CN210736625U - Electron-grade nitrogen methyl pyrrolidone purification system - Google Patents
Electron-grade nitrogen methyl pyrrolidone purification system Download PDFInfo
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- CN210736625U CN210736625U CN201921279026.9U CN201921279026U CN210736625U CN 210736625 U CN210736625 U CN 210736625U CN 201921279026 U CN201921279026 U CN 201921279026U CN 210736625 U CN210736625 U CN 210736625U
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- purification system
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- 238000000746 purification Methods 0.000 title claims abstract description 21
- OTYYBJNSLLBAGE-UHFFFAOYSA-N CN1C(CCC1)=O.[N] Chemical compound CN1C(CCC1)=O.[N] OTYYBJNSLLBAGE-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 230000018044 dehydration Effects 0.000 claims abstract description 23
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 23
- 239000002699 waste material Substances 0.000 claims abstract description 20
- 238000009835 boiling Methods 0.000 claims abstract description 18
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000007670 refining Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 16
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- -1 alkali metal salts Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling 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
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- Pyrrole Compounds (AREA)
Abstract
The utility model provides an electronic grade nitrogen methyl pyrrolidone purification system, which comprises a mixing tank, a preheating tank, a dehydration device, a separation device, a refining device, a buffer tank, an impurity removal device and a finished product tank; the mixing tank, the preheating tank, the dewatering device, the separating device, the refining device, the cache tank, the impurity removing device and the finished product tank are sequentially communicated through a pipeline. The utility model is provided with the raw material mixing tank, can treat the waste liquid with the NMP content of 60-99 percent, and has high equipment utilization rate; the utility model has the advantages that the separated waste water and low boiling point components are returned to the recovery system from the new part, the inside forms a closed cycle, no waste is discharged, and the NMP utilization rate is greatly improved; the utility model discloses equipment is simple, and technology structure is compact, and production flow is short, has realized circular economy and green production, and the heat make full use of in the device system, equipment energy consumption is low, and economic benefits is high. The utility model discloses a two-stage series connection edulcoration device effectively clears away impurities such as heavy metal ion in the NMP, and gained product purity is high, and the colourity is low.
Description
Technical Field
The utility model relates to a lithium ion battery, chemical material technical field especially relate to an electron level nitrogen methyl pyrrolidone purification system.
Background
NMP is colorless transparent oily liquid, has slight amine smell, can be mutually dissolved with water, alcohol, ether, ester, ketone, halogenated hydrocarbon, aromatic hydrocarbon and castor oil, is an organic solvent commonly used in the chemical field, has low volatility, good thermal stability and chemical stability, can be volatilized along with water vapor, has hygroscopicity and is sensitive to light. With the development of new energy automobiles, lithium ion batteries as a power source of the new energy automobiles enter a rapid development period, electronic grade NMP is generally used at present at a positive pole slurry mixing stage in a lithium ion production process, but with the increase of manufacturing cost of battery enterprises and the requirement of environmental protection, a plurality of enterprises begin to use recovered and purified NMP as a solvent.
The existing nitrogen methyl pyrrolidone production technology generally adopts a multi-stage rectification mode to produce an ultra-pure electronic grade reagent, and the high-purity nitrogen methyl pyrrolidone is prepared by adopting a multi-rectification process in U.S. Pat. No. 4,989,370, European patent EP346086A2, Japanese patent JP06-279401A and JP 08-109167A. The dehydration problem of the azomethyl pyrrolidone in China is also widely concerned, CN101696182A is to remove water by adsorbing the azomethyl pyrrolidone to be purified through a molecular sieve column, the limit of adsorption speed and adsorption capacity is limited, and the treatment capacity is only 0.4-0.8 liter/hour; CN200910064504.9 discloses a purification method of N-methyl pyrrolidone, wherein a water-blocking agent is added into raw material N-methyl pyrrolidone, and then continuous reduced pressure distillation is carried out by a three-tower combined rectification system, so that the purity of the prepared product is more than 99.9%, and the moisture content is less than 0.01%. For the removal of metal ions, U.S. Pat. No. 4,983,370 discloses a process for removing metal ions as impurities by adding alkali metals or alkali metal salts, followed by continuous fractional rectification to obtain high purity NMP. Generally, the current methods have complex process operation, difficult operation control, large energy consumption and low efficiency.
In conclusion, how to realize simple and efficient purification of NMP, the defects of high energy consumption, complex operation and the like of the dehydration technology in the existing NMP purification process are overcome, and the problem of green, environment-friendly and efficient production of enterprises is urgently needed to be solved at present.
SUMMERY OF THE UTILITY MODEL
Based on the technical problem who exists among the background art, the utility model provides an electron level nitrogen methyl pyrrolidone purification system.
The utility model provides an electronic grade nitrogen methyl pyrrolidone purification system, which comprises a mixing tank, a preheating tank, a dehydration device, a separation device, a refining device, a buffer tank, an impurity removal device and a finished product tank; the mixing tank, the preheating tank, the dewatering device, the separating device, the refining device, the cache tank, the impurity removing device and the finished product tank are sequentially communicated through a pipeline.
Preferably, a stirring device is arranged in the mixing tank.
Preferably, the system also comprises a first heater and a first cooler, the first heater supplies heat to the dehydration device, a liquid outlet of the dehydration device is communicated with a liquid inlet of the separation device through a pipeline, a water outlet of the dehydration device is communicated with a water inlet of the first cooler through a pipeline, and a water outlet of the first cooler is communicated with the mixing tank through a pipeline.
Preferably, the dehydration device adopts a fractionating tower, a rectifying tower or a dehydration tower.
Preferably, the system also comprises a second heater and a second cooler, the second heater supplies heat to the separation device, the separation device separates the waste liquid according to different boiling points of the components, a high boiling point component outlet of the separation device is communicated with a liquid inlet of the refining device through a pipeline, a low boiling point component outlet of the separation device is communicated with a liquid inlet of the second cooler through a pipeline, and a liquid outlet of the second cooler is communicated with the dehydration device through a pipeline.
Preferably, the system also comprises a third heater and a third cooler, the third heater supplies heat to the refining device, the refining device separates the waste liquid according to different boiling points of the components, a low-boiling-point component outlet of the refining device is communicated with a liquid inlet of the third cooler through a pipeline, and a liquid outlet of the third cooler is communicated with the cache tank through a pipeline.
Preferably, the impurity removing device comprises a first-stage impurity removing device and a second-stage impurity removing device which are connected in sequence.
Preferably, the system also comprises a heat supplier for supplying heat to the preheating tank, the first heater, the second heater and the third heater.
The utility model provides an electron level nitrogen methyl pyrrolidone purification system through the waste liquid to different nitrogen methyl pyrrolidone contents, through heating the waste liquid, makes the solute of difference wherein reach the boiling point, separates out impurity such as moisture, light low boiling point component in the waste liquid, uses porous resin to adsorb heavy metal ion wherein through the physics method again, reaches the purpose of purification nitrogen methyl pyrrolidone.
The utility model is provided with the raw material mixing tank, can treat the waste liquid with the NMP content of 60-99 percent, and has high equipment utilization rate; the utility model has the advantages that the separated waste water and low boiling point components are returned to the recovery system from the new part, the inside forms a closed cycle, no waste is discharged, and the NMP utilization rate is greatly improved; the utility model has simple equipment, compact process structure, short production flow, realization of circular economy and green production, full utilization of heat in the device system, low energy consumption of the equipment and high economic benefit; the utility model discloses a two-stage series connection edulcoration device effectively clears away impurities such as heavy metal ion in the NMP, and gained product purity is high, and the colourity is low.
Drawings
FIG. 1 is a flow chart of a system for purifying electronic grade N-methyl pyrrolidone according to the present invention.
Detailed Description
Referring to fig. 1, the utility model provides an electronic grade nitrogen methyl pyrrolidone purification system, which comprises a mixing tank, a preheating tank, a dehydration device, a separation device, a refining device, a cache tank, an impurity removal device, a finished product tank, a first heater, a first cooler, a second heater, a second cooler, a third heater, a third cooler and a heater; the heater supplies heat for the preheating tank, the first heater, the second heater and the third heater.
A stirring device is arranged in the mixing tank, NMP waste liquid in the raw material mixing tank is mechanically stirred for a certain time to be uniformly mixed and then is led into the preheating tank through a pipeline, a heat supplier supplies heat to the preheating tank to preliminarily heat the waste liquid, and the preliminarily heated waste liquid is led into the dehydration device through a pipeline; the dehydration device adopts a fractionating tower, a rectifying tower or a dehydration tower, the second heater supplies heat to the dehydration device to further heat the waste liquid, after the boiling point of water is reached, the water is evaporated and directly enters the first cooler, the water is cooled and then is led into the mixing tank through a pipeline, and the rest waste liquid is led into the separation device through a pipeline; the second heater supplies heat to the separation device, further heats the waste liquid, introduces components with a boiling point lower than that of NMP into the second cooler through a pipeline, introduces the components into the dehydration device through a pipeline after cooling, and introduces the residual NMP components into the refining device through a pipeline; the third heater is a station of the refining device, liquid is further heated, components with the boiling point higher than that of NMP are separated, the residual pure NMP components are led into the third cooler, and are led into the buffer tank for temporary storage after being cooled; and finally, introducing the NMP solution into a finished product tank through a pipeline, and waiting for filling and shipment after the NMP solution is checked to be qualified.
The utility model discloses a to the waste liquid of different nitrogen methyl pyrrolidone contents, through the heating waste liquid, make different solutes wherein reach the boiling point, isolate impurity such as moisture, light low boiling point component in the waste liquid, use porous resin to adsorb heavy metal ion wherein through the physics method again, reach the purpose of purification nitrogen methyl pyrrolidone.
The above, only be the concrete implementation of the preferred embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art is in the technical scope of the present invention, according to the technical solution of the present invention and the utility model, the concept of which is equivalent to replace or change, should be covered within the protection scope of the present invention.
Claims (8)
1. An electronic-grade N-methyl pyrrolidone purification system is characterized by comprising a mixing tank, a preheating tank, a dehydration device, a separation device, a refining device, a cache tank, an impurity removal device and a finished product tank; the mixing tank, the preheating tank, the dewatering device, the separating device, the refining device, the cache tank, the impurity removing device and the finished product tank are sequentially communicated through a pipeline.
2. The electronic-grade N-methylpyrrolidone purification system according to claim 1, wherein an agitation device is disposed within the mixing tank.
3. The purification system of electronic-grade N-methyl pyrrolidone as claimed in claim 1 or 2, further comprising a first heater and a first cooler, wherein the first heater supplies heat to the dehydration device, a liquid outlet of the dehydration device is communicated with a liquid inlet of the separation device through a pipeline, a water outlet of the dehydration device is communicated with a water inlet of the first cooler through a pipeline, and a water outlet of the first cooler is communicated with the mixing tank through a pipeline.
4. The electronic-grade N-methylpyrrolidone purification system according to claim 3, wherein the dehydration device is a fractionating tower, a rectifying tower or a dehydration tower.
5. The electronic-grade nitrogen methyl pyrrolidone purification system of claim 3, further comprising a second heater and a second cooler, wherein the second heater supplies heat to the separation device, the separation device separates the waste liquid according to different boiling points of the components, the outlet of the high boiling point component of the separation device is communicated with the liquid inlet of the refining device through a pipeline, the outlet of the low boiling point component of the separation device is communicated with the liquid inlet of the second cooler through a pipeline, and the liquid outlet of the second cooler is communicated with the dehydration device through a pipeline.
6. The electronic-grade nitrogen methyl pyrrolidone purification system of claim 5, further comprising a third heater and a third cooler, wherein the third heater supplies heat to the refining device, the refining device separates the waste liquid according to different boiling points of components, a low boiling point component outlet of the refining device is communicated with a liquid inlet of the third cooler through a pipeline, and a liquid outlet of the third cooler is communicated with the buffer tank through a pipeline.
7. The electronic-grade N-methylpyrrolidone purification system according to claim 6, wherein the impurity removal device comprises a first-stage impurity removal device and a second-stage impurity removal device which are connected in sequence.
8. The electronic-grade nitrogen methyl pyrrolidone purification system of claim 7, further comprising a heat supply for supplying heat to the preheat tank, the first heater, the second heater, and the third heater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921279026.9U CN210736625U (en) | 2019-08-08 | 2019-08-08 | Electron-grade nitrogen methyl pyrrolidone purification system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921279026.9U CN210736625U (en) | 2019-08-08 | 2019-08-08 | Electron-grade nitrogen methyl pyrrolidone purification system |
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| Publication Number | Publication Date |
|---|---|
| CN210736625U true CN210736625U (en) | 2020-06-12 |
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| CN201921279026.9U Active CN210736625U (en) | 2019-08-08 | 2019-08-08 | Electron-grade nitrogen methyl pyrrolidone purification system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978233A (en) * | 2020-09-15 | 2020-11-24 | 安徽英特力工业工程技术有限公司 | Device for improving purity of NMP crude product after methylamine removal |
-
2019
- 2019-08-08 CN CN201921279026.9U patent/CN210736625U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978233A (en) * | 2020-09-15 | 2020-11-24 | 安徽英特力工业工程技术有限公司 | Device for improving purity of NMP crude product after methylamine removal |
| CN111978233B (en) * | 2020-09-15 | 2024-05-14 | 安徽英特力工业工程技术有限公司 | Device for improving purity of NMP crude product after demethanization |
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