CN106435194A - Efficient desulfurization technology for waste lead-acid cell lead plaster - Google Patents
Efficient desulfurization technology for waste lead-acid cell lead plaster Download PDFInfo
- Publication number
- CN106435194A CN106435194A CN201610874467.8A CN201610874467A CN106435194A CN 106435194 A CN106435194 A CN 106435194A CN 201610874467 A CN201610874467 A CN 201610874467A CN 106435194 A CN106435194 A CN 106435194A
- Authority
- CN
- China
- Prior art keywords
- lead
- lead plaster
- waste
- waste lead
- ore pulp
- 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.)
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Classifications
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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
- 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
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
The invention discloses an efficient desulfurization technology for waste lead-acid cell lead plaster. The technology comprises the steps that firstly, the waste lead plaster generated during dismounting of a waste lead-acid cell is collected and placed in a freezing device to be frozen; secondly, the frozen waste lead plaster is placed in a nylon ball milling tank, an agate ball serves as a milling ball, ball milling is continuously conducted for 2 hours, waste lead plaster powder is obtained, and drying and refining are facilitated after grinding; thirdly, according to the fact that the waste lead plaster powder is different in sulfur content, water is added in the waste lead plaster in a reaction kettle capable of forming strong convection, and then the ore pulp with the mass percent ranging from 35% to 65% is prepared; fourthly, Na2CO3 is added in the ore pulp, the adding amount of the Na2CO3 is larger than the theoretical usage amount calculated according to the sulfur content of the waste lead plaster by 1.3-1.4 times, and stirring is continuously conducted for 25 min-35 min after Na2CO3 is added; fifthly, the ore pulp is placed in a reaction kettle capable of generating strong collision, extrusion and friction actions to be subjected to the reaction; and sixthly, after the reaction is conducted for 20 min-30 min, the reactant is subjected to solid and liquid separation, and the desulfurized mother liquor and the desulfurized lead plaster are obtained.
Description
Technical field
The present invention relates to reviver technical field is and in particular to a kind of waste lead acid battery lead plaster high-efficiency desulfurization 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.Chinese patent literature CN103880630A and
CN103771459A etc. is all using the method, but the method, when adding desulfurizing agent excessive (pH 10), can produce impurity NaPb2
(CO3)2OH；When desulfurizing agent is not enough, have part PbSO again4Cannot desulfurization.Chinese patent literature CN103523820A is using containing
Amino material and the method for carbonaceous material desulfurization, make the desulfurization degree of scrap lead cream reach 99%；Chinese patent literature
It is 1 with the molar ratio of sodium bicarbonate that CN103374657A adopts sodium carbonate：The sulfur method of 2 compound desulfuration solution, makes to give up
The desulfurization degree of lead plaster has reached more than 98.5%.Above sulfur removal technology obtains target product after needing roasting or electrolysis, and flow process is longer,
There is the shortcomings of, high energy consumption high to production equipment requirements, long flow path.
Content of the invention
The technical problem to be solved is to provide a kind of method simple, good in economic efficiency, free of contamination waste and old
Lead-acid battery lead plaster high-efficiency desulfurization technique.
The technical problem to be solved employs the following technical solutions to realize：
A kind of waste lead acid battery lead plaster high-efficiency desulfurization technique, comprises the following steps that：
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, be placed in freezing equipment, at a temperature of -25 DEG C
Freezed, cooling time is to expand it is therefore an objective to make lead plaster interior tissue produce for 30～60 minutes, improves follow-up grinding technics.
(2) the scrap lead cream after freezing is put in nylon ball grinder, with agate ball as abrading-ball, ball material mass ratio is 6：1,
Under conditions of rotating speed is 150 revs/min, continuous ball milling 2 hours, obtain scrap lead cream powder, be beneficial to after grinding dry and refine；
(3) difference according to scrap lead cream powder sulfur content, joins being formed in the reactor of strong convection, scrap lead cream to add water
It is set to the ore pulp of mass fraction 35%-65%；
(4) to addition Na interior in the ore pulp of step (3)2CO3, wherein Na2CO3Addition be according to waste diachylon sulfur-bearing
1.3-1.4 times of the theoretical amount that amount calculates, adds continuous stirring 25-35 minute after sodium carbonate, and process does not need to heat；
(5) ore pulp is put in a reactor that can produce strong impaction, extruding, rubbing action and reacted, by desulfurization
During apply in PbSO4The PbCO on surface3Layer open, makes PbSO4In the solution with Na2CO3It is fully contacted, thus improving desulfurization effect
Rate, reaches the purpose forcing desulfurization；
(6), after reaction 20-30 minute, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster；
Wherein unnecessary in desulphurization mother solution Na2CO3Removed using the lead sulfate in waste diachylon lead plaster, it is unnecessary to remove
Na2CO3The direct desalination of desulphurization mother solution, desulfurization lead plaster wash water uses as configuring new doctor solution, can be with return to step (3), use
In preparing ore pulp.
The invention has the beneficial effects as follows：The inventive method is simple, solves the halfway defect of traditional sulfur removal technology,
Abrasive, low energy consumption, low cost, belong to green high-efficient and reclaim project, be conducive to innoxious to used and scrapped battery regenerated resources
Comprehensive utilization and green reclaim.
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 waste lead acid battery lead plaster high-efficiency desulfurization technique, comprises the following steps that：
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, be placed in freezing equipment, at a temperature of -25 DEG C
Freezed, cooling time is to expand it is therefore an objective to make lead plaster interior tissue produce for 30 minutes, improves follow-up grinding technics.
(2) the scrap lead cream after freezing is put in nylon ball grinder, with agate ball as abrading-ball, ball material mass ratio is 6：1,
Under conditions of rotating speed is 150 revs/min, continuous ball milling 2 hours, obtain scrap lead cream powder, be beneficial to after grinding dry and refine；
(3) difference according to scrap lead cream powder sulfur content, joins being formed in the reactor of strong convection, scrap lead cream to add water
It is set to the ore pulp of mass fraction 35%；
(4) to addition Na interior in the ore pulp of step (3)2CO3, wherein Na2CO3Addition be according to waste diachylon sulfur-bearing
1.3-1.4 times of the theoretical amount that amount calculates, adds continuous stirring 25-35 minute after sodium carbonate, and process does not need to heat；
(5) ore pulp is put in a reactor that can produce strong impaction, extruding, rubbing action and reacted, by desulfurization
During apply in PbSO4The PbCO on surface3Layer open, makes PbSO4In the solution with Na2CO3It is fully contacted, thus improving desulfurization effect
Rate, reaches the purpose forcing desulfurization；
(6), after reaction 20-30 minute, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster；
Wherein unnecessary in desulphurization mother solution Na2CO3Removed using the lead sulfate in waste diachylon lead plaster, it is unnecessary to remove
Na2CO3The direct desalination of desulphurization mother solution, desulfurization lead plaster wash water uses as configuring new doctor solution, can be with return to step (3), use
In preparing ore pulp.
Embodiment 2
A kind of waste lead acid battery lead plaster high-efficiency desulfurization technique, comprises the following steps that：
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, be placed in freezing equipment, at a temperature of -25 DEG C
Freezed, cooling time is to expand it is therefore an objective to make lead plaster interior tissue produce for 60 minutes, improves follow-up grinding technics.
(2) the scrap lead cream after freezing is put in nylon ball grinder, with agate ball as abrading-ball, ball material mass ratio is 6：1,
Under conditions of rotating speed is 150 revs/min, continuous ball milling 2 hours, obtain scrap lead cream powder, be beneficial to after grinding dry and refine；
(3) difference according to scrap lead cream powder sulfur content, joins being formed in the reactor of strong convection, scrap lead cream to add water
It is set to the ore pulp of mass fraction 65%；
(4) to addition Na interior in the ore pulp of step (3)2CO3, wherein Na2CO3Addition be according to waste diachylon sulfur-bearing
1.3-1.4 times of the theoretical amount that amount calculates, adds continuous stirring 25-35 minute after sodium carbonate, and process does not need to heat；
(5) ore pulp is put in a reactor that can produce strong impaction, extruding, rubbing action and reacted, by desulfurization
During apply in PbSO4The PbCO on surface3Layer open, makes PbSO4In the solution with Na2CO3It is fully contacted, thus improving desulfurization effect
Rate, reaches the purpose forcing desulfurization；
(6), after reaction 20-30 minute, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster；
Wherein unnecessary in desulphurization mother solution Na2CO3Removed using the lead sulfate in waste diachylon lead plaster, it is unnecessary to remove
Na2CO3The direct desalination of desulphurization mother solution, desulfurization lead plaster wash water uses as configuring new doctor solution, can be with return to step (3), use
In preparing ore pulp.
Embodiment 3
A kind of waste lead acid battery lead plaster high-efficiency desulfurization technique, comprises the following steps that：
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, be placed in freezing equipment, at a temperature of -25 DEG C
Freezed, cooling time is to expand it is therefore an objective to make lead plaster interior tissue produce for 45 minutes, improves follow-up grinding technics.
(2) the scrap lead cream after freezing is put in nylon ball grinder, with agate ball as abrading-ball, ball material mass ratio is 6：1,
Under conditions of rotating speed is 150 revs/min, continuous ball milling 2 hours, obtain scrap lead cream powder, be beneficial to after grinding dry and refine；
(3) difference according to scrap lead cream powder sulfur content, joins being formed in the reactor of strong convection, scrap lead cream to add water
It is set to the ore pulp of mass fraction 45%；
(4) to addition Na interior in the ore pulp of step (3)2CO3, wherein Na2CO3Addition be according to waste diachylon sulfur-bearing
1.3-1.4 times of the theoretical amount that amount calculates, adds continuous stirring 25-35 minute after sodium carbonate, and process does not need to heat；
(5) ore pulp is put in a reactor that can produce strong impaction, extruding, rubbing action and reacted, by desulfurization
During apply in PbSO4The PbCO on surface3Layer open, makes PbSO4In the solution with Na2CO3It is fully contacted, thus improving desulfurization effect
Rate, reaches the purpose forcing desulfurization；
(6), after reaction 20-30 minute, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster；
Wherein unnecessary in desulphurization mother solution Na2CO3Removed using the lead sulfate in waste diachylon lead plaster, it is unnecessary to remove
Na2CO3The direct desalination of desulphurization mother solution, desulfurization lead plaster wash water uses as configuring new doctor solution, can be with return to step (3), use
In preparing ore pulp.
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 (5)
1. a kind of waste lead acid battery lead plaster high-efficiency desulfurization technique is it is characterised in that comprise the following steps that：
(1) collect the scrap lead cream that waste lead acid battery disassembles middle generation, be placed in freezing equipment, carry out at a temperature of -25 DEG C
Freezing, cooling time is 30～60 minutes；
(2) the scrap lead cream after freezing is put in nylon ball grinder, with agate ball as abrading-ball, ball material mass ratio is 6：1, in rotating speed
Under conditions of 150 revs/min, continuous ball milling 2 hours, obtain scrap lead cream powder, be beneficial to after grinding dry and refine；
(3) difference according to scrap lead cream powder sulfur content, is configured to being formed in the reactor of strong convection, scrap lead cream to add water
The ore pulp of mass fraction 35%-65%；
(4) to addition Na interior in the ore pulp of step (3)2CO3, wherein Na2CO3Addition be according to waste diachylon sulfur content calculate
1.3-1.4 times of theoretical amount, add continuous stirring 25-35 minute after sodium carbonate, process does not need to heat；
(5) ore pulp is put in a reactor that can produce strong impaction, extruding, rubbing action and reacted, by sweetening process
In apply in PbSO4The PbCO on surface3Layer open, makes PbSO4In the solution with Na2CO3It is fully contacted；
(6), after reaction 20-30 minute, solid-liquid separation is carried out to reactant, obtains desulphurization mother solution and desulfurization lead plaster.
2. waste lead acid battery lead plaster high-efficiency desulfurization technique matter content according to claim 1 method it is characterised in that
Wherein unnecessary in desulphurization mother solution Na2CO3Removed using the lead sulfate in waste diachylon lead plaster, remove unnecessary Na2CO3Desulfurization
The direct desalination of mother solution, desulfurization lead plaster wash water uses as configuring new doctor solution, in return to step (3), is used for preparing ore pulp.
3. waste lead acid battery lead plaster high-efficiency desulfurization technique matter content according to claim 1 method it is characterised in that
In above-mentioned steps (1), cooling time is 30 minutes.
4. waste lead acid battery lead plaster high-efficiency desulfurization technique matter content according to claim 1 method it is characterised in that
In above-mentioned steps (1), cooling time is 60 minutes.
5. waste lead acid battery lead plaster high-efficiency desulfurization technique matter content according to claim 1 method it is characterised in that
In above-mentioned steps (1), cooling time is 45 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610874467.8A CN106435194A (en) | 2016-09-30 | 2016-09-30 | Efficient desulfurization technology for waste lead-acid cell lead plaster |
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| CN201610874467.8A CN106435194A (en) | 2016-09-30 | 2016-09-30 | Efficient desulfurization technology for waste lead-acid cell lead plaster |
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| CN106435194A true CN106435194A (en) | 2017-02-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834734A (en) * | 2017-03-18 | 2017-06-13 | 江西理工大学 | A kind of agitating ball mill high-efficiency desulfurization method |
| CN107117647A (en) * | 2017-05-22 | 2017-09-01 | 南京工程学院 | A kind of device for being used in lead-containing compounds purify ceruse |
| CN112375908A (en) * | 2020-10-26 | 2021-02-19 | 骆驼集团(安徽)再生资源有限公司 | Lead refining process for recycling lead-acid battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834734A (en) * | 2017-03-18 | 2017-06-13 | 江西理工大学 | A kind of agitating ball mill high-efficiency desulfurization method |
| CN107117647A (en) * | 2017-05-22 | 2017-09-01 | 南京工程学院 | A kind of device for being used in lead-containing compounds purify ceruse |
| CN112375908A (en) * | 2020-10-26 | 2021-02-19 | 骆驼集团(安徽)再生资源有限公司 | Lead refining process for recycling lead-acid battery |
| CN112375908B (en) * | 2020-10-26 | 2022-04-19 | 骆驼集团(安徽)再生资源有限公司 | Lead refining process for recycling lead-acid battery |
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