for waste lead plaster in waste lead-acid storage battery

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Application publication date: 20170201

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