CN107464964A - From the method for lithium ion battery recovery N methyl pyrrolidones - Google Patents
From the method for lithium ion battery recovery N methyl pyrrolidones Download PDFInfo
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- CN107464964A CN107464964A CN201710656593.0A CN201710656593A CN107464964A CN 107464964 A CN107464964 A CN 107464964A CN 201710656593 A CN201710656593 A CN 201710656593A CN 107464964 A CN107464964 A CN 107464964A
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- CN
- China
- Prior art keywords
- methylpyrrolidone
- lithium ion
- ion battery
- battery recovery
- molecular sieve
- 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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- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Secondary Cells (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
Abstract
The present invention relates to a kind of method from lithium ion battery recovery N methyl pyrrolidones, N methyl pyrrolidone mother liquors are obtained using the waste material of electrode material of lithium battery as raw materials for production are processed, then by mother liquor rectifying, major impurity water and a small amount of heavy constituent are removed, then is further dehydrated through over-molecular sieve to obtain N methyl pyrrolidone finished products.The present invention reduce further rectifying and obtain the moisture of N methyl pyrrolidone crude products using molecular sieve dehydration energy consumption is low, free of contamination feature;The main content of N methyl pyrrolidones that the present invention obtains is high, moisture is low, meets the demand of LITHIUM BATTERY product.
Description
Technical field
The present invention relates to battery material field, more particularly to a kind of side that 1-METHYLPYRROLIDONE is reclaimed from lithium ion battery
Method.
Background technology
High with its energy density since lithium rechargeable battery comes out before and after the nineties, operating voltage is high, self discharge
It is small, have extended cycle life, memory-less effect, the advantages that security is good and environmentally friendly gradually takes in small-sized secondary batteries field
Turn into the main flow of commercial high-grade secondary cell for nickel-cadmium cell and Ni-MH battery, it is a variety of to turn into mobile phone, notebook computer etc.
The ideal source of portable electronic digital product, it is also the ideal source of electric automobile light high-energy electrokinetic cell.At present, with
Lithium rechargeable battery using more and more extensive, lithium ion battery manufacture quantity is also multiplied year by year, to lithium ion battery
Recovery it is also more and more, manufacture and removal process in caused waste and old 1-METHYLPYRROLIDONE it is also more and more, easily to ring
Border pollutes, therefore, it is necessary to be reclaimed to it.The recycling of 1-METHYLPYRROLIDONE had both overcome it to environment
Caused by pollution, make use of resource once more, not only with great economic interests, and also have great society in terms of environmental protection
Can meaning.
The waste material of electrode material of lithium battery obtains the 1-METHYLPYRROLIDONE mother liquor of high-moisture after roughing, through refined
The purpose of recycling can be reached after water removal.
The content of the invention
The present invention is intended to provide a kind of method from lithium ion battery recovery 1-METHYLPYRROLIDONE, is prepared main content
1-METHYLPYRROLIDONE high, water content is low, so as to be applied to again in lithium battery material.
A kind of method from lithium ion battery recovery 1-METHYLPYRROLIDONE of the present invention, including rectifying and molecular sieve water removal
Two steps;
The rectifying specifically comprises the following steps:
S1. the electrolyte of lithium ion battery is subjected to rectification and purification and obtains 1-METHYLPYRROLIDONE mother liquor, mother liquor reclaimed water contains
Measure as 1000-5000ppm;
S2. vacuumized after adding 1-METHYLPYRROLIDONE mother liquor in a kettle, absolute pressure≤1000Pa, be warming up to kettle
Warm 45-50 DEG C, partially liq is taken out from tower top, it is 2 to control reflux ratio:1-4:1, distillate main component now is water;
S3. it is persistently overheating to 110-120 DEG C of kettle temperature, it is thick to start collection cut 1-METHYLPYRROLIDONE when pushing up warm 70-80 DEG C
Product;
S4. 120-130 DEG C of kettle temperature is continuously heating to, pushes up warm 80-90 DEG C, the collection of 1-METHYLPYRROLIDONE crude product is completed;
The molecular sieve water removal specifically includes:By 1-METHYLPYRROLIDONE crude product injection efficient molecular sieve dehydration dress
Put, it is 20-50 DEG C to control temperature, stands 2-8 hours, is cooled to after room temperature to be dehydrated and produces 1-METHYLPYRROLIDONE finished product.
Preferably, heating rate is 0.5-2 DEG C/min in the step S2 and S3.
Preferably, heated up again after first adding water entrainer in the step S2.
Preferably, the water entrainer is the one or more in dimethylbenzene, toluene, hexamethylene.
Preferably, reflux ratio is 2 in the step S3:1-4:1.
Preferably, water content is 100-150ppm in the 1-METHYLPYRROLIDONE crude product.
Preferably, main content >=99.8% of the 1-METHYLPYRROLIDONE finished product.
Preferably, water content≤10ppm in the 1-METHYLPYRROLIDONE finished product.
The beneficial effects of the invention are as follows:
1) present invention is effectively returned using the waste material of lithium ion battery as reaction raw materials to 1-METHYLPYRROLIDONE
Receive and utilize, avoid and environment is polluted;
2) present invention reduce further rectifying and obtain N- methyl using molecular sieve dehydration energy consumption is low, free of contamination feature
The moisture of pyrrolidones crude product, moisture in crude product after rectifying is dropped into below 10ppm from 100-150ppm;
3) appropriate reflux ratio is controlled in the present invention, improves the main content of 1-METHYLPYRROLIDONE, while reduce water
Content;
4) setting of time of repose both ensure that dehydrating effect in molecular sieve removal process of the invention, in turn ensure that dehydration
Efficiency;
5) the main content of the obtained 1-METHYLPYRROLIDONE of the present invention is high, moisture is low, meets the demand of LITHIUM BATTERY product.
Embodiment
Embodiment 1
Present embodiment discloses a kind of method from lithium ion battery recovery 1-METHYLPYRROLIDONE, including rectifying and molecule
Two steps of water are screened out, the rectifying specifically comprises the following steps:The electrolyte of lithium ion battery is carried out into rectification and purification to obtain
1-METHYLPYRROLIDONE mother liquor, water content is 2000ppm in mother liquor;Then 2.5kg 1-METHYLPYRROLIDONE mother liquors are poured into instead
Answer in kettle, the use of toluene is water entrainer, open vavuum pump, it is 1000Pa to make absolute pressure, is warming up to 50 DEG C of kettle temperature, heating rate
For 0.5 DEG C/min, go out partially liq from overhead extraction, it is 3 to control reflux ratio:1, distillate main component now is water;After
It is continuous to be warming up to 110 DEG C of kettle temperature, 75 DEG C of top temperature, control reflux ratio 3:1, start to collect cut 1-METHYLPYRROLIDONE crude product, continue
120 DEG C of kettle temperature is warming up to, 80 DEG C of top temperature, obtains 2.39kgN- methyl pyrrolidone crude products, moisture 150ppm.
The molecular sieve water removal specifically includes:By 1-METHYLPYRROLIDONE crude product injection efficient molecular sieve dehydration dress
Put, it is 50 DEG C to control temperature, is dehydrated after standing 2 hours and produces 1-METHYLPYRROLIDONE finished product.It is too short if left standing for the time, can not
Ensure dehydrating effect, time of repose is long, then reduces dewatering efficiency;The setting of time of repose both ensure that dehydration in the present invention
Effect, it in turn ensure that dewatering efficiency.
The obtained main content of 1-METHYLPYRROLIDONE is 99.87% in the present embodiment, water content 10ppm, be can be used for
In the electrode material of lithium ion battery.
Embodiment 2
Present embodiment discloses a kind of method from lithium ion battery recovery 1-METHYLPYRROLIDONE, including rectifying and molecule
Two steps of water are screened out, the rectifying specifically comprises the following steps:The electrolyte of lithium ion battery is carried out into rectification and purification to obtain
1-METHYLPYRROLIDONE mother liquor, water content is 1000ppm in mother liquor;Then 2.5kg 1-METHYLPYRROLIDONE mother liquors are poured into instead
Answer in kettle, the use of dimethylbenzene is water entrainer, open vavuum pump, it is 500Pa to make absolute pressure, is warming up to 45 DEG C of kettle temperature, heating speed
Rate is 2 DEG C/min, and partially liq is taken out from tower top, and it is 2 to control reflux ratio:1, distillate main component now is water;Continue
120 DEG C of kettle temperature is warming up to, 72 DEG C of top temperature, controls reflux ratio 2:1, start to collect cut 1-METHYLPYRROLIDONE crude product, continue to rise
Temperature 90 DEG C of top temperature, obtains 2.37kgN- methyl pyrrolidone crude products, water content 100ppm to 130 DEG C of kettle temperature.
The molecular sieve water removal specifically includes:By 1-METHYLPYRROLIDONE crude product injection efficient molecular sieve dehydration dress
Put, it is 20 DEG C to control temperature, is dehydrated after standing 8 hours and produces 1-METHYLPYRROLIDONE finished product.It is too short if left standing for the time, can not
Ensure dehydrating effect, time of repose is long, then reduces dewatering efficiency;The setting of time of repose both ensure that dehydration in the present invention
Effect, it in turn ensure that dewatering efficiency.
The obtained main content of 1-METHYLPYRROLIDONE is 99.82% in the present embodiment, water content 8ppm, can be used for lithium
In the electrode material of ion battery.
Embodiment 3
It is 1 that the present embodiment, which controls the reflux ratio in course of reaction,:1, other reaction raw materials and experiment condition with embodiment 2
In it is identical.
The obtained main content of 1-METHYLPYRROLIDONE is 99.78% in the present embodiment, water content 50ppm.
By the contrast of embodiment 2 and embodiment 3 it can be found that controlling appropriate reflux ratio, N- methyl pyrroles are not only increased
The main content of pyrrolidone, while reduce water content.
Embodiment 4
Present embodiment discloses a kind of method from lithium ion battery recovery 1-METHYLPYRROLIDONE, including rectifying and molecule
Two steps of water are screened out, the rectifying specifically comprises the following steps:The electrolyte of lithium ion battery is carried out into rectification and purification to obtain
1-METHYLPYRROLIDONE mother liquor, water content is 4000ppm in mother liquor;Then 2.5kg 1-METHYLPYRROLIDONE mother liquors are poured into instead
Answer in kettle, the use of hexamethylene is water entrainer, open vavuum pump, it is 500Pa to make absolute pressure, is warming up to 45 DEG C of kettle temperature, heating speed
Rate is 1.5 DEG C/min, and partially liq is taken out from tower top, and it is 2.5 to control reflux ratio:1, distillate main component now is water;
120 DEG C of kettle temperature is continuously heating to, 75 DEG C of top temperature, controls reflux ratio 2.5:1, start to collect cut 1-METHYLPYRROLIDONE crude product,
130 DEG C of kettle temperature is continuously heating to, 90 DEG C of top temperature, obtains 2.38kg 1-METHYLPYRROLIDONE crude products, water content 30ppm.
The molecular sieve water removal specifically includes:By 1-METHYLPYRROLIDONE crude product injection efficient molecular sieve dehydration dress
Put, it is 50 DEG C to control temperature, is dehydrated after standing 4 hours and produces 1-METHYLPYRROLIDONE finished product.It is too short if left standing for the time, can not
Ensure dehydrating effect, time of repose is long, then reduces dewatering efficiency;The setting of time of repose both ensure that dehydration in the present invention
Effect, it in turn ensure that dewatering efficiency.
The obtained main content of 1-METHYLPYRROLIDONE is 99.89% in the present embodiment, water content 8.5ppm, be can be used for
In the electrode material of lithium ion battery.
The beneficial effects of the invention are as follows:
1) present invention is effectively returned using the waste material of lithium ion battery as reaction raw materials to 1-METHYLPYRROLIDONE
Receive and utilize, avoid and environment is polluted;
2) present invention reduce further rectifying and obtain N- methyl using molecular sieve dehydration energy consumption is low, free of contamination feature
The moisture of pyrrolidones crude product, moisture in crude product after rectifying is dropped into below 10ppm from 100-150ppm;
3) appropriate reflux ratio is controlled in the present invention, improves the main content of 1-METHYLPYRROLIDONE, while reduce water
Content;
4) setting of time of repose both ensure that dehydrating effect in molecular sieve removal process of the invention, in turn ensure that dehydration
Efficiency;
5) the main content of the obtained 1-METHYLPYRROLIDONE of the present invention is high, moisture is low, meets the demand of LITHIUM BATTERY product.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (8)
1. from the method for lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that including rectifying and molecular sieve water removal two
Individual step;
The rectifying specifically comprises the following steps:
S1. the electrolyte of lithium ion battery is subjected to rectification and purification and obtains 1-METHYLPYRROLIDONE mother liquor, water content is in mother liquor
1000-5000ppm;
S2. vacuumized after adding 1-METHYLPYRROLIDONE mother liquor in a kettle, absolute pressure≤1000Pa, be warming up to kettle temperature
45-50 DEG C, partially liq is taken out from tower top, it is 2 to control reflux ratio:1-4:1, distillate main component now is water;
S3. it is persistently overheating to 110-120 DEG C of kettle temperature, start to collect cut 1-METHYLPYRROLIDONE crude product when pushing up warm 70-80 DEG C;
S4. 120-130 DEG C of kettle temperature is continuously heating to, pushes up warm 80-90 DEG C, the collection of 1-METHYLPYRROLIDONE crude product is completed;
The molecular sieve water removal specifically includes:The 1-METHYLPYRROLIDONE crude product is injected into efficient molecular sieve dehydration device, control
Temperature processed is 20-50 DEG C, stands 2-8 hours, is cooled to after room temperature to be dehydrated and produces 1-METHYLPYRROLIDONE finished product.
2. the method according to claim 1 from lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that described
Heating rate is 0.5-2 DEG C/min in step S2 and S3.
3. the method according to claim 1 or 2 from lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that
Heated up again after first adding water entrainer in the step S2.
4. the method according to claim 3 from lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that described
Water entrainer is the one or more in dimethylbenzene, toluene, hexamethylene.
5. the method according to claim 4 from lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that described
Reflux ratio is 2 in step S3:1-4:1.
6. according to claim 1 or 5 from the method for lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that
Water content is 100-150ppm in the 1-METHYLPYRROLIDONE crude product.
7. the method according to claim 6 from lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that described
Main content >=99.8% of 1-METHYLPYRROLIDONE finished product.
8. the method according to claim 7 from lithium ion battery recovery 1-METHYLPYRROLIDONE, it is characterised in that described
Water content≤10ppm in 1-METHYLPYRROLIDONE finished product.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020029053A1 (en) * | 2018-08-07 | 2020-02-13 | 南通百川新材料有限公司 | Method for recovering n-methylpyrrolidone from lithium ion battery |
CN111138336A (en) * | 2019-12-31 | 2020-05-12 | 江苏中德电子材料科技有限公司 | Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone |
CN113173875A (en) * | 2021-05-12 | 2021-07-27 | 南京长江江宇环保科技有限公司 | Method for recycling N-methyl pyrrolidone from waste anode electrode slurry in lithium battery production |
CN113480464A (en) * | 2021-07-22 | 2021-10-08 | 哈尔滨万鑫石墨谷科技有限公司 | Method for extracting NMP solvent from conductive slurry |
CN114288999A (en) * | 2021-12-27 | 2022-04-08 | 东莞市鹏锦机械科技有限公司 | Specific water-absorbing composite material, preparation method thereof and application thereof in treatment of waste gas with high moisture content and low NMP content |
CN114907248A (en) * | 2022-06-02 | 2022-08-16 | 北京化工大学 | Method for recovering N-methyl pyrrolidone in lithium battery anode waste liquid |
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CN102544627A (en) * | 2010-12-29 | 2012-07-04 | 比亚迪股份有限公司 | Method for recycling N-methyl-2-pyrrolidone from lithium battery electrode material |
CN103664728A (en) * | 2012-09-26 | 2014-03-26 | 中山天贸电池有限公司 | Method for recovering nuclear matrix protein (NMP) solvent in production of lithium ion battery |
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JP2005238220A (en) * | 2004-01-30 | 2005-09-08 | Ryoka Forward Kk | Apparatus and method for recovering n-methyl-2-pyrrolidone |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020029053A1 (en) * | 2018-08-07 | 2020-02-13 | 南通百川新材料有限公司 | Method for recovering n-methylpyrrolidone from lithium ion battery |
CN111138336A (en) * | 2019-12-31 | 2020-05-12 | 江苏中德电子材料科技有限公司 | Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone |
CN113173875A (en) * | 2021-05-12 | 2021-07-27 | 南京长江江宇环保科技有限公司 | Method for recycling N-methyl pyrrolidone from waste anode electrode slurry in lithium battery production |
CN113480464A (en) * | 2021-07-22 | 2021-10-08 | 哈尔滨万鑫石墨谷科技有限公司 | Method for extracting NMP solvent from conductive slurry |
CN114288999A (en) * | 2021-12-27 | 2022-04-08 | 东莞市鹏锦机械科技有限公司 | Specific water-absorbing composite material, preparation method thereof and application thereof in treatment of waste gas with high moisture content and low NMP content |
CN114288999B (en) * | 2021-12-27 | 2024-06-07 | 东莞市鹏锦机械科技有限公司 | Specific water-absorbing composite material, preparation method thereof and application thereof in high-moisture low-NMP-content waste gas treatment |
CN114907248A (en) * | 2022-06-02 | 2022-08-16 | 北京化工大学 | Method for recovering N-methyl pyrrolidone in lithium battery anode waste liquid |
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Application publication date: 20171212 |