CN109336803A - A kind of method and its system of NMP devil liquor recovery production super-clean high-purity solvent - Google Patents
A kind of method and its system of NMP devil liquor recovery production super-clean high-purity solvent Download PDFInfo
- Publication number
- CN109336803A CN109336803A CN201811296250.9A CN201811296250A CN109336803A CN 109336803 A CN109336803 A CN 109336803A CN 201811296250 A CN201811296250 A CN 201811296250A CN 109336803 A CN109336803 A CN 109336803A
- Authority
- CN
- China
- Prior art keywords
- nmp
- raw material
- treatment
- liquor recovery
- devil liquor
- 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.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000011084 recovery Methods 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002904 solvent Substances 0.000 title claims abstract description 15
- 239000002699 waste material Substances 0.000 claims abstract description 41
- 239000002994 raw material Substances 0.000 claims abstract description 40
- 230000018044 dehydration Effects 0.000 claims abstract description 20
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 20
- 238000004064 recycling Methods 0.000 claims abstract description 20
- 238000007670 refining Methods 0.000 claims abstract description 11
- 238000000746 purification Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 56
- 239000007789 gas Substances 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 29
- 239000007792 gaseous phase Substances 0.000 claims description 20
- 239000002918 waste heat Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 10
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000009835 boiling Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 3
- 238000005215 recombination Methods 0.000 claims description 3
- 230000006798 recombination Effects 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 230000002262 irrigation Effects 0.000 abstract 1
- 238000003973 irrigation Methods 0.000 abstract 1
- 230000000116 mitigating effect Effects 0.000 abstract 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 74
- 239000007791 liquid phase Substances 0.000 description 19
- 238000010992 reflux Methods 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 8
- 230000008901 benefit Effects 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003880 polar aprotic solvent Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004065 wastewater treatment Methods 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses the methods and its system of a kind of NMP devil liquor recovery production super-clean high-purity solvent, belong to dangerous waste recycling industry, it is refined as lithium ion battery industry NMP recycling field, it is small to be intended to provide a kind of investment, low energy consumption, while mitigating environmental pollution, recycle the method and its system of high-purity N MP product, its drip irrigation device is as follows, step 1. raw material preheating, step 2. deoxidation treatment, step 3. dehydration, step 4. rectification process, step 5. refinement treatment, into luwa evaporator, further depth recycles NMP after purification bottom product is collected, unrenewable heavy constituent sends processing outside.A kind of system of NMP devil liquor recovery production superelevation pure solvent characterized by comprising raw material preheating device, device for deoxidizing, dehydration device, rectifier unit, refining plant, exhaust gas processing device.
Description
Technical field
The present invention relates to dangerous waste treatment industry and lithium ion battery industry NMP devil liquor recovery fields, in particular to a kind of
NMP devil liquor recovery produces the method and its system of high pure solvent.
Background technique
NMP also known as N-Methyl pyrrolidone (English name: N-methyl-2-pyrrolidone, NMP) are colorless transparent oil
Shape liquid, micro- smell for having amine.It can dissolve each other with water, alcohol, ether, ester, ketone, halogenated hydrocarbons, aromatic hydrocarbons and castor oil, be that chemical field is common
Organic solvent.Its volatility is low, and thermal stability, chemical stability are good, can volatilize with vapor and have hygroscopicity and right
Photaesthesia.
NMP is a kind of strong selectivity and the good polar solvent of stability and important industrial chemicals, and a kind of polar
Aprotic solvent, have viscosity it is low, volatility is low, and stability is good, toxicity is low, boiling point is high, dissolving power is strong, it is nonflammable, can
Biodegrade, recoverable, using it is safe and be suitable for multiple formulations purposes the advantages that, be widely used in lithium battery, height
The shelves industries such as coating and electronic isolation.
Auxiliary material NMP important as lithium battery anode, be widely used, especially lithium battery industry in recent years
It rapidly develops, NMP demand is increasing, finally also generates adverse effect to environment, since it is expensive, greatly increases
The production cost of lithium battery industry is added.Therefore industrial cost can be effectively reduced to the recycling of NMP waste liquid, and mitigates subsequent
Exhaust gas and treatment pressure of sewage.Ultra-clean and high pure chemical reagent is one kind of chemical reagent, refer to bulk composition purity be greater than 99.99%, it is miscellaneous
Matter ion especially impurity cationic and particle number meet the chemical reagent of strict demand.
Chinese patent 201810190451.4 proposes the industry stream of the i.e. multistage concentration of two tower process of one kind, rectifying, purification
Journey recycles the NMP in NMP waste liquid.But to obtain high-purity N MP product, the dehydration rate requirement in the technique is high,
And NMP boiling point is higher, therefore the technique requires very big reflux ratio, energy consumption needed for causing the technique is very high, and an once tower
Fluctuation, two tower NMP product purities cannot be guaranteed, and reduce waste water, tail gas that the stability of the technique, especially device generate
With kettle is residual to efficiently use, secondary pollution is generated to environment, energy consumption is very high under especially big reflux ratio.
Summary of the invention
The object of the present invention is to provide it is a kind of investment it is small, low energy consumption, mitigate environmental pollution while, in high yield, it is pollution-free,
Depth recycles the method and its system of ultra-pure NMP product, has high economic benefit and industrial value.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of method of NMP devil liquor recovery production super-clean high-purity solvent comprises the technical steps that:
Step 1. raw material preheating carries out waste heat recycling to NMP waste liquid and preheats；
NMP waste liquid after preheating in step 1 is carried out deoxidation and de- fixed gas is handled by step 2. deoxidation treatment；
NMP waste liquid after deoxidation in step 2 is carried out dehydrating, obtains gaseous component and tower reactor group by step 3. dehydration
Point；
NMP waste liquid dewatered in step 3 is carried out rectification process by step 4. rectification process, obtains light component and tower reactor recombination
Point；
Step 5. refinement treatment, by after rectifying in step 4 NMP waste liquid carry out refinement treatment, obtain first order gaseous phase materials and
First order raffinate, the first order gaseous phase materials obtain after heating in such a way that waste heat recycles to raw material in raw material preheating device
To NMP；
Step 6. vent gas treatment carries out carrying out washing treatment to tail gas using spray liquid by way of water circulated sprinkling；
In the step 5, is boiled again after the first order raffinate is collected, obtain second level gaseous phase materials and second
Grade raffinate, the second level gaseous phase materials are passed back into refining plant with first order gaseous phase materials jointly in raw material preheating device
In waste heat recycle by way of to raw material heating after obtain NMP, will the second level raffinate collect after be discharged, send processing outside.
Further, purification tower overhead gas phase materials carry out waste heat recycling with the NMP waste liquid in raw material preheating device, make
The NMP waste liquid temperature increases.
Further, the operating pressure of step 2 is -0.1 ~ -0.05MPa, and operation temperature is 45-100 DEG C.
Further, the operating pressure of step 3 is -0.1 ~ -0.05MPa, and operation temperature is 45-140 DEG C, and reflux ratio is
0.5-10, preferably 1-5.
Further, enter exhaust gas processing device after the gaseous component condensation in step 3.
Further, the operating pressure of step 4 is -0.1 ~ -0.05MPa, and operating temperature is 50-150 DEG C, and reflux ratio is
0.5-10, preferably 1-5.
Further, device for deoxidizing circular treatment is back to after the light component condensation in step 4.
Further, the operating pressure of step 5 subtractive process is -0.1 ~ -0.05MPa, and operation temperature is 50-150 DEG C, is returned
Flowing ratio is 0.5-10, preferably 1-5.
Further, in step 6, the tail gas after washing enters gas emission device, the absorbing liquid during vent gas treatment
Circular treatment is sent into device for deoxidizing.
Further, the spray liquid in step 6 is the waste water generated in dehydration device, and operation temperature is 30-70 DEG C, liquid gas
Mass ratio is 1-300, preferably 1-100.
A kind of system of NMP devil liquor recovery production superelevation pure solvent includes: raw material preheating device, pre- for carrying out to raw material
Heat；Device for deoxidizing, for carrying out deoxidation treatment to the raw material after preheating；Dehydration device, for being taken off to the raw material after deoxidation
Water process；Rectifier unit, for carrying out dehydration rectification process to dewatered raw material；Refining plant, after to rectification process
Material carry out refinement treatment；Exhaust gas processing device, for handling tail gas；The raw material preheating device, which is additionally provided with, to be changed
Hot device carries out waste heat recycling with NMP waste liquid for the gaseous phase materials after refinement treatment, increases NMP waste liquid temperature.
Further, refining plant includes luwa evaporator, for refining plant, treated that raffinate boils again,
And send the gaseous phase materials obtained after boiling back to raw material preheating device and the progress waste heat recycling of NMP waste liquid after condensing, it will boil
The raffinate discharge obtained afterwards, carries out sending processing outside.
In conclusion the invention has the following advantages:
1. using, device for deoxidizing carries out deoxidation to raw material and de- fixed gas is handled, and the rectifying for avoiding higher temperature makes raw material exist
The N of oxygen and fixed gas, that is, a small amount of2In the presence of occur charing, coking, to improve the coloration of NMP product, it is ensured that superelevation
The quality of pure NMP product；
2. the gaseous phase materials obtained after refinement treatment are sent back in raw material preheating device, the gas obtained after refinement treatment is utilized
Phase object exchanges heat with raw material NMP waste liquid, gives full play to its energy-conserving action, and material liquid is preheated to a 45-90 DEG C of left side from room temperature
The right side saves steam energy consumption；
3. the raffinate after refinement treatment is boiled the NMP in recycling raffinate using luwa evaporator by the present invention again, NMP is effectively improved
Yield, have significant economic benefit；
4. returning rectifier unit after absorbing liquid cyclic absorption to a certain concentration to continue to recycle NMP, in abundant Recycling of waste liquid
NMP, not only environmentally friendly, the NMP waste liquid return system secondary recovery after absorption also can increase product yield, significantly reduce
The pressure of exhaust gas processing device, while alleviating the pressure of waste water treatment system.
5. directly being preheated to raw material NMP waste liquid since the gaseous phase materials temperature that refining plant generates in step 5 is excessively high
It will lead to the gasification of raw material NMP waste liquid, and require liquid phase feeding in device for deoxidizing, therefore to step 5 in technical solution of the present invention
The gaseous phase materials that middle refining plant generates send back to progress waste heat recycling in raw material preheating device again after being condensed, ensure that de-
Normal charging in oxygen device.
Detailed description of the invention
Fig. 1 is the NMP Mead-Bauer recovery system schematic diagram in embodiment.
1 feed preheater, 2 deoxidation tanks, 3 dehydrating towers, 4 dehydration column reboilers, 5 dehydrating tower condensers, 6 rectifying columns, 7 rectifying
Tower reboiler, 8 rectifying column condensers, 9 treating columns, 10 purification tower reboilers, 11 luwa evaporators, 12 treating column condensers, 13
Tail gas washing tower, 14 circulating pumps.
Specific embodiment
Below in conjunction with attached drawing, invention is further described in detail.
Embodiment 1: as shown in Figure 1, a kind of system of NMP devil liquor recovery, including feed preheater 1, deoxidation tank 2, dehydration
Tower 3, rectifying column 6.Specific recovery method includes the following steps:
Step 1. raw material preheating: the waste liquid from NMP waste tank is preheated with the hot device 1 of pre- raw material is pumped to；
Step 2. deoxidation treatment: the NMP waste liquid after preheating in step 1 is entered into deoxidation tank 2 and is carried out at deoxidation and de- fixed gas
Reason, the operation temperature of deoxidation tank 2 is 45 DEG C, and operating pressure is -0.1MPa；
Step 3. dehydration: the NMP waste liquid after deoxidation treatment is carried out dehydrating with dehydrating tower 3 is pumped to, dehydration column overhead
Temperature is 50 DEG C, and dehydrating tower bottom temperature is 120 DEG C, and the control of dehydration column overhead pressure is -0.1MPa, reflux ratio 1.5, tower top
Light component enters tail gas washing tower 13 after condensing by dehydrating tower condenser 5；
Step 4. rectification process: it is sampled detection in the liquid phase discharge port of dehydrating tower 3, the moisture to tower reactor liquid phase discharge port contains
Amount is less than 300ppm, and the liquid phase material of dehydrating tower 3 is sent by pumping in rectifying column 6 and carries out rectifying, 6 tower top temperature 95 of rectifying column
DEG C, 120 DEG C of bottom temperature, tower top pressure control be -0.1MPa, reflux ratio 1.7, tower top light component pass through rectifying column condenser
2 circular treatment of oxygen tank back off after 8 condensations；
Step 5. refinement treatment: it is sampled detection in the liquid phase discharge port of rectifying column 6, the moisture to tower reactor liquid phase discharge port contains
Amount is less than 30ppm, and the liquid phase material of rectifying column 6 is sent by pumping in treating column 9 and carries out refinement treatment, and 105 DEG C of tower top temperature,
135 DEG C of bottom temperature, reflux ratio 1, tower top pressure control is -0.1MPa, and NMP is discharged by top gaseous phase (or side line), through essence
Tower condenser 12 processed cools down, obtains NMP after 1 recovery waste heat of feed preheater, and tower reactor recombination lease making luwa evaporator 11 is boiled again, filled
After dividing recycling NMP, raffinate sends processing outside after collecting；
Step 6. is sent to 13 absorption of tail gas washing tower after exhaust collection containing NMP and is handled, and absorbing liquid comes from 3 overhead condensation of dehydrating tower
Water, absorbing liquid cyclic absorption exhaust gas containing NMP, absorbing liquid pass through the return deoxidation tank 2 of circulating pump 14 after reaching a certain concentration, repeat
NMP recycling step.
Embodiment 2
As shown in Figure 1, a kind of system of NMP devil liquor recovery, including feed preheater 1, deoxidation tank 2, dehydrating tower 3, rectifying column 6.
Specific recovery method includes the following steps:
Step 1. raw material preheating: the waste liquid from NMP waste tank is preheated with feed preheater 1 is pumped to；
Step 2. deoxidation treatment: the NMP waste liquid after preheating in step 1 is entered into deoxidation tank 2 and is carried out at deoxidation and de- fixed gas
Reason, the operation temperature of deoxidation tank 2 is 45 DEG C, and operating pressure is -0.08MPa；
Step 3. dehydration: the NMP waste liquid after deoxidation treatment is carried out dehydrating with dehydrating tower 3 is pumped to, dehydration column overhead
Temperature is 60 DEG C, and 3 bottom temperature of dehydrating tower is 130 DEG C, 3 tower top pressure of dehydrating tower control be -0.08MPa, reflux ratio 4.5,
Tower top light component enters tail gas washing tower 13 after condensing by dehydrating tower condenser 5；
Step 4. rectification process: it is sampled detection in the liquid phase discharge port of dehydrating tower 3, the moisture to tower reactor liquid phase discharge port contains
Amount is less than 300ppm, and the liquid phase material of dehydrating tower 3 is sent by pumping in rectifying column 6 and carries out rectifying, 6 tower top temperature of rectifying column
105 DEG C, 130 DEG C of bottom temperature, tower top pressure control is -0.08MPa, and reflux ratio 4.2, it is cold that tower top light component passes through rectifying column
2 circular treatment of oxygen tank back off after condenser 8 condenses；
Step 5. refinement treatment: it is sampled detection in the liquid phase discharge port of rectifying column 6, the moisture to tower reactor liquid phase discharge port contains
Amount is less than 30ppm, and the liquid phase material of institute's rectifying column 6 is sent by pumping in treating column 9 and carries out refinement treatment, tower top temperature 115
DEG C, 145 DEG C of bottom temperature, tower top pressure control be -0.08MPa, reflux ratio 4.7, NMP by top gaseous phase (or side line) go out
Expect, NMP is obtained after the cooling for the treatment of column condenser 12,1 recovery waste heat of feed preheater, and tower reactor recombinates lease making luwa evaporator 11 again
Boiling, after sufficiently recycling NMP, raffinate sends processing outside after collecting；
Step 6. is sent to 13 absorption of tail gas washing tower after exhaust collection containing NMP and is handled, and absorbing liquid comes from 3 overhead condensation of dehydrating tower
Water, absorbing liquid cyclic absorption exhaust gas containing NMP, absorbing liquid pass through the return deoxidation tank 2 of circulating pump 14 after reaching a certain concentration, repeat
NMP recycling step.
Embodiment 3.
As shown in Figure 1, a kind of system of NMP devil liquor recovery, including feed preheater 1, deoxidation tank 2, dehydrating tower 3, rectifying column 6.
Specific recovery method includes the following steps:
Step 1. raw material preheating: the waste liquid from NMP waste tank is preheated with feed preheater 1 is pumped to；
Step 2. deoxidation treatment: the NMP waste liquid after preheating in step 1 is entered into deoxidation tank 2 and is carried out at deoxidation and de- fixed gas
Reason, the operation temperature of deoxidation tank 2 is 65 DEG C, and operating pressure is -0.09MPa；
Step 3. dehydration: the NMP waste liquid after deoxidation treatment is carried out dehydrating with dehydrating tower 3 is pumped to, 3 tower of dehydrating tower
Push up temperature be 55 DEG C, dehydrating tower bottom temperature is 125 DEG C, dehydration column overhead pressure control be -0.09MPa, reflux ratio 2.5,
Tower top light component enters tail gas washing tower 13 after condensing by dehydrating tower condenser 5；
Step 4. rectification process: it is sampled detection in the liquid phase discharge port of dehydrating tower 3, the moisture to tower reactor liquid phase discharge port contains
Amount is less than 300ppm, and the liquid phase material of dehydrating tower 3 is sent by pumping in rectifying column 6 and carries out rectifying, the top of the distillation column temperature 100
DEG C, 125 DEG C of bottom temperature, tower top pressure control be -0.09MPa, reflux ratio 2.5, tower top light component by rectifying column condensation
2 circular treatment of oxygen tank back off after device 8 condenses；
Step 5. refinement treatment: it is sampled detection in the liquid phase discharge port of rectifying column 6, the moisture to tower reactor liquid phase discharge port contains
Amount is less than 30ppm, and the liquid phase material of institute's rectifying column 6 is sent by pumping in treating column 9 and carries out refinement treatment, tower top temperature 110
DEG C, 140 DEG C of bottom temperature, tower top pressure control be -0.09MPa, reflux ratio 2.5, NMP by top gaseous phase (or side line) go out
Expect, NMP is obtained after the cooling for the treatment of column condenser 12,1 recovery waste heat of feed preheater, and tower reactor recombinates lease making luwa evaporator 11 again
Boiling, after sufficiently recycling NMP, raffinate sends processing outside after collecting；
Step 6. is sent to 13 absorption of tail gas washing tower after exhaust collection containing NMP and is handled, and absorbing liquid comes from 3 overhead condensation of dehydrating tower
Water, absorbing liquid cyclic absorption exhaust gas containing NMP, absorbing liquid pass through the return deoxidation tank 2 of circulating pump 14 after reaching a certain concentration, repeat
NMP recycling step.
The present invention controls the reflux ratio of each tower in process flow in the range of 1-5, effectively the saving energy；And with year
80,000 tons of NMP scale meters are produced, about 840 tons of NMP in raffinate can be recycled every year, brought benefits about 10,000,000 yuan, economic benefit is bright
It is aobvious.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art
Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this
All by the protection of Patent Law in the scope of the claims of invention.
Claims (8)
1. a kind of method of NMP devil liquor recovery production super-clean high-purity solvent, which is characterized in that comprise the technical steps that:
Step 1. raw material preheating carries out waste heat recycling to NMP waste liquid and preheats；
NMP waste liquid after preheating in step 1 is carried out deoxidation and de- fixed gas is handled by step 2. deoxidation treatment；
NMP waste liquid after deoxidation in step 2 is carried out dehydrating, obtains gaseous component and tower reactor group by step 3. dehydration
Point；
NMP waste liquid dewatered in step 3 is carried out rectification process by step 4. rectification process, obtains light component and tower reactor recombination
Point；
Step 5. refinement treatment, by after rectifying in step 4 NMP waste liquid carry out refinement treatment, obtain first order gaseous phase materials and
First order raffinate, the first order gaseous phase materials obtain after heating in such a way that waste heat recycles to raw material in raw material preheating device
To NMP；
Step 6. vent gas treatment washs tail gas using spray liquid by way of water circulated sprinkling；
In the step 5, is boiled again after the first order raffinate is collected, obtain second level gaseous phase materials and second
Grade raffinate, the second level gaseous phase materials are passed back into refining plant with first order gaseous phase materials jointly in raw material preheating device
In waste heat recycle by way of to raw material heating after obtain NMP, will the second level raffinate collect after be discharged, send processing outside.
2. a kind of method of NMP devil liquor recovery production super-clean high-purity solvent according to claim 1, which is characterized in that institute
It states purification tower overhead gas phase materials and carries out waste heat recycling with the NMP waste liquid in raw material preheating device, make the NMP waste liquid temperature
It increases.
3. a kind of method of NMP devil liquor recovery production super-clean high-purity solvent according to claim 1, which is characterized in that institute
Enter exhaust gas processing device after stating the gaseous component condensation in step 3.
4. a kind of method of NMP devil liquor recovery production super-clean high-purity solvent according to claim 1, which is characterized in that institute
Device for deoxidizing circular treatment is back to after stating the light component condensation in step 4.
5. a kind of method of NMP devil liquor recovery production super-clean high-purity solvent according to claim 1, which is characterized in that institute
It states in step 6, the tail gas after washing enters gas emission device, and the absorbing liquid during vent gas treatment is sent to be followed into device for deoxidizing
Ring processing.
6. a kind of method of NMP devil liquor recovery production super-clean high-purity solvent according to claim 1, which is characterized in that institute
Stating the spray liquid in step 6 is the waste water generated in dehydration device, and operation temperature is 30-70 DEG C, and liquid gas mass ratio is 1-300.
7. a kind of system of NMP devil liquor recovery production super-clean high-purity solvent characterized by comprising raw material preheating device is used for
Raw material is preheated；Device for deoxidizing, for carrying out deoxidation treatment to the raw material after preheating；Dehydration device, after to deoxidation
Raw material be carried out dehydrating；Rectifier unit, for carrying out dehydration rectification process to dewatered raw material；Refining plant is used for
Product treatment is refined out to the material after rectification process；Exhaust gas processing device, for handling tail gas；The raw material
Preheating device is additionally provided with heat exchanger, carries out waste heat recycling with NMP waste liquid for the gaseous phase materials after refinement treatment, makes raw material
NMP waste liquid temperature increases.
8. a kind of system of NMP devil liquor recovery production super-clean high-purity solvent according to claim 7, which is characterized in that institute
Stating refining plant includes luwa evaporator, for refining plant, treated that raffinate boils again, and will be obtained after boiling
Gaseous phase materials send raw material preheating device and NMP waste liquid back to after condensing and carry out waste heat recycling, the raffinate obtained after boiling is arranged
Out, it carries out sending processing outside.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811296250.9A CN109336803B (en) | 2018-11-01 | 2018-11-01 | Method and system for recovering production solvent from NMP waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811296250.9A CN109336803B (en) | 2018-11-01 | 2018-11-01 | Method and system for recovering production solvent from NMP waste liquid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109336803A true CN109336803A (en) | 2019-02-15 |
| CN109336803B CN109336803B (en) | 2021-10-08 |
Family
ID=65313326
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811296250.9A Active CN109336803B (en) | 2018-11-01 | 2018-11-01 | Method and system for recovering production solvent from NMP waste liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109336803B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912485A (en) * | 2019-04-09 | 2019-06-21 | 慈溪市赛思德环保科技有限公司 | A kind of method and system of NMP waste liquid purification |
| CN110668989A (en) * | 2019-10-21 | 2020-01-10 | 南京佳华工程技术有限公司 | Energy-saving separation method and system for DCB-NMP mixture |
| CN111494977A (en) * | 2020-05-19 | 2020-08-07 | 上海盛剑环境系统科技股份有限公司 | Stripping waste liquid recovery system and recovery method |
| CN112225379A (en) * | 2020-10-12 | 2021-01-15 | 重庆工商大学 | Method and device for recovering solvent from chemical synthesis pharmaceutical wastewater |
| CN113354567A (en) * | 2021-06-24 | 2021-09-07 | 索闻特环保科技(上海)有限公司 | Method for preparing anhydrous NMP by mixed solution of NMP and water |
| CN115557872A (en) * | 2022-11-01 | 2023-01-03 | 江苏顺海新能源有限公司 | NMP waste liquid recovery treatment method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013018747A (en) * | 2011-07-12 | 2013-01-31 | Japan Organo Co Ltd | Nmp purification system in electrode production process |
| CN206467171U (en) * | 2017-02-22 | 2017-09-05 | 岳阳市德立机械设备有限公司 | Reclaim, purify the device of N methyl pyrrolidones |
| CN108218756A (en) * | 2018-03-08 | 2018-06-29 | 梁沛文 | A low-temperature recovery system and method for NMP waste water |
| CN207811625U (en) * | 2018-01-08 | 2018-09-04 | 陈宇 | A kind of NMP Mead-Bauer recovery systems |
| CN108658829A (en) * | 2018-07-17 | 2018-10-16 | 天津中福环保科技股份有限公司 | The refined method and apparatus of NMP recycling in a kind of production of lithium battery |
-
2018
- 2018-11-01 CN CN201811296250.9A patent/CN109336803B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013018747A (en) * | 2011-07-12 | 2013-01-31 | Japan Organo Co Ltd | Nmp purification system in electrode production process |
| CN206467171U (en) * | 2017-02-22 | 2017-09-05 | 岳阳市德立机械设备有限公司 | Reclaim, purify the device of N methyl pyrrolidones |
| CN207811625U (en) * | 2018-01-08 | 2018-09-04 | 陈宇 | A kind of NMP Mead-Bauer recovery systems |
| CN108218756A (en) * | 2018-03-08 | 2018-06-29 | 梁沛文 | A low-temperature recovery system and method for NMP waste water |
| CN108658829A (en) * | 2018-07-17 | 2018-10-16 | 天津中福环保科技股份有限公司 | The refined method and apparatus of NMP recycling in a kind of production of lithium battery |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912485A (en) * | 2019-04-09 | 2019-06-21 | 慈溪市赛思德环保科技有限公司 | A kind of method and system of NMP waste liquid purification |
| CN109912485B (en) * | 2019-04-09 | 2024-05-31 | 慈溪市赛思德环保科技有限公司 | NMP waste liquid purification method and system |
| CN110668989A (en) * | 2019-10-21 | 2020-01-10 | 南京佳华工程技术有限公司 | Energy-saving separation method and system for DCB-NMP mixture |
| CN110668989B (en) * | 2019-10-21 | 2023-04-07 | 南京佳华科技股份有限公司 | Energy-saving separation method and system for DCB-NMP mixture |
| CN111494977A (en) * | 2020-05-19 | 2020-08-07 | 上海盛剑环境系统科技股份有限公司 | Stripping waste liquid recovery system and recovery method |
| CN111494977B (en) * | 2020-05-19 | 2023-08-25 | 上海盛剑环境系统科技股份有限公司 | Stripping waste liquid recovery system and recovery method |
| CN112225379A (en) * | 2020-10-12 | 2021-01-15 | 重庆工商大学 | Method and device for recovering solvent from chemical synthesis pharmaceutical wastewater |
| CN113354567A (en) * | 2021-06-24 | 2021-09-07 | 索闻特环保科技(上海)有限公司 | Method for preparing anhydrous NMP by mixed solution of NMP and water |
| CN115557872A (en) * | 2022-11-01 | 2023-01-03 | 江苏顺海新能源有限公司 | NMP waste liquid recovery treatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109336803B (en) | 2021-10-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109336803A (en) | A kind of method and its system of NMP devil liquor recovery production super-clean high-purity solvent | |
| CN108383085B (en) | Device and method for preparing hydrogen chloride gas by full-resolution of hydrochloric acid by continuous method | |
| CN104817481B (en) | Technological method for recovering DMSO from DMSO aqueous solution | |
| CN210085330U (en) | Separation unit for dimethyl sulfoxide recovery | |
| CN108654130A (en) | The method and apparatus of NMP recycling heat pump distillation in a kind of production of lithium electricity | |
| CN109052336A (en) | A kind of dry by-product dilute sulfuric acid purification enrichment facility of chloromethanes and technique | |
| CN114276269A (en) | Recycling treatment method for wastewater in fiber production | |
| CN104926675A (en) | Recovery process of low concentration dimethylacetamide | |
| CN106243068A (en) | A kind of method by coupling rectification purification of tetrahydrofuran | |
| CN110404285A (en) | Four-column distillation and membrane separation integrated system and method for distilling ethanol | |
| CN108939590A (en) | Energy-saving ethylene glycol rectification and purification equipment and technique | |
| CN108658829A (en) | The refined method and apparatus of NMP recycling in a kind of production of lithium battery | |
| CN107973725A (en) | A kind of method and device that DMAC N,N' dimethyl acetamide is recycled from waste water | |
| CN107032555A (en) | A kind of method for handling oil-containing coal gasification waste water | |
| CN107137949A (en) | A kind of extracting rectifying partitioned column device and method of low concentration aqueous isopropanol dehydration | |
| CN104771926A (en) | Rectification device and technological method for recovery of acetic acid from acetic acid aqueous solution | |
| CN110902742A (en) | Method for recovering organic matters in high-concentration organic wastewater | |
| CN107792904A (en) | A kind of technique and device of continuous removal of ammonia and nitrogen light component organic matter and salt | |
| CN207193154U (en) | A kind of recycling treatment system of the recovery of the rectifying from ethanol, water and oily mixed liquor ethanol | |
| CN206980184U (en) | A kind of Pervaporation membrane dehydration of organic solvent equipment | |
| CN214680106U (en) | High-purity anhydrous alcohol production system | |
| CN111921219B (en) | A gas phase separation device and separation method for low boiling point impurities in titanium tetrachloride | |
| CN212594874U (en) | Fusel oil cyclic utilization device in methanol production | |
| CN211836347U (en) | Useless solvent recovery system | |
| CN210506160U (en) | NMP retrieves and hypergravity rectification purification system in lithium cell production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 210009 block D, 19 / F, building B, Jinshan building, No. 8, Shanxi Road, Gulou District, Nanjing, Jiangsu Province Patentee after: Nanjing Jiahua Technology Co.,Ltd. Address before: 210009 -9G, Jinshan building, 8 Shanxi Road, Gulou District, Nanjing, Jiangsu, B Patentee before: NANJING JIAHUA ENGINEERING TECHNOLOGY Co.,Ltd. |