CN108546243A - A kind of lithium battery production double tower NMP recycling purification systems and its recycling method of purification - Google Patents
A kind of lithium battery production double tower NMP recycling purification systems and its recycling method of purification Download PDFInfo
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- CN108546243A CN108546243A CN201810781476.1A CN201810781476A CN108546243A CN 108546243 A CN108546243 A CN 108546243A CN 201810781476 A CN201810781476 A CN 201810781476A CN 108546243 A CN108546243 A CN 108546243A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 36
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004064 recycling Methods 0.000 title claims abstract description 25
- 238000000605 extraction Methods 0.000 claims abstract description 53
- 238000010521 absorption reaction Methods 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010992 reflux Methods 0.000 claims description 51
- 239000007789 gas Substances 0.000 claims description 31
- 239000000470 constituent Substances 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 20
- 239000012530 fluid Substances 0.000 claims description 18
- 239000002912 waste gas Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 230000002745 absorbent Effects 0.000 claims description 3
- 239000002250 absorbent Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000002918 waste heat Substances 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 79
- 230000009102 absorption Effects 0.000 description 37
- 239000000463 material Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Gas Separation By Absorption (AREA)
Abstract
A kind of lithium battery production double tower NMP recycling purification systems of present invention offer and its recycling method of purification, recycling method of purification include that water absorption NMP exhaust gas obtains NMP waste liquids;NMP waste liquids input next door rectifying column and carry out a rectifying;Secondary rectifying will be carried out in the middle part of the rectifying column of next door and in tower reactor extraction NMP and heavy seeds input rectifying column, overhead extraction light component NMP concentration is not less than 99.9%.The beneficial effects of the invention are as follows:Using the novel double columns rectification process of next door rectifying column+rectifying column; the NMP exhaust gas generated in Production Process of Lithium Battery can be absorbed, rectification and purification; final recycling obtains electron level NMP products; it can re-use in the production of lithium batteries; significantly improve NMP utilization rates; be conducive to environmental protection, there is high Social benefit and economic benefit, is conducive to promote and apply.
Description
Technical field
The invention belongs to rectifying separation technology fields, more particularly, to a kind of lithium battery production double tower NMP recycling purifications system
System and its recycling method of purification.
Background technology
Demand for automobile and high-power, high-energy density the lithium rechargeable battery of compact power supply is in
The growth of explosion type.On lithium battery manufacturing line, a large amount of uses and expensive N-Methyl pyrrolidone solvent
(NMP), a big chunk of battery manufacture cost is occupied.NMP is a kind of colourless transparent oil liquid, and volatility is low, and heat is steady
It is qualitative, chemical stability is good, can volatilize with vapor.In coating process, NMP can become gas phase as dry gas is arranged together
Go out, if with with abandoning, it is not only uneconomical but also not environmentally, it is necessary to be recycled.In face of its fancy price and environmental problem, recycling
It is main flow direction using the waste liquid containing NMP generated in production process, but the composition of recovered liquid is relative complex, directly recycling obtains
NMP includes other type impurity, can not directly be utilized.Therefore, a kind of NMP products that can obtain extreme high purity are found, and efficiently
Energy-efficient NMP purification systems and its method become the task of top priority.
Invention content
The problem to be solved in the present invention is to provide a kind of purifying the NMP waste gas recoveries generated in Production Process of Lithium Battery
High purity N MP products, the lithium battery production double tower NMP recycling purification systems for meeting environmentally protective theory and its recycling purification side
Method.
In order to solve the above technical problems, the technical solution adopted by the present invention is:A kind of production double tower NMP recycling of lithium battery carries
Pure lines are united, including absorption plant, fluid reservoir, next door rectifier unit and the rectifier unit being sequentially communicated, the absorption plant include
Absorption tower and absorption reflux pump, the absorption tower top are equipped with lean solution inlet, and the absorption tower lower part is equipped with waste gas inlet,
Be equipped with gas discharge outlet at the top of the absorption tower, the absorption tower rich solution liquid outlet all the way by the absorption reflux pump with it is described
Absorption tower reflux inlet connection, another way connect the fluid reservoir inlet;The liquid outlet of the fluid reservoir and next door essence
Distillation unit feed inlet connects, and the tower reactor extraction mouth of the next door rectifier unit is connect with the feed inlet of the rectifier unit, described
Next door rectifier unit overhead extraction mouth is connect with the lean solution inlet of the absorption plant, extraction in the middle part of the next door rectifier unit
Mouth is connected to the fluid reservoir inlet.
In technical solution, it is preferred that the next door rectifier unit includes next door rectifying column, the first overhead reflux pipeline and
One tower reactor boils pipeline again, and the first overhead reflux pipeline passes sequentially through the first condenser, the first return tank, the first reflux pump will
The next door rectifying column tower top extraction mouth and the connection of tower upper return entrance, first condensator outlet are also filled with the absorption
The absorbent entrance connection set;First tower reactor boil again pipeline pass sequentially through the first tower reactor pump, the first reboiler will it is described every
Wall tower bottom of rectifying tower extraction mouth be connected to tower lower return entrance, in the middle part of the next door rectifying column extraction mouth and the fluid reservoir into
Liquid mouth is connected to.
In technical solution, it is preferred that the rectifier unit include rectifying column, the second overhead reflux pipeline and the second tower reactor again
Pipeline is boiled, the first tower reactor pump discharge is connect with the rectifying column feed inlet, and the second overhead reflux pipeline passes sequentially through
Second condenser, the second return tank, the rectifying column tower top is produced mouth to the second reflux pump and tower upper return entrance is connected to, institute
State the second reflux pump discharge connection light component pipeline;Second tower reactor boils pipeline and passes sequentially through the second tower reactor pump, second again again
Next door tower bottom of rectifying tower extraction mouth is connected to by boiling device with tower lower return entrance, the second tower reactor pump discharge connection recombination
It is in charge of line.
In technical solution, it is preferred that the is arranged between next door rectifying column tower top extraction mouth and first drainer
One heat exchanger, the absorption plant discharge port are connect with the next door rectifier unit feed inlet by the First Heat Exchanger;Institute
It states and the second heat exchanger, the first tower reactor pump discharge, next door is set between rectifying column tower top extraction mouth and second drainer
Extraction mouth is connect with the rectifying column feed inlet by second heat exchanger respectively in the middle part of rectifying column.
In technical solution, it is preferred that the public stripping section of the next door rectifying column and rectifying section.
A kind of lithium battery production double tower NMP recycling methods of purification, include the following steps:
(1) the NMP exhaust gas utilization water in Production Process of Lithium Battery is absorbed, obtain purified gas and contains NMP
And the NMP recovered liquids of heavy constituent impurity;
(2) NMP recovered liquids input next door rectifying column is subjected to a rectifying, next door rectifying column tower top is made to produce in light component
NMP concentration is not more than 400mg/L, extraction component input next door rectifying column feed inlet in the middle part of the rectifying column of next door is carried out again smart
It evaporates;
(3) the heavy constituent impurity of step (2) median septum tower bottom of rectifying tower extraction and NMP input rectifying columns are subjected to secondary fine
It evaporates, rectifying column produces NMP concentration in light component and is not less than 99.9%.
In technical solution, it is preferred that in step (2) (3), by the waste heat of next door rectifying column, rectifying column tower top light component point
Not Yong Yu next door rectifying column and rectifying column feeding preheating.
In technical solution, it is preferred that the light component of step (2) median septum rectifying column tower top extraction is used for step through liquefaction
(1) absorption of NMP exhaust gas in.
In technical solution, it is preferred that the number of theoretical plate of the next door rectifying column is 45-60 blocks, operating pressure 10-
100kpa, tower top temperature are 60-100 DEG C, and bottom temperature is 135-175 DEG C, mass reflux ratio 0.1-1.
In technical solution, it is preferred that in step (3), the number of theoretical plate of the rectifying column is 35-50 blocks, and operating pressure is
10-50kpa, tower top temperature are 140-170 DEG C, and bottom temperature is 145-175 DEG C, mass reflux ratio 0.5-3.
The invention has the advantages and positive effects that:
It 1, can be to being generated in Production Process of Lithium Battery using the novel double columns rectification process of next door rectifying column+rectifying column
NMP exhaust gas absorbed, rectification and purification, and final recycling obtains electron level NMP products, can re-use in the production of lithium batteries,
NMP utilization rates are significantly improved, environmental protection is conducive to, there is high Social benefit and economic benefit, are conducive to promote and apply;
2, the moisture isolated is re-applied in NMP waste gas absorptions, internal system forms closed circulation, removes NMP products
Outer only gas and part heavy constituent residue of the discharge containing a small amount of NMP, reduces danger discharge, and recycling profit is carried out to danger
With meeting the theory of green chemical industry;
3, the thermal energy that partial liquefaction release is stored by the way that heat exchanger is arranged is used to preheat raw material, and that improves thermal energy has
Effect utilizes, and reduces energy consumption;
4, novel double columns rectification process reduces a set of tower, reduces floor space compared with traditional three tower process, saves
About equipment investment.
Description of the drawings
Fig. 1 is the structural schematic diagram of the embodiment of the present invention.
In figure:
1, absorption plant 2, fluid reservoir 3, next door rectifier unit
4, rectifier unit 5, absorption tower 6, absorption reflux pump
7, next door rectifying column 8, heat exchanger 9, condenser
10, return tank 11, reflux pump 12, tower reactor pump
13, reboiler 14, rectifying column 15, heat exchanger
16, condenser 17, return tank 18, reflux pump
19, tower reactor pump 20, reboiler
Specific implementation mode
As shown in Figure 1, the present embodiment provides a kind of lithium battery production double tower NMP to recycle purification system, including it is sequentially communicated
Absorption plant 1, fluid reservoir 2, next door rectifier unit 3 and rectifier unit 4, the rich solution liquid outlet of absorption plant 1 and fluid reservoir 2
Inlet connects, and the liquid outlet of fluid reservoir 2 is connect with 3 feed inlet of next door rectifier unit, and the tower reactor of next door rectifier unit 3 produces mouth
It being connect with the feed inlet of rectifier unit 4, rectifier unit 3 overhead extraction mouth in next door is connect with the lean solution inlet of absorption plant 1, every
3 middle part extraction mouth of wall rectifier unit is connected to 2 inlet of fluid reservoir.
Absorption plant 1 includes absorption tower 5 and absorbs reflux pump 6, and 5 top of absorption tower is equipped with lean solution inlet, under absorption tower 5
Portion is equipped with waste gas inlet, and 5 top of absorption tower is equipped with gas discharge outlet, and 5 rich solution liquid outlet of absorption tower is flowed back by absorbing all the way
Pump 6 is connect with 5 reflux inlet of absorption tower, and another way connects 2 inlet of fluid reservoir.
Next door rectifier unit 3 boils pipeline again including next door rectifying column 7, the first overhead reflux pipeline and the first tower reactor, and first
Overhead reflux pipeline passes sequentially through condenser 9, return tank 10, reflux pump 11 by 7 overhead extraction mouth of next door rectifying column and tower top
Reflux inlet is connected to, and the outlet of condenser 9 is also connect with the absorbent entrance of absorption plant 1;First tower reactor is boiled pipeline and is led to successively again
Cross tower reactor pump 12,7 tower reactor of next door rectifying column extraction mouth is connected to by reboiler 13 with tower lower return entrance.7 tower of next door rectifying column
Heat exchanger 8 is set between top extraction mouth and the first drainer, 1 discharge port of absorption plant passes through with 3 feed inlet of next door rectifier unit
Heat exchanger 8 connects, and rectifying column 7 middle part extraction mouth in next door is connected to 2 inlet of fluid reservoir.
7 public stripping section of next door rectifying column and rectifying section.
Next door rectifying column 7 (Dividing Wall Column, abbreviation DWC) is that a vertical wall is arranged in rectifying column,
Vertical wall can be extended to tower top or bottom of tower, DWC towers can have common rectifying section or stripping by the separated two parts of partition wall
Section, or have common rectifying section and stripping section simultaneously.DWC towers are thermodynamically comparatively ideal system structures, mixed detaching 3 components
When closing object, with identical number of theoretical plate, same separation task is completed, it need to be less than traditional two-tower process using DWC towers
Boiling hot amount and condensation number again.For certain given materials, divided-wall distillation column 7 is compared with conventional rectification tower needs smaller reflux
Than, therefore operation capacity increases, and it is energy saving to can reach 60% or more, equipment investment 30% may be saved.DWC towers can be answered widely
It is detached for petroleum refining, petrochemical industry, chemicals and gas.
Rectifier unit includes that rectifying column 14, the second overhead reflux pipeline and the second tower reactor boil pipeline, 12 outlet of tower reactor pump again
It is connect with 14 feed inlet of rectifying column, the second overhead reflux pipeline passes sequentially through condenser 16, return tank 17, reflux pump 18 by rectifying
14 overhead extraction mouth of tower and the connection of tower upper return entrance, the outlet of reflux pump 18 connection light component pipeline;Second tower reactor boils pipe again
Road passes sequentially through tower reactor pump 19,7 tower reactor of next door rectifying column extraction mouth is connected to by reboiler 20 with tower lower return entrance, tower reactor pump
19 outlet connection heavy constituent pipelines.Heat exchanger 15, tower reactor pump 12 are set between 14 overhead extraction mouth of rectifying column and the second drainer
Outlet, 7 middle part extraction mouth of next door rectifying column are connect with 14 feed inlet of rectifying column by heat exchanger 15 respectively.
A kind of lithium battery production double tower NMP recycling methods of purification, include the following steps:
(1) exhaust gas containing NMP generated in Production Process of Lithium Battery is passed through in absorption plant 1, is made by water spray
Gas containing NMP comes into full contact with water, and the NMP in the gas is made to be fully absorbed by water, obtains purified gas and contains NMP
And the NMP recovered liquids of heavy constituent impurity;
(2) NMP recovered liquids are buffered through fluid reservoir 2, are preheated by heat exchanger 8, input next door rectifying column 7 middle part into
Material mouth carries out a rectifying, and the number of theoretical plate of next door rectifying column is 45-60 blocks, operating pressure 10-100kpa, and tower top temperature is
60-100 DEG C, bottom temperature is 135-175 DEG C, mass reflux ratio 0.1-1.
NMP concentration is not more than 400mg/L in 7 overhead extraction light component vapor of next door rectifying column, by heat exchanger 8 to water
The waste heat of steam is stored, and condensed device 9 condenses rear portion and returns to be continued as lean solution to NMP exhaust gas in absorption plant 1
It is sprayed, another part enters return tank 10, and is back to 7 top of next door rectifying column through the supercharging of reflux pump 18;
NMP and heavy constituent impurity are assembled to tower reactor, and after 12 supercharging of tower reactor pump, a part returns after the heating of reboiler 13
7 lower part of next door rectifying column, another part are sent into 14 middle part feed inlet of rectifying column after the preheating of heat exchanger 15;
7 middle part extraction mouth extraction NMP of next door rectifying column and minute quantity moisture re-enter the 7 middle part charging of next door rectifying column
Mouth carries out rectifying again;
(3) NMP of 7 tower reactor of step (2) median septum rectifying column extraction and heavy constituent impurity are carried out by heat exchanger 15 pre-
Heat, 14 middle part feed inlet of input rectifying column carry out secondary rectifying, and the number of theoretical plate of rectifying column is 35-50 blocks, operating pressure 10-
50kpa, tower top temperature are 140-170 DEG C, and bottom temperature is 145-175 DEG C, mass reflux ratio 0.5-3.
NMP concentration is not less than 99.9% in 14 overhead extraction light component of rectifying column, is handed over partial heat by heat exchanger 15
It changing, condensed device 16 enters return tank 17 after condensing, it is pressurized through reflux pump 18, a part is back to 14 top of rectifying column, another
Part flow to light component pipeline and is collected to NMP products;
Heavy constituent impurity is assembled to tower reactor, and after 19 supercharging of tower reactor pump, a part returns to rectifying after the heating of reboiler 20
14 tower lower part of tower, another part flow to heavy constituent pipeline and counterweight composition impurity is collected.
The present invention uses the novel double columns rectification process of next door rectifying column 7+ rectifying columns 14, can be in Production Process of Lithium Battery
The NMP exhaust gas of generation absorbed, rectification and purification, and final recycling obtains electron level NMP products, can in the production of lithium batteries again
It utilizes, significantly improves NMP utilization rates, be conducive to environmental protection, there is high Social benefit and economic benefit, answered conducive to popularization
With;The moisture isolated is re-applied in NMP waste gas absorptions, internal system forms closed circulation, is only discharged in addition to NMP products
Gas containing a small amount of NMP and part heavy constituent residue, reduce danger discharge, carry out recycling to danger, meet
The theory of green chemical industry;The thermal energy that partial liquefaction release is stored by the way that heat exchanger is arranged is used to preheat raw material, improves heat
Energy efficiently uses, and reduces energy consumption;Novel double columns rectification process compared with traditional three tower process, reduce a reboiler and
One tower, reduces floor space, has saved equipment investment.
Lithium battery of the present invention production double tower NMP recycling method of purification is described further below by way of several embodiments,
But the not any restrictions caused by the condition and application effect of each embodiment are to the present invention.
Embodiment 1
A kind of lithium battery production double tower NMP recycling methods of purification, include the following steps:
(1) exhaust gas containing NMP generated in Production Process of Lithium Battery is passed through in absorption plant 1, is made by water spray
Gas containing NMP comes into full contact with water, and the NMP in the gas is made to be fully absorbed by water, obtains purified gas and contains NMP
And the NMP recovered liquids of heavy constituent impurity;
(2) NMP recovered liquids are buffered through fluid reservoir 2, are preheated by heat exchanger 8, input next door rectifying column 7 middle part into
Material mouth carries out a rectifying, and the number of theoretical plate of next door rectifying column 7 is 55 pieces, operating pressure 20kpa, and tower top temperature is 65 DEG C,
Bottom temperature is 142 DEG C, mass reflux ratio 0.7;
It is mainly water in 7 overhead extraction light component of next door rectifying column, NMP concentration is not more than 400mg/L, passes through heat exchanger 8
The partial heat energy of vapor liquefaction release is stored, condensed device 9 condenses rear portion and returns in absorption plant 1 as poor
Liquid continues to spray NMP exhaust gas, and another part enters return tank 10, and is back to next door rectifying column through the supercharging of reflux pump 18
7 tops;
NMP and heavy constituent impurity are assembled to tower reactor, and it includes mainly NMP99.1%, heavy seeds that tower reactor, which produces in heavy constituent,
0.9%, free ammonium 0.5mg/L, metal ion 31mg/L, the content 70mg/L of water, after 12 supercharging of tower reactor pump, a part is through again
It boils and returns to rectifying column 7 lower part in next door after device 13 heats, another part is sent into 14 middle part charging of rectifying column after the preheating of heat exchanger 15
Mouthful;
The middle part of next door rectifying column 7 extraction mouth extraction NMP65% and moisture 35%, re-enter 7 middle part of next door rectifying column into
Material mouth carries out rectifying again;
(3) NMP of 7 tower reactor of step (2) median septum rectifying column extraction and heavy constituent impurity are carried out by heat exchanger 15 pre-
Heat, 14 middle part feed inlet of input rectifying column carry out secondary rectifying, and the number of theoretical plate of rectifying column 14 is 41, operating pressure 30kpa,
Tower top temperature is 151 DEG C, and bottom temperature is 158 DEG C, mass reflux ratio 2.5;
NMP a concentration of 99.95% in 14 overhead extraction light component of rectifying column, is exchanged partial heat by heat exchanger 15,
Condensed device 16 enters return tank 17 after condensing, and is pressurized through reflux pump 18, and a part is back to 14 top of rectifying column, another part
It flow to light component pipeline to be collected NMP products, NMP products can be directly used for lithium battery production;
Heavy constituent impurity is assembled to tower reactor, and after 19 supercharging of tower reactor pump, a part returns to rectifying after the heating of reboiler 20
14 tower lower part of tower, another part flow to heavy constituent pipeline and counterweight composition impurity is collected, and contains in tower reactor extraction
NMP65%, heavy seeds 35%, metal ion 510mg/L.
Embodiment 2
A kind of lithium battery production double tower NMP recycling methods of purification, include the following steps:
(1) exhaust gas containing NMP generated in Production Process of Lithium Battery is passed through in absorption plant 1, is made by water spray
Gas containing NMP comes into full contact with water, and the NMP in the gas is made to be fully absorbed by water, obtains purified gas and contains NMP
And the NMP recovered liquids of heavy constituent impurity;
(2) NMP recovered liquids are buffered through fluid reservoir 2, are preheated by heat exchanger 8, input next door rectifying column 7 middle part into
Material mouth carries out a rectifying, and the number of theoretical plate of next door rectifying column 7 is 59, and operating pressure 70kpa, tower top temperature is 84 DEG C, tower
Kettle temperature degree is 167 DEG C, mass reflux ratio 1;
It is mainly water in 7 overhead extraction light component of next door rectifying column, NMP concentration is not more than 400mg/L, passes through heat exchanger 8
The partial heat energy of vapor liquefaction release is stored, condensed device 9 condenses rear portion and returns in absorption plant 1 as poor
Liquid continues to spray NMP exhaust gas, and another part enters return tank 10, and is back to next door rectifying column through the supercharging of reflux pump 18
7 tops;
NMP and heavy constituent impurity are assembled to tower reactor, and it includes mainly NMP98.8%, heavy seeds that tower reactor, which produces in heavy constituent,
1.1%, free ammonium 0.8mg/L, metal ion 41mg/L, the content 58mg/L of water, after 12 supercharging of tower reactor pump, a part is through again
It boils and returns to rectifying column 7 lower part in next door after device 13 heats, another part is sent into 14 middle part charging of rectifying column after the preheating of heat exchanger 15
Mouthful;
The middle part of next door rectifying column 7 extraction mouth extraction NMP 80% and moisture 20%, re-enter 7 middle part of next door rectifying column into
Material mouth carries out rectifying again;
(3) NMP of 7 tower reactor of step (2) median septum rectifying column extraction and heavy constituent impurity are carried out by heat exchanger 15 pre-
Heat, 14 middle part feed inlet of input rectifying column carry out secondary rectifying, and the number of theoretical plate of rectifying column 14 is 47, operating pressure 10kpa,
Tower top temperature is 136 DEG C, and bottom temperature is 141 DEG C, mass reflux ratio 1.8;
NMP a concentration of 99.97% in 14 overhead extraction light component of rectifying column, is exchanged partial heat by heat exchanger 15,
Condensed device 16 enters return tank 17 after condensing, and is pressurized through reflux pump 18, and a part is back to 14 top of rectifying column, another part
It flow to light component pipeline to be collected NMP products, NMP products can be directly used for lithium battery production;
Heavy constituent impurity is assembled to tower reactor, and after 19 supercharging of tower reactor pump, a part returns to rectifying after the heating of reboiler 20
14 tower lower part of tower, another part flow to heavy constituent pipeline and counterweight composition impurity is collected, and contains in tower reactor extraction
NMP84%, heavy seeds 16%, metal ion 790mg/L.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention,
It should not be construed as limiting the practical range of the present invention.Any changes and modifications in accordance with the scope of the present application,
It should all still fall within the scope of the patent of the present invention.
Claims (10)
1. a kind of lithium battery production double tower NMP recycles purification system, it is characterised in that:Including be sequentially communicated absorption plant, storage
Flow container, next door rectifier unit and rectifier unit, the absorption plant include absorption tower and absorption reflux pump, the absorption tower top
Equipped with lean solution inlet, the absorption tower lower part is equipped with waste gas inlet, and gas discharge outlet is equipped at the top of the absorption tower, described
Absorption tower rich solution liquid outlet is connect by the absorption reflux pump with the absorption tower reflux inlet all the way, described in another way connection
Fluid reservoir inlet;The liquid outlet of the fluid reservoir is connect with the next door rectifier unit feed inlet, the next door rectifier unit
Tower reactor extraction mouth connect with the feed inlet of the rectifier unit, the middle part of the next door rectifier unit produces mouth and the storage
Flow container inlet is connected to, and the next door rectifier unit overhead extraction mouth is connect with the lean solution inlet of the absorption plant.
2. lithium battery production double tower NMP according to claim 1 recycles purification system, it is characterised in that:The next door essence
Distillation unit includes that next door rectifying column, the first overhead reflux pipeline and the first tower reactor boil pipeline, the first overhead reflux pipeline again
It passes sequentially through the first condenser, the first return tank, the first reflux pump and the next door rectifying column tower top is produced into mouth and tower top time
Inflow entrance is connected to, and first condensator outlet is also connect with the absorbent entrance of the absorption plant;First tower reactor is again
Boiling pipeline passes sequentially through the first tower reactor pump, the next door tower bottom of rectifying tower is produced mouth and tower lower return entrance by the first reboiler
The middle part extraction mouth of connection, the next door rectifying column is connected to the fluid reservoir inlet.
3. lithium battery production double tower NMP according to claim 2 recycles purification system, it is characterised in that:The rectifying dress
It sets and boils pipeline, the first tower reactor pump discharge and the rectifying again including rectifying column, the second overhead reflux pipeline and the second tower reactor
Tower feed inlet connects, and the second overhead reflux pipeline passes sequentially through the second condenser, the second return tank, the second reflux pump by institute
Rectifying column tower top extraction mouth and the connection of tower upper return entrance are stated, the second reflux pump discharge connects light component pipeline;It is described
Second tower reactor boil again pipeline pass sequentially through the second tower reactor pump, the second reboiler will the next door tower bottom of rectifying tower extraction mouth and tower under
Portion's reflux inlet connection, the second tower reactor pump discharge connect heavy constituent pipeline.
4. lithium battery production double tower NMP according to claim 3 recycles purification system, it is characterised in that:The next door essence
It evaporates and First Heat Exchanger, the absorption plant discharge port and the next door is set between column overhead extraction mouth and first drainer
Rectifier unit feed inlet is connected by the First Heat Exchanger;Between the rectifying column tower top extraction mouth and second drainer
Second heat exchanger is set, in the middle part of the first tower reactor pump discharge, next door rectifying column extraction mouth respectively with the rectifying column feed inlet
It is connected by second heat exchanger.
5. recycling purification system according to any lithium battery production double tower NMP of claim 2-4, it is characterised in that:It is described
The public stripping section of next door rectifying column and rectifying section.
6. a kind of lithium battery production double tower NMP recycles method of purification, which is characterized in that include the following steps:
(1) the NMP exhaust gas utilization water in Production Process of Lithium Battery is absorbed, obtains purified gas and containing NMP and again
The NMP recovered liquids of composition impurity;
(2) NMP recovered liquids input next door rectifying column is subjected to a rectifying, next door rectifying column tower top is made to produce NMP in light component
Concentration is not more than 400mg/L, and extraction component input next door rectifying column inlet in the middle part of the rectifying column of next door is carried out rectifying again;
(3) the heavy constituent impurity of step (2) median septum tower bottom of rectifying tower extraction and NMP input rectifying columns are subjected to secondary rectifying,
Rectifying column produces NMP concentration in light component and is not less than 99.9%.
7. lithium battery production double tower NMP according to claim 6 recycles method of purification, it is characterised in that:Step (2) (3)
In, the waste heat of next door rectifying column, rectifying column tower top light component is respectively used to the feeding preheating of next door rectifying column and rectifying column.
8. the lithium battery production double tower NMP described according to claim 6 or 7 recycles method of purification, it is characterised in that:Step (2)
Absorption of the light component through liquefying for NMP exhaust gas in step (1) of median septum rectifying column tower top extraction.
9. NMP according to claim 6 recycles method of purification, it is characterised in that:In step (2), the next door rectifying column
Number of theoretical plate be 45-60 blocks, operating pressure 10-100kpa, tower top temperature be 60-100 DEG C, bottom temperature 135-175
DEG C, mass reflux ratio 0.1-1.
10. NMP according to claim 6 recycles method of purification, it is characterised in that:In step (3), the reason of the rectifying column
It is 35-50 blocks by plate number, operating pressure 10-50kpa, tower top temperature is 140-170 DEG C, and bottom temperature is 145-175 DEG C, matter
Amount reflux ratio is 0.5-3.
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