CN107863582A - The removal technique of metallic lead in a kind of old and useless battery encapsulating material - Google Patents
The removal technique of metallic lead in a kind of old and useless battery encapsulating material Download PDFInfo
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- CN107863582A CN107863582A CN201710971242.9A CN201710971242A CN107863582A CN 107863582 A CN107863582 A CN 107863582A CN 201710971242 A CN201710971242 A CN 201710971242A CN 107863582 A CN107863582 A CN 107863582A
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- encapsulating material
- old
- useless battery
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- metallic lead
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to old and useless battery material recovery, specifically, it is related to a kind of removal technique of metallic lead in old and useless battery encapsulating material, including：(1) collect the encapsulating material of old and useless battery and be broken into powder；(2) acid solution soaks, and filtering, surfactant is mixed into filter residue, adds in ball mill and grinds；(3) soak, filter in acid solution again, wash, drying；(4) by after drying filter residue input comminutor in, after melting, extrude, cool down pelletizing obtain encapsulating material returns finished product；The present invention is leached using solution, and grinding proposes the mode being combined, and avoids the waste of water resource caused by removing metallic lead using the mode of warm water shower；The content of metallic lead in encapsulating material returns is effectively reduced, the phenomenon that battery caused by the presence of metallic lead uninterruptedly discharges when thoroughly having prevented old and useless battery encapsulating material returns use in the prior art.
Description
Technical field
The present invention relates to old and useless battery material recovery, specifically, being related to metallic lead in a kind of old and useless battery encapsulating material
Remove technique.
Background technology
The battery that automobile, electric bicycle use at present is mainly lead-acid accumulator, and its cost is cheap, manufacturing process is simple
It is single, occupied an leading position in electric bicycle market, 2011, the yield of national lead-acid accumulator reached 2.4 hundred million kilovolt-amperes
When.Automobile, the service life of lead-acid accumulator of electric bicycle are a year and a half to time of 2 years, although strictly being pressed during production
According to process control quality, can after half a year many batteries all can aging so as to shortening its service life.It is waste and old automobile, electronic
Bicycle lead-acid accumulator increases year by year, and total amount is huge, and very big influence is caused to environment.
For the discarded lead-acid accumulator of scientific and normal recovery, country has set up special recovery market, plumbic acid
The recovery of battery includes the steps such as the recovery of lead, the recycling of shell, the separation of acid solution.The shell of lead-acid accumulator with
Based on PP, so the development of the recovery and reuse technology of PP shells, not only sends out for a long time for electric bicycle lead-acid accumulator industry
Exhibition provides safeguard, and even more saves the requirement for the sustainable development that raw material and resource secondary utilize.
Recovery method of the prior art is all simple broken, adds part of auxiliary and is regenerated, and after crushing
Containing metal ions such as a small amount of lead elements in casing material, the lead-acid accumulator after preparing is caused uninterrupted electric discharge phenomena to be present,
So that the service life of lead-acid accumulator shortens.Applicant of the present invention is in Application No. " CN 201510181654.3 ", patent
Disclosed in entitled " junked-auto, the micro- lead of electric car lead-acid battery shell again separating technology " and a kind of improve old and useless battery encapsulation
The separating technology of micro lead in material, the technique effectively realize the reduction of the content of metallic lead in reworked material, prevented wherein
The lead element of residual influences the normal work of lead-acid accumulator.Its key takeaway is " alternating temperature shower precipitation " technology, is removing
Need to expend substantial amounts of water during lead, cause a large amount of wastes of water resource.
The content of the invention
It is an object of the invention to provide a kind of removal technique of metallic lead in old and useless battery encapsulating material, metal is being ensured
While effective reduction of lead content, processing cost is reduced, while avoids polluting environment.
To achieve these goals, the present invention is achieved using following technical scheme：
The removal technique of metallic lead, comprises the following steps in a kind of old and useless battery encapsulating material：
(1) collect the encapsulating material of old and useless battery and be broken into powder；
(2) encapsulating material powder is immersed into acid solution and soaks 3-5h, stirred in immersion process every 20min
10min；Filtering, the surfactant of 0.01-0.2 times of weight is mixed into filter residue, is stirred, and is then added in ball mill and is ground
Mill；
(3) filter residue after ball milling is immersed into acid solution again and soaks 3-5h, filtered, washed 2-3 times, drying；
(4) by after drying filter residue input comminutor in, after melting, extrude, cool down pelletizing obtain encapsulating material reuse
Expect finished product；
Wherein, the pH of the tie rod cooling water of fused mass is 8.5-9.
For the ease of operating and improving treatment effeciency, the present invention is first carried out the encapsulating material for the old and useless battery being collected into
Broken, crushing process is the conventional method of art, and the present invention does not have particular/special requirement to this, and after crushing, powder is crossed into 200 mesh
Sieve.
Encapsulating material powder is immersed into acid solution and soaks 3-5h, during this, the PbSO in encapsulating material powder4
And PbO2Rapidly it is dissolved into acid solution, in order to improve the efficiency of immersion, can selects in immersion process every one section
Time is stirred, and is then filtered, and filter residue is mixed with surfactant, and into ball mill grinding, grinding makes
Obtain encapsulating material powder to be ground out, so as to the PbSO contained in internal layer4And PbO2Expose and, then carry out immersion again and go
Remove.By aforesaid operations, the heavy metal elements such as the lead element in encapsulating material are removed, avoid occurring after being back to use encapsulating material
The phenomenon uninterruptedly discharged, shorten the service life of lead-acid accumulator.
The purpose of acid solution is in the lead-containing compounds in encapsulating material powder is dissolved in the present invention, and the present invention is to the acid
The species of property solution does not have special requirement, can often know for one of ordinary skill in the art, for example, the acid source can be
Inorganic acid and/or organic acid, the inorganic acid can be hydrochloric acid, nitric acid, sulfuric acid, boric acid, perchloric acid, thiocyanic acid, sulfurous acid, phosphorus
At least one of acid, phosphorous acid, hypochlorous acid etc.；The organic acid can be in formic acid, acetic acid, benzoic acid, benzene sulfonic acid etc.
It is at least one.
The dosage of described acid solution is necessary to ensure that encapsulating material powder can be totally submerged wherein, heretofore described
Encapsulating material powder and acid solution volume ratio be 1：(1.5-3)., it is further, described in order to improve the efficiency of immersion
Encapsulating material powder leaching process in keep the acid solution temperature to be 70-90 DEG C.
By adding surfactant, the surface free energy of encapsulating material powder is reduced, promotes PbSO in process of lapping4
And PbO2The solution modeling for being easy to next step to top layer is separated out, surfactant of the present invention is nonionic surfactant.
It is further preferred that the nonionic surfactant is ester type surfactant, ether type surfactant, amine type surface-active
At least one of agent, acid amide type surfactant and ester-ether type surfactant.It is specific as follows：Ester type surfactant can be with
For at least one of sorbitan fatty acid ester and polyoxyethylene fatty acid ester etc..Ether type surfactant can be polyoxy
At least one of vinyl alkyl alcohol ether and polyethenoxy alkylphenols etc..Amine surfactant can be Polyoxyethylene fatty
Amine etc..Acidamide surfactant can be such as polyoxyethylate amide.Ester ether surface active agent can be sorbitan esters of fatty
Acid ester polyoxyethylene ether type (tween type) etc..It is preferred that sorbitan fatty acid ester, polyoxyethylene fatty acid ester, polyoxyethylene fat
Fat amine, polyoxyethylate amide or APEO, more preferred polyoxyethylene fatty amine, polyoxyethylate amide or polyoxyethylene
Ether.Fat in wherein described fatty acid ester, fatty amine refers to C2-C4 straight-chain hydrocarbons.In alkyl alcohol ether, alkylbenzene phenolic ether
Alkyl is C2-C4 straight-chain hydrocarbons.
Operated, the most of minor metallic element contained in old and useless battery encapsulating material is removed, so by above-mentioned processing
It is granulated afterwards by comminutor, is easy to the use that subsequently feeds intake, in of the invention, described comminutor is double screw extruder, specifically,
The SHJ-20 type equidirectional parallel double-screw extruders of Nanjing Jie Ya Equipment Limiteds manufacture, screw speed 50- can be selected
80r/min, each area's temperature of double screw extruder are：One area：150-152 DEG C, 2nd area：155-157 DEG C, 3rd area：158-160
DEG C, 4th area：163-165 DEG C, 5th area：163-165 DEG C, 6th area：165-167℃.
It is granulated obtained graininess encapsulating material returns again by melting mixing, when tie rod cools down, can passes through
The heavy metal element for the very low amounts that cooling water contains to appearance carries out leaching proposition, and the pH of tie rod cooling water is 8.5-9, by this
The cooling water of alkalescence further leaches to the trace meter in fused mass, the further content for reducing trace meter.
The present invention has following technique effect：
1st, the removal technique of metallic lead of the present invention, is leached using solution, and grinding proposes the mode being combined, and avoids
The waste of water resource caused by using the mode of warm water shower removing metallic lead；
2nd, in old and useless battery encapsulating material proposed by the present invention metallic lead removal technique, effectively reduce encapsulating material
The content of metallic lead in returns, metallic lead during old and useless battery encapsulating material returns use is in the prior art thoroughly prevented
The phenomenon that the battery in the presence of caused by uninterruptedly discharges, greatly improve the service life and electricity of lead-acid accumulator.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is furture elucidated.
Embodiment 1
The removal technique of metallic lead in a kind of old and useless battery encapsulating material：
(1) collect the encapsulating material of old and useless battery and be broken into powder, powder is crossed into 200 mesh sieves；
(2) encapsulating material powder is immersed into hydrochloric acid solution and soaks 4h, it is 80 DEG C to keep hydrochloric acid solution temperature, package material
The volume ratio of feed powder end and hydrochloric acid solution is 1：2,10min is stirred every 20min in immersion process；Filtering, is mixed into filter residue
The sorbitan fatty acid ester of 0.1 times of weight, stirs, and then adds in ball mill and grinds；
(3) filter residue after ball milling is immersed into hydrochloric acid solution again and soaks 4h, the encapsulating material powder and hydrochloric acid are molten
The volume ratio of liquid is 1：2, it is 8 DEG C to keep hydrochloric acid solution temperature, filtering, is washed 2 times, drying；
(4) filter residue after drying is put into double screw extruder, screw speed 70r/min, each area of comminutor
Temperature is：One area：152 DEG C, 2nd area：156 DEG C, 3rd area：159 DEG C, 4th area：164 DEG C, 5th area：164 DEG C, 6th area：166 DEG C, through molten
Melt, extrude, cool down after pelletizing obtain encapsulating material returns finished product；
Wherein, the pH of the tie rod cooling water of fused mass is 8.6.
Embodiment 2
The removal technique of metallic lead in a kind of old and useless battery encapsulating material：
(1) collect the encapsulating material of old and useless battery and be broken into powder, powder is crossed into 200 mesh sieves；
(2) encapsulating material powder is immersed into salpeter solution and soaks 3h, it is 70 DEG C to keep salpeter solution temperature, package material
The volume ratio of feed powder end and salpeter solution is 1：1.5,10min is stirred every 20min in immersion process；Filtering, mixed into filter residue
Enter the polyoxyethylene fatty acid ester of 0.01 times of weight, stir, then add in ball mill and grind；
(3) filter residue after ball milling is immersed into salpeter solution again and soaks 3h, the encapsulating material powder and nitric acid are molten
The volume ratio of liquid is 1：1.5, it is 70 DEG C to keep salpeter solution temperature, filtering, is washed 2 times, drying；
(4) filter residue after drying is put into double screw extruder, screw speed 50r/min, each area of comminutor
Temperature is：One area：150 DEG C, 2nd area：155 DEG C, 3rd area：158 DEG C, 4th area：163 DEG C, 5th area：163 DEG C, 6th area：165 DEG C, through molten
Melt, extrude, cool down after pelletizing obtain encapsulating material returns finished product；
Wherein, the pH of the tie rod cooling water of fused mass is 8.5.
Embodiment 3
The removal technique of metallic lead in a kind of old and useless battery encapsulating material：
(1) collect the encapsulating material of old and useless battery and be broken into powder, powder is crossed into 200 mesh sieves；
(2) encapsulating material powder is immersed into sulfuric acid solution and soaks 5h, it is 90 DEG C to keep sulfuric acid solution temperature, package material
The volume ratio of feed powder end and sulfuric acid solution is 1：3,10min is stirred every 20min in immersion process；Filtering, is mixed into filter residue
The polyoxyethylene fatty amine of 0.2 times of weight, stirs, and then adds in ball mill and grinds；
(3) filter residue after ball milling is immersed into sulfuric acid solution again and soaks 5h, the encapsulating material powder and sulfuric acid are molten
The volume ratio of liquid is 1：3, it is 90 DEG C to keep sulfuric acid solution temperature, filtering, is washed 3 times, drying；
(4) filter residue after drying is put into double screw extruder, screw speed 80r/min, each area of comminutor
Temperature is：One area：152 DEG C, 2nd area：157 DEG C, 3rd area：160 DEG C, 4th area：165 DEG C, 5th area：165 DEG C, 6th area：167 DEG C, through molten
Melt, extrude, cool down after pelletizing obtain encapsulating material returns finished product；
Wherein, the pH of the tie rod cooling water of fused mass is 9.
Performance test：
Encapsulating material returns finished product and undressed encapsulating material are obtained in Example 1-3, uses Japanese Shimadzu
X-ray fluorescence analysis device EDX-LE processed is analyzed micro heavy content therein, and test result recorded in table 1.
Table 1
It can be seen from data above in old and useless battery encapsulating material provided by the invention metallic lead removal technique, pole
The big content for reducing wherein metallic lead.
General principle, principal character and the features of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement is both fallen within the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.
Claims (4)
- A kind of 1. removal technique of metallic lead in old and useless battery encapsulating material, it is characterised in that：Comprise the following steps：(1) collect the encapsulating material of old and useless battery and be broken into powder；(2) encapsulating material powder is immersed into acid solution and soaks 3-5h, 10min is stirred every 20min in immersion process；Cross Filter, the surfactant of 0.01-0.2 times of weight is mixed into filter residue, is stirred, and is then added in ball mill and is ground；(3) filter residue after ball milling is immersed into acid solution again and soaks 3-5h, filtered, washed 2-3 times, drying；(4) by after drying filter residue input comminutor in, after melting, extrude, cool down pelletizing obtain encapsulating material returns into Product；Wherein, the pH of the tie rod cooling water of fused mass is 8.5-9.
- 2. the removal technique of metallic lead in old and useless battery encapsulating material according to claim 1, it is characterised in that：In step (2), in (3), the volume ratio of described encapsulating material powder and acid solution is 1：(1.5-3).
- 3. the removal technique of metallic lead in old and useless battery encapsulating material according to claim 1, it is characterised in that：In step (2) it is 70-90 DEG C that acid solution temperature is kept, in (3), in encapsulating material powder leaching process.
- 4. the removal technique of metallic lead in old and useless battery encapsulating material according to claim 1, it is characterised in that：In step (4) in, described comminutor is double screw extruder, screw speed 50-80r/min；And/orEach area's temperature of comminutor is：One area：150-152 DEG C, 2nd area：155-157 DEG C, 3rd area：158-160 DEG C, 4th area： 163-165 DEG C, 5th area：163-165 DEG C, 6th area：165-167℃.
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| CN201710971242.9A CN107863582B (en) | 2017-10-18 | 2017-10-18 | The removal technique of metallic lead in a kind of old and useless battery encapsulating material |
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| CN101722175A (en) * | 2009-11-10 | 2010-06-09 | 伟翔环保科技发展(上海)有限公司 | Method for producing thermoplastic plastics by recycling nonmetal materials of discarded printed circuit boards and related thermoplastic plastics |
| CN103928726A (en) * | 2014-04-10 | 2014-07-16 | 界首市双特新材料科技有限公司 | Integrated energy-saving processing process for modified reprocessed plastic |
| CN104626516A (en) * | 2014-12-15 | 2015-05-20 | 曹承君 | Bracing, pelletizing and molding device and bracing, pelletizing and molding method for ultrahigh-liquidity thermoplastic resin |
| CN106058350A (en) * | 2016-07-18 | 2016-10-26 | 安徽省华鑫铅业集团有限公司 | Environment-friendly treatment process for waste lead-acid storage battery |
-
2017
- 2017-10-18 CN CN201710971242.9A patent/CN107863582B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101246979A (en) * | 2008-03-19 | 2008-08-20 | 陈永松 | Method for treating waste lead storage battery |
| CN101722175A (en) * | 2009-11-10 | 2010-06-09 | 伟翔环保科技发展(上海)有限公司 | Method for producing thermoplastic plastics by recycling nonmetal materials of discarded printed circuit boards and related thermoplastic plastics |
| CN103928726A (en) * | 2014-04-10 | 2014-07-16 | 界首市双特新材料科技有限公司 | Integrated energy-saving processing process for modified reprocessed plastic |
| CN104626516A (en) * | 2014-12-15 | 2015-05-20 | 曹承君 | Bracing, pelletizing and molding device and bracing, pelletizing and molding method for ultrahigh-liquidity thermoplastic resin |
| CN106058350A (en) * | 2016-07-18 | 2016-10-26 | 安徽省华鑫铅业集团有限公司 | Environment-friendly treatment process for waste lead-acid storage battery |
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Denomination of invention: A process for removing metal lead from waste battery packaging materials Effective date of registration: 20201203 Granted publication date: 20191001 Pledgee: The development of small and medium-sized enterprises financing Company Limited by Guarantee Jieshou City Pledgor: JIESHOU SHUANGTE NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2020980008804 |
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Denomination of invention: A Process for Removing Metal Lead from Waste Battery Packaging Materials Granted publication date: 20191001 Pledgee: The development of small and medium-sized enterprises financing Company Limited by Guarantee Jieshou City Pledgor: Anhui Tianlu New Material Co.,Ltd. Registration number: Y2024980016951 |