CN110436593A - A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid - Google Patents
A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid Download PDFInfo
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- CN110436593A CN110436593A CN201910759590.9A CN201910759590A CN110436593A CN 110436593 A CN110436593 A CN 110436593A CN 201910759590 A CN201910759590 A CN 201910759590A CN 110436593 A CN110436593 A CN 110436593A
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- anode
- nmp
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/122—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using filter presses
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Sludge (AREA)
Abstract
A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid carries out flocculation separation to spent anolyte with flocculant, then carries out filters pressing to gained flocculation gelatinous precipitate, and filtrate is the aqueous solution of NMP, and filter residue is the solid containing noble metal, carbon dust etc.；More thoroughly to realize that NMP is separated from waste liquid, by the way that diatomite is added, it is uniformly mixing to obtain diatomite mud；Filters pressing is carried out to diatomite mud again, realizes and is separated by solid-liquid separation.It can recycle NMP therein without heating energy consumption, be also convenient for recycling noble metal therein, and this method was not only economical, but also environmental protection, be suitble to industrialized production.Through testing, using separation method of the invention, the rate of recovery of NMP is up to 95% or more in spent anolyte.
Description
Technical field:
The present invention relates to the processing skills of the liquid waste disposal technique generated in Production Process of Lithium Battery more particularly to spent anolyte
Art.
Background technique:
In Production Process of Lithium Battery, spent anolyte can be all generated, currently, to the anode generated in Production Process of Lithium Battery
Waste liquid all carries out harmless treatment as waste liquid, costly according to existing harmless treatment scheme without recycling and reusing,
Generally at 20,000 yuan or more, this virtually increases the production cost of lithium battery.
The Main Components of spent anolyte are N methyl pyrrolidone (abbreviation NMP), nano-scale carbon powder particles, colloid substance, molten
Agent, inorganic salts and water etc..
In spent anolyte, NMP, noble metal, nano-scale carbon powder particles are all the raw materials for being worth reuse.Currently, someone couple
The anode waste material generated in Production Process of Lithium Battery has carried out flash distillation or heating evaporation processing test, can distill out part therein
NMP, and the higher waste residue of solid content is obtained, noble metal, nano-scale carbon powder particles wherein, pass through the side of this separation of solid and liquid
Although the waste residue that method can obtain useful NMP and can recycle, device therefor destilling tower easily incrustation cause to block, and
It is difficult cleaning vegetable to lead to, service life is not grown, while energy consumption is high, and the earning rate of recycling is too low, without commercial value, therefore, mesh
The commercial processes scheme of preceding maturation not yet.
Applicant tests distillation under vacuum, analyzes and calculates, although this method can be valuable constituent therein
NMP (N methyl pyrrolidone) is separated, but the recovery rate of object N methyl pyrrolidone is 75% or so, from waste liquid per ton
In the value of acquired N methyl pyrrolidone there was only 5000 yuan or so, consume energy very big, and equipment investment is big, integrated treatment
Cost is as high as 5500 yuan/ton, and obtained secondary liquid waste still needs to harmless treatment after processing, meanwhile, the equipment of vacuum distillation
Service life only has 1 year or so, and input-output ratio is extremely uneconomical.Therefore, this scheme is only limitted to test level, and the current country does not have
There are the scheme and case of industrial applications.
Summary of the invention:
The present invention provides a kind of methods of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid, it is without heating consumption
NMP therein can be recycled, this method was not only economical, but also environmental protection.
The technical solution adopted by the present invention is as follows:
A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid, it is characterized in that:
Including carrying out flocculation separation to spent anolyte with flocculant.
Further, the method for recycling N methyl pyrrolidone in Anode of lithium cell waste liquid, characterized in that including as follows
Step:
Step 1: spent anolyte is injected in processing pond；
Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond, after mixing evenly, stand
Precipitating 12 hours or more, supernatant liquid was the aqueous solution of NMP, and lower sediment thing is the flocculent gel for including carbon dust, noble metal, NMP
Shape sediment；
Step 3: carrying out filters pressing to gained flocculation gelatinous precipitate, filtrate is the aqueous solution of NMP, your gold filter residue is containing
The solid of category, carbon dust etc.；
Filtrate obtained in supernatant liquid and third step in second step is all the aqueous solution of NMP.
Further, the method for recycling N methyl pyrrolidone in Anode of lithium cell waste liquid, characterized in that including as follows
Step:
Step 1: spent anolyte is injected in processing pond；
Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond, after mixing evenly, then plus
Enter diatomite, is uniformly mixing to obtain diatomite mud；
Step 3 carries out filters pressing to diatomite mud, realizes and be separated by solid-liquid separation, obtain filtrate and filter residue, filtrate is the water of NMP
Solution, filter residue are the solids containing noble metal, carbon dust etc..
Further, the method for recycling N methyl pyrrolidone in Anode of lithium cell waste liquid, characterized in that including as follows
Step:
Step 1: spent anolyte is injected in processing pond；
Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond, it is after mixing evenly, static
12 hours or more, supernatant liquid be NMP aqueous solution, lower sediment thing be include carbon dust, noble metal, NMP flocculation gelatinous precipitate
Object；
Step 3: diatomite is added into flocculation gelatinous precipitate again, it is uniformly mixing to obtain diatomite mud, then to diatom
Native mud carries out filters pressing, realizes and is separated by solid-liquid separation, obtains filter residue and filtrate, filtrate is the aqueous solution of NMP, your gold filter residue is containing
Belong to, the solid of carbon dust.
Further, in above-mentioned recycling Anode of lithium cell waste liquid in the method for N methyl pyrrolidone, the diatomite
Additional amount is greater than the 1% of liquid quality to be processed.
Further, the additional amount of diatomite should be greater than the 5%~15% of liquid quality to be processed.
Further, in above-mentioned processing method, the flocculant is PAS polyaluminium sulfate, PAC aluminium polychloride, PFC
Poly-ferric chloride, PFS bodied ferric sulfate or 12 hydrazine aluminum sulfate potassium or their mixture.
Further, the flocculant is PAS polyaluminium sulfate, and PAC aluminium polychloride, PFC poly-ferric chloride, PFS are poly-
Close ferric sulfate or 12 hydrazine aluminum sulfate potassium.
Further, the flocculant is PAS polyaluminium sulfate.
Further, the filters pressing is to be greater than 10 kilograms using pressure, plate compression equipment more than 200 mesh of filter cloth.
The present invention is physics solid-liquid isolation method, can both be staticly settled after flocculant is added and first take out sediment, point
NMP aqueous solution and black gelatinous precipitate are separated out, then diatomite is added to black gelatinous precipitate and passes through after mixing evenly
Filters pressing mode isolates remaining NMP aqueous solution and the filter residue containing noble metal, carbon dust etc..Flocculant stirring can also be added
After uniformly, it is directly added into diatomite stirring, obtains NMP aqueous solution and filter residue finally by filters pressing.Through testing, using of the invention
Separation method, the rate of recovery of NMP is up to 95% or more in spent anolyte.
Specific embodiment:
A specific embodiment of the invention is exemplified below:
A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid includes the following steps:
Step 1: spent anolyte is injected in processing pond；
Pass through after mixing evenly Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond
Any one of following three kinds of paths are handled:
First paths: staticly settling 4 hours or more, and supernatant liquid is the aqueous solution of NMP, and lower sediment thing is precipitating glue
Shape flocculate precipitates gluey flocculate to gained and carries out filters pressing, filtrate is the water of NMP including carbon dust, noble metal and NMP
Solution, filter residue are the solid containing noble metal, carbon dust etc..
By this physics sedimentation method for separating, in former spent anolyte 95% NMP can be separated, be recycled
The aqueous solution of NMP, current market recycling valence is 10,000 yuan/ton or so；Solid containing noble metal, carbon dust etc. in filter residue is
The raw material of precious metal refineries enterprise, it is 2.5 ten thousand yuan/ton or so that valence is recycled in market.
Second paths: diatomite is added in the waste liquid obtained to step 2, stirs evenly, obtains diatomite mud, silicon
The additional amount of diatomaceous earth be greater than waste liquid quality to be processed 1%, preferably 1%~15%, diatomite addition more multiple pressure filter effect more
Good, filter cake is also more dry, selects the effect of superfine diatomite best, carries out filters pressing to diatomite mud, is obtained by being separated by solid-liquid separation
Filtrate and filter residue, filtrate are the aqueous solutions of NMP, and filter residue is the solid containing noble metal, carbon dust etc., are that noble metal and carbon dust return
Receive the raw material of enterprise.
Third path: after step 2 completion, static 12 hours or more, so that the complete flocculation sedimentation of carbon powder particle,
Supernatant liquor and the lower beds of precipitation are obtained, supernatant liquor is the aqueous solution of NMP, and the lower beds of precipitation are the glues containing noble metal, carbon dust
Flocculate is added diatomite in gluey flocculate, stirs evenly, and obtains diatomite mud, the additional amount of diatomite be greater than to
The 1% of the quality that disposes waste liquid, preferably 1%~15%, then to diatomite mud carry out filters pressing, by be separated by solid-liquid separation obtain filtrate and
Filter residue, filtrate are the aqueous solutions of NMP, and it is noble metal and carbon dust returned enterprise that filter residue, which is the solid containing noble metal, carbon dust etc.,
Raw material.
Embodiment 1: it is molten that the PAS polyaluminium sulfate that 200ML concentration is 0.5~5% is first added in 1000ML spent anolyte
Liquid adds 5-20g diatomite after mixing evenly, static after mixing evenly, will be obvious that lamination within static 1 hour, quiet
After setting 12 hours, the volume of bottom black colloidal fluid is 350ML, and supernatant liquor 850ML, moisture 17.8% is (in former spent anolyte
Moisture content 1%), remaining black colloidal liquid isolates wherein remaining NMP by filters pressing mode, and diatomite addition is got over
Multiple pressure filter effect is better, and filter cake is also more dry, using superfine diatomite better effect.
Embodiment 2: the PAC aluminium polychloride that 200ML concentration is 0.5~5% is first added in 1000ML spent anolyte and wads a quilt with cotton
Solidifying agent solution, adds 5-20g diatomite after mixing evenly, static after mixing evenly, will be obvious that within static 1 hour that layering is existing
As after standing 12 hours, the volume of bottom black colloidal fluid is 350ML, and supernatant liquor 850ML, (Yuanyang is extremely useless for moisture 17.8%
Liquid moisture 1%), bottom black colloidal fluid separates out wherein remaining NMP, the more multiple pressure filter effect of diatomite addition by filters pressing mode
Fruit is better, and filter cake is also more dry, using superfine diatomite better effect.
Embodiment 3: the PFS bodied ferric sulfate that 200ML concentration is 0.5~5% is first added in 1000ML spent anolyte and wads a quilt with cotton
Solidifying agent solution, adds 5-20g diatomite after mixing evenly, static after mixing evenly, will be obvious that within static 1 hour that layering is existing
As after standing 12 hours, the volume of bottom black colloidal fluid is 350ML, and supernatant liquor 850ML, (Yuanyang is extremely useless for moisture 17.8%
Liquid moisture 1%), bottom black colloidal fluid isolates wherein remaining NMP, the more multiple pressure filter of diatomite addition by filters pressing mode
Effect is better, and filter cake is also more dry, using superfine diatomite better effect.
Embodiment 4: 200ML concentration is added first in 1000ML spent anolyte as 0.5~5% 12 hydrazine aluminum sulfate potassium wadding
Solidifying agent solution, adds 5-20g diatomite after mixing evenly, static after mixing evenly, will be obvious that within static 1 hour that layering is existing
As after standing 12 hours, the volume of bottom black colloidal fluid is 350ML, and supernatant liquor 850ML, (Yuanyang is extremely useless for moisture 17.8%
Liquid moisture 1%), i.e., by sedimentation method, 70%NMP in former spent anolyte can be separated, remaining black liquor
Wherein remaining NMP is isolated by filters pressing mode or the way of distillation, the more multiple pressure filter effect of diatomite addition is better, filter cake
It is more dry, using superfine diatomite better effect.
Through testing, flocculation treatment first is carried out with flocculant, diatomite is then added again and carries out secondary treatment spent anolyte, adopt
Reach 10 kilograms with pressure, the above plate compression equipment of 200 mesh of filter cloth handles spent anolyte, daily handling ability reach 100 tons/
It, can separate in former spent anolyte 95% NMP, and gained filtrate is NMP aqueous solution, can be with recycling and reusing, gained
The solid content of solid filter residue can be used as the raw material of noble metal and carbon dust returned enterprise, or carry out harmless treatment 75% or more.
There are many embodiments of the present invention, and the technical thought of embodiment according to the present invention is enlightenment, said by above-mentioned
Bright content, relevant staff completely can without departing from the scope of the technological thought of the present invention', carry out multiplicity change with
And modification.The technical scope of the present invention is not limited to the contents of the specification, it is necessary to according to scope of the claims come
Determine its technical scope.
Claims (10)
1. a kind of method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid, it is characterized in that: including with flocculant to anode
Waste liquid carries out flocculation separation.
2. recycling the method for N methyl pyrrolidone in Anode of lithium cell waste liquid according to claim 1, characterized in that including
Following steps:
Step 1: spent anolyte is injected in processing pond；
It is staticly settled after mixing evenly Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond
12 hours or more, supernatant liquid was the aqueous solution of NMP, lower sediment thing be include that carbon dust, noble metal, the flocculation glue of NMP are heavy
Starch；
Step 3: carrying out filters pressing to gained flocculation gelatinous precipitate, filtrate is the aqueous solution of NMP, and filter residue is containing noble metal, carbon
The solid of powder etc.；
Filtrate obtained in supernatant liquid and third step in second step is all the aqueous solution of NMP.
3. recycling the method for N methyl pyrrolidone in Anode of lithium cell waste liquid according to claim 1, characterized in that including
Following steps:
Step 1: spent anolyte is injected in processing pond；
Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond adds silicon after mixing evenly
Diatomaceous earth is uniformly mixing to obtain diatomite mud；
Step 3 carries out filters pressing to diatomite mud, realizes and be separated by solid-liquid separation, obtain filtrate and filter residue, filtrate is the water-soluble of NMP
Liquid, filter residue are the solids containing noble metal, carbon dust etc..
4. recycling the method for N methyl pyrrolidone in Anode of lithium cell waste liquid according to claim 1, characterized in that including
Following steps:
Step 1: spent anolyte is injected in processing pond；
Step 2: the flocculant that mass ratio is 0.5-1% is added into anode liquid waste processing pond, after mixing evenly, static 12 is small
When more than, supernatant liquid be NMP aqueous solution, lower sediment thing be include carbon dust, noble metal, NMP flocculation gelatinous precipitate；
Step 3: diatomite is added into flocculation gelatinous precipitate again, it is uniformly mixing to obtain diatomite mud, then to diatomite mud
Slurry carries out filters pressing, realizes and is separated by solid-liquid separation, obtains filter residue and filtrate, filtrate is the aqueous solution of NMP, and filter residue is containing noble metal, carbon
The solid of powder.
5. according to the method for N methyl pyrrolidone in the recycling Anode of lithium cell waste liquid of claim 3,4, characterized in that silicon
The additional amount of diatomaceous earth is greater than the 1% of liquid quality to be processed.
6. recycling the method for N methyl pyrrolidone in Anode of lithium cell waste liquid according to claim 5, characterized in that diatom
The additional amount of soil should be greater than the 5%~15% of liquid quality to be processed.
7. -4 method for recycling N methyl pyrrolidone in Anode of lithium cell waste liquids according to claim 1, characterized in that In
In above-mentioned processing method, the flocculant is PAS polyaluminium sulfate, PAC aluminium polychloride, PFC poly-ferric chloride, PFS polymerization
Ferric sulfate or 12 hydrazine aluminum sulfate potassium or their mixture.
8. recycling the method for N methyl pyrrolidone in Anode of lithium cell waste liquid according to claim 7, characterized in that described
Flocculant is PAS polyaluminium sulfate, PAC aluminium polychloride, PFC poly-ferric chloride, PFS bodied ferric sulfate or 12 hydrated sulfuric acids
Aluminium potassium.
9. recycling the method for N methyl pyrrolidone in Anode of lithium cell waste liquid according to claim 7, characterized in that described
Flocculant is PAS polyaluminium sulfate.
10. the method for N methyl pyrrolidone in the recycling Anode of lithium cell waste liquid according to claim 2-4, characterized in that institute
Stating filters pressing is to be greater than 10 kilograms using pressure, plate compression equipment more than 200 mesh of filter cloth.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910759590.9A CN110436593A (en) | 2019-08-16 | 2019-08-16 | A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid |
| CN202010713670.3A CN111620424A (en) | 2019-08-16 | 2020-07-22 | Method for recovering N-methyl pyrrolidone in lithium battery anode waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910759590.9A CN110436593A (en) | 2019-08-16 | 2019-08-16 | A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid |
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| CN110436593A true CN110436593A (en) | 2019-11-12 |
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| CN201910759590.9A Pending CN110436593A (en) | 2019-08-16 | 2019-08-16 | A method of N methyl pyrrolidone in recycling Anode of lithium cell waste liquid |
| CN202010713670.3A Withdrawn CN111620424A (en) | 2019-08-16 | 2020-07-22 | Method for recovering N-methyl pyrrolidone in lithium battery anode waste liquid |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010713670.3A Withdrawn CN111620424A (en) | 2019-08-16 | 2020-07-22 | Method for recovering N-methyl pyrrolidone in lithium battery anode waste liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113690502A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Method for recycling waste battery slurry |
| CN114702170A (en) * | 2022-04-20 | 2022-07-05 | 惠州锂威新能源科技有限公司 | Cathode waste liquid recovery treatment method |
| CN115367906A (en) * | 2022-07-04 | 2022-11-22 | 浙江南都电源动力股份有限公司 | Method for recovering NMP cleaning waste liquid of lithium battery |
| CN115465988A (en) * | 2021-11-12 | 2022-12-13 | 金为环保科技(常州)有限公司 | Process for recovering NMP (N-methyl pyrrolidone) in waste lithium batteries and product thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112279797B (en) * | 2020-10-28 | 2022-07-22 | 重庆工商大学 | Method for recovering N-methyl pyrrolidone from polyurethane adhesive cleaning waste liquid |
| CN115466842A (en) * | 2021-11-12 | 2022-12-13 | 金为环保科技(常州)有限公司 | Treatment method and application of waste lithium battery waste liquid |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113690502A (en) * | 2021-07-23 | 2021-11-23 | 广东邦普循环科技有限公司 | Method for recycling waste battery slurry |
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| CN115465988A (en) * | 2021-11-12 | 2022-12-13 | 金为环保科技(常州)有限公司 | Process for recovering NMP (N-methyl pyrrolidone) in waste lithium batteries and product thereof |
| CN114702170A (en) * | 2022-04-20 | 2022-07-05 | 惠州锂威新能源科技有限公司 | Cathode waste liquid recovery treatment method |
| CN115367906A (en) * | 2022-07-04 | 2022-11-22 | 浙江南都电源动力股份有限公司 | Method for recovering NMP cleaning waste liquid of lithium battery |
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| Publication number | Publication date |
|---|---|
| CN111620424A (en) | 2020-09-04 |
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