CN111138336A - Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone - Google Patents
Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone Download PDFInfo
- Publication number
- CN111138336A CN111138336A CN201911409442.0A CN201911409442A CN111138336A CN 111138336 A CN111138336 A CN 111138336A CN 201911409442 A CN201911409442 A CN 201911409442A CN 111138336 A CN111138336 A CN 111138336A
- Authority
- CN
- China
- Prior art keywords
- methyl pyrrolidone
- purity
- ultra
- environment
- saving
- 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.)
- Pending
Links
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000010924 continuous production Methods 0.000 title claims abstract description 31
- 238000004821 distillation Methods 0.000 claims abstract description 41
- OTYYBJNSLLBAGE-UHFFFAOYSA-N CN1C(CCC1)=O.[N] Chemical compound CN1C(CCC1)=O.[N] OTYYBJNSLLBAGE-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 239000002808 molecular sieve Substances 0.000 claims abstract description 24
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 claims abstract description 24
- 238000009833 condensation Methods 0.000 claims abstract description 14
- 230000005494 condensation Effects 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 150000002500 ions Chemical class 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 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
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
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)
- Pyrrole Compounds (AREA)
Abstract
The embodiment of the invention discloses an efficient, energy-saving and environment-friendly continuous production process of ultra-clean and high-purity N-methyl pyrrolidone, which comprises the steps of rectifying a N-methyl pyrrolidone raw material to prepare N-methyl pyrrolidone steam, then condensing to prepare N-methyl pyrrolidone, then entering from the bottom of a molecular sieve adsorption tower, dehydrating by the molecular sieve adsorption tower, then flowing out from the top of the tower, and performing ion resin exchange filtration to prepare the ultra-clean and high-purity N-methyl pyrrolidone. The embodiment of the invention provides an efficient, energy-saving and environment-friendly continuous production process for ultra-clean high-purity isopropanol, and the ultra-clean high-purity N-methyl pyrrolidone is prepared by rectification, condensation, impurity removal and filtration, so that the problem of low purity of the ultra-clean high-purity N-methyl pyrrolidone in the prior art can be effectively solved; in addition, the raw material of the nitrogen methyl pyrrolidone is added into a distillation still for treatment by adopting the rectification method of the invention, so that impurities can be further removed, and the yield is improved.
Description
Technical Field
The invention relates to the field of microelectronic chemical reagent production, in particular to an efficient, energy-saving and environment-friendly continuous production process of ultra-clean and high-purity N-methyl pyrrolidone.
Background
N-methyl pyrrolidone, named NMP in Chinese, is a colorless transparent oily liquid and has slight odor of amine. It can be mutually dissolved with water, alcohol, ether, ester, ketone, halohydrocarbon, aromatic hydrocarbon and castor oil, and has the advantages of low volatility, good thermal stability and chemical stability, and can be volatilized with water vapor, and has hygroscopicity and photosensitivity to light. The ultra-pure N-methyl pyrrolidone (NMP) is a common solvent in the electronic industry, and the quality of N-methyl pyrrolidone products directly influences the production and quality of high-end electronic products.
At present, the technology for producing electronic grade N-methyl pyrrolidone in a large scale is mainly monopolized by developed countries, and the purity of the ultra-pure N-methyl pyrrolidone is not high, so that the normal use of people is influenced. Therefore, how to improve the purity of N-methylpyrrolidone (NMP) is a problem to be solved.
Disclosure of Invention
Therefore, the embodiment of the invention provides an efficient, energy-saving, environment-friendly and continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which aims to solve the problem that the purity of the ultra-clean high-purity N-methyl pyrrolidone is not high in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
according to the first aspect of the embodiment of the invention, an efficient, energy-saving and environment-friendly continuous production process of ultra-clean and high-purity N-methyl pyrrolidone is provided, which comprises the steps of rectifying a N-methyl pyrrolidone raw material to prepare N-methyl pyrrolidone steam, then condensing to prepare N-methyl pyrrolidone, then entering from the bottom of a molecular sieve adsorption tower, dehydrating by the molecular sieve adsorption tower, then flowing out from the top of the tower, and performing ion resin exchange filtration to prepare the ultra-clean and high-purity N-methyl pyrrolidone.
Further, the rectification treatment comprises the steps that the raw material of the nitrogen methyl pyrrolidone is added into a distillation still at one time, liquid in the distillation still is heated to be boiled and then is transferred into a condenser for condensation, part of condensed liquid flows into the top of the tower, and when the liquid in the distillation still is reduced to a preset value, the liquid in the distillation still is discharged and condensed at one time.
Further, when the liquid in the distillation kettle is reduced to a preset value, the raw material of the N-methyl pyrrolidone is added again for rectification treatment, and continuous production is realized.
Furthermore, during the distillation, various fractions in different time periods are collected by a plurality of fraction tanks, and the various fractions in the time periods can be recycled, so that the generation of waste liquid is avoided, and the method is green and environment-friendly.
Further, the rectification treatment comprises the step of preparing the nitrogen methyl pyrrolidone steam in a rectification tower of the nitrogen methyl pyrrolidone raw material.
Furthermore, the raw material of the nitrogen methyl pyrrolidone is an industrial grade nitrogen methyl pyrrolidone raw material.
Further, the nitrogen methyl pyrrolidone steam is condensed in a condenser.
Furthermore, the temperature in the whole reaction environment is 86-96 ℃, and the pressure is 0.1 atm.
According to the second aspect of the embodiment of the invention, the ultra-clean high-purity N-methyl pyrrolidone is prepared by the efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methyl pyrrolidone.
The embodiment of the invention has the following advantages: the embodiment of the invention provides an efficient, energy-saving and environment-friendly continuous production process for ultra-clean high-purity isopropanol, and the ultra-clean high-purity N-methyl pyrrolidone is prepared by rectification, condensation, impurity removal and filtration, so that the problem of low purity of the ultra-clean high-purity N-methyl pyrrolidone in the prior art can be effectively solved; in addition, the raw material of the nitrogen methyl pyrrolidone is added into a distillation still for treatment by adopting the rectification method of the invention, so that impurities can be further removed, and the yield is improved. The whole process is simple to operate, mild in reaction conditions, the temperature is controlled to be 86-96 ℃ and the pressure is 0.1atm in the whole process, the high efficiency and energy conservation of the production process are guaranteed, no waste liquid is generated in production, and the environment is protected.
Drawings
FIG. 1 is a process flow chart of the high-efficiency, energy-saving and environment-friendly continuous production process of ultra-clean and high-purity isopropanol provided by the invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that unless otherwise specified, technical terms or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the present invention pertains, and experimental materials in the following examples are commercially available unless otherwise specified, and the experimental methods described are general experimental methods unless otherwise specified.
In view of the deficiencies in the prior art, the inventor of the present invention has made extensive studies and extensive practices to propose the technical solution of the present invention, and further explains the technical solution, the implementation process and the principle thereof, etc.
As shown in fig. 1, an aspect of an embodiment of the present invention provides an efficient, energy-saving, environment-friendly and continuous production process of ultra-clean and high-purity nitrogen methyl pyrrolidone, which includes rectifying raw material of nitrogen methyl pyrrolidone to obtain nitrogen methyl pyrrolidone steam, then condensing to obtain nitrogen methyl pyrrolidone, then entering the bottom of a molecular sieve adsorption tower, dehydrating the nitrogen methyl pyrrolidone in the molecular sieve adsorption tower, flowing out from the top of the tower, and performing ion resin exchange filtration to obtain the ultra-clean and high-purity nitrogen methyl pyrrolidone.
Preferably, the rectification treatment comprises the steps of adding the raw material of the nitrogen methyl pyrrolidone into a distillation kettle at one time, heating the liquid in the distillation kettle to boil, transferring the liquid into a condenser for condensation, allowing part of the condensed liquid to flow into the top of the tower, and discharging the liquid in the distillation kettle for condensation at one time when the liquid in the distillation kettle is reduced to a preset value.
Preferably, when the liquid in the distillation kettle is reduced to a preset value, the raw material of the N-methyl pyrrolidone is added again for rectification treatment, so that continuous production is realized.
Preferably, during the distillation, a plurality of fraction tanks are used for collecting various fractions in different time periods, and the various fractions in each time period can be recycled, so that waste liquid is avoided, and the method is green and environment-friendly.
Preferably, the rectification treatment comprises the step of rectifying the raw material of the N-methyl pyrrolidone in a rectifying tower to obtain N-methyl pyrrolidone steam.
Preferably, the raw material of the nitrogen methyl pyrrolidone is industrial nitrogen methyl pyrrolidone raw material.
Preferably, the nitrogen methyl pyrrolidone vapour is condensed in a condenser.
Preferably, the temperature in the whole reaction environment is 86-96 ℃ and the pressure is 0.1 atm.
According to the second aspect of the embodiment of the invention, the ultra-clean high-purity N-methyl pyrrolidone is prepared by the efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methyl pyrrolidone. The technical solution of the present invention is further described in detail by the following examples. However, the examples are chosen only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of adding an industrial-grade N-methyl pyrrolidone raw material into a distillation kettle at one time under the integral reaction environment with the temperature of 86-91 ℃ and the pressure of 0.1atm, heating liquid in the distillation kettle to boil and then transferring the liquid into a condenser for condensation, allowing a condensate part to flow into the top of the tower, discharging the liquid in the distillation kettle into the condenser at one time when the liquid in the distillation kettle is reduced to a preset value, condensing to obtain N-methyl pyrrolidone, introducing the N-methyl pyrrolidone into the bottom of a molecular sieve adsorption tower, dehydrating the N-methyl pyrrolidone in the molecular sieve adsorption tower, flowing out of the top of the tower, and performing ion resin exchange filtration to obtain the ultra-clean high-purity N.
Example 2
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of putting an industrial-grade N-methyl pyrrolidone raw material into a rectifying tower for rectification under the integral reaction environment with the temperature of 86-91 ℃ and the pressure of 0.1atm to prepare N-methyl pyrrolidone steam, then transferring the N-methyl pyrrolidone steam into a condenser, preparing N-methyl pyrrolidone after condensation, then entering the N-methyl pyrrolidone through the bottom of a molecular sieve adsorption tower, flowing out from the top of the tower after dehydration of the molecular sieve adsorption tower, and performing ion resin exchange filtration to prepare the ultra-clean high-purity N-methyl pyrrolidone.
Example 3
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of adding an industrial-grade N-methyl pyrrolidone raw material into a distillation kettle at one time under the integral reaction environment with the temperature of 91-96 ℃ and the pressure of 0.1atm, heating liquid in the distillation kettle to boil and then transferring the liquid into a condenser for condensation, allowing a condensate part to flow into the top of the tower, discharging the liquid in the distillation kettle into the condenser at one time when the liquid in the distillation kettle is reduced to a preset value, condensing to obtain N-methyl pyrrolidone, introducing the N-methyl pyrrolidone into the bottom of a molecular sieve adsorption tower, dehydrating the N-methyl pyrrolidone in the molecular sieve adsorption tower, flowing out of the top of the tower, and performing ion resin exchange filtration to obtain the ultra-clean high-purity N.
Example 4
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of putting an industrial-grade N-methyl pyrrolidone raw material into a rectifying tower for rectification under the integral reaction environment with the temperature of 91-96 ℃ and the pressure of 0.1atm to prepare N-methyl pyrrolidone steam, then transferring the N-methyl pyrrolidone steam into a condenser, preparing N-methyl pyrrolidone after condensation, then entering the N-methyl pyrrolidone through the bottom of a molecular sieve adsorption tower, flowing out from the top of the tower after dehydration of the molecular sieve adsorption tower, and performing ion resin exchange filtration to prepare the ultra-clean high-purity N-methyl pyrrolidone.
Example 5
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of adding an industrial-grade N-methyl pyrrolidone raw material into a distillation kettle at one time under the integral reaction environment with the temperature of 80-85 ℃ and the pressure of 0.1atm, heating liquid in the distillation kettle to boil and then transferring the liquid into a condenser for condensation, allowing a condensate part to flow into the top of the tower, discharging the liquid in the distillation kettle into the condenser at one time when the liquid in the distillation kettle is reduced to a preset value, condensing to obtain N-methyl pyrrolidone, introducing the N-methyl pyrrolidone into the bottom of a molecular sieve adsorption tower, dehydrating the N-methyl pyrrolidone in the molecular sieve adsorption tower, flowing out of the top of the tower, and performing ion resin exchange filtration to obtain the ultra-clean high-purity N.
Example 6
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of putting an industrial-grade N-methyl pyrrolidone raw material into a rectifying tower for rectification under the integral reaction environment that the temperature is 80-85 ℃ and the pressure is 0.1atm to prepare N-methyl pyrrolidone steam, then transferring the N-methyl pyrrolidone steam into a condenser, preparing N-methyl pyrrolidone after condensation, then entering the N-methyl pyrrolidone through the bottom of a molecular sieve adsorption tower, flowing out from the top of the tower after dehydration of the molecular sieve adsorption tower, and performing ion resin exchange filtration to prepare the ultra-clean high-purity N-methyl pyrrolidone.
Example 7
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of adding an industrial-grade N-methyl pyrrolidone raw material into a distillation kettle at one time under the integral reaction environment with the temperature of 97-102 ℃ and the pressure of 0.1atm, heating liquid in the distillation kettle to boil and then transferring the liquid into a condenser for condensation, allowing a condensate part to flow into the top of the tower, discharging the liquid in the distillation kettle into the condenser at one time when the liquid in the distillation kettle is reduced to a preset value, condensing to obtain N-methyl pyrrolidone, introducing the N-methyl pyrrolidone into the bottom of a molecular sieve adsorption tower, dehydrating the N-methyl pyrrolidone in the molecular sieve adsorption tower, flowing out of the top of the tower, and performing ion resin exchange filtration to obtain the ultra-clean high-purity N.
Example 8
The embodiment provides an efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which comprises the steps of putting an industrial-grade N-methyl pyrrolidone raw material into a rectifying tower for rectification under the integral reaction environment with the temperature of 97-102 ℃ and the pressure of 0.1atm to prepare N-methyl pyrrolidone steam, then transferring the N-methyl pyrrolidone steam into a condenser, preparing N-methyl pyrrolidone after condensation, then entering the N-methyl pyrrolidone through the bottom of a molecular sieve adsorption tower, flowing out from the top of the tower after dehydration of the molecular sieve adsorption tower, and performing ion resin exchange filtration to prepare the ultra-clean high-purity N-methyl pyrrolidone.
The yields of ultra-clean high-purity N-methyl pyrrolidone in examples 1 to 8 are shown in the following tables, and examples 1, 3, 5 and 7 were treated by the distillation method of the present invention in a distillation still, while examples 2, 4, 6 and 8 were treated by directly placing them in a distillation column; wherein, the temperature of the whole reaction environment of the application is 86-96 ℃ lower than that of the example 5 and the example 6, and the temperature of the whole reaction environment of the application is 86-96 ℃ higher than that of the example 7 and the example 8.
The experimental results show that the impurity can be further removed by adding the raw material of the nitrogen methyl pyrrolidone into the distillation kettle for treatment by adopting the rectification method, so that the yield is improved; the temperature of the whole reaction environment is lower than or higher than 86-96 ℃ of the temperature of the whole reaction environment, and the yield is greatly reduced.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (9)
1. An efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone, which is characterized by comprising the following steps: the method comprises the steps of rectifying a raw material of the nitrogen methyl pyrrolidone to prepare nitrogen methyl pyrrolidone steam, then condensing to prepare the nitrogen methyl pyrrolidone, then entering the nitrogen methyl pyrrolidone from the bottom of a molecular sieve adsorption tower, dehydrating the nitrogen methyl pyrrolidone in the molecular sieve adsorption tower, then flowing out from the top of the tower, and performing ion resin exchange filtration to prepare the ultra-clean high-purity nitrogen methyl pyrrolidone.
2. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 1, characterized by comprising the following steps: the rectification treatment comprises the steps that the raw material of the nitrogen methyl pyrrolidone is added into a distillation still at one time, liquid in the distillation still is heated to be boiled and then is transferred into a condenser for condensation, part of condensed liquid flows into the top of the tower, and when the liquid in the distillation still is reduced to a preset value, the liquid in the distillation still is discharged and condensed at one time.
3. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 2, characterized by comprising the following steps: when the liquid in the distillation kettle is reduced to a preset value, the raw material of the N-methyl pyrrolidone is added again for rectification treatment.
4. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 2, characterized by comprising the following steps: during the distillation, various fractions were collected for different periods of time using multiple distillation pots.
5. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 1, characterized by comprising the following steps: the rectification treatment comprises the step of preparing nitrogen methyl pyrrolidone steam in a nitrogen methyl pyrrolidone raw material rectification tower.
6. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 1, characterized by comprising the following steps: the raw material of the nitrogen methyl pyrrolidone is an industrial grade nitrogen methyl pyrrolidone raw material.
7. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 1, characterized by comprising the following steps: the nitrogen methyl pyrrolidone vapour is condensed in a condenser.
8. The efficient, energy-saving and environment-friendly continuous production process of the ultra-clean high-purity N-methylpyrrolidone according to claim 1, characterized by comprising the following steps: the temperature in the whole reaction environment is 86-96 ℃, and the pressure is 0.1 atm.
9. An ultra-clean high-purity N-methyl pyrrolidone is characterized in that: the ultra-clean high-purity N-methyl pyrrolidone is prepared by the high-efficiency energy-saving environment-friendly continuous production process of the ultra-clean high-purity N-methyl pyrrolidone disclosed by any one of claims 1-8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911409442.0A CN111138336A (en) | 2019-12-31 | 2019-12-31 | Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911409442.0A CN111138336A (en) | 2019-12-31 | 2019-12-31 | Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111138336A true CN111138336A (en) | 2020-05-12 |
Family
ID=70522659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911409442.0A Pending CN111138336A (en) | 2019-12-31 | 2019-12-31 | Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111138336A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001986A (en) * | 2010-12-23 | 2011-04-06 | 上海化学试剂研究所 | Method for improving quality of industrial N-methylpyrrolidone |
| CN107464964A (en) * | 2017-08-03 | 2017-12-12 | 百川化工(如皋)有限公司 | From the method for lithium ion battery recovery N methyl pyrrolidones |
| CN108299266A (en) * | 2018-01-30 | 2018-07-20 | 宁波大学 | The preparation method of high purity N-methyl pyrrolidone |
| CN108794371A (en) * | 2017-04-27 | 2018-11-13 | 迈奇化学股份有限公司 | A kind of process for purification of N-Methyl pyrrolidone product |
| CN110183369A (en) * | 2019-05-23 | 2019-08-30 | 安徽京控环境技术服务有限公司 | A method of the separating-purifying N-Methyl pyrrolidone from useless paint stripper |
-
2019
- 2019-12-31 CN CN201911409442.0A patent/CN111138336A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001986A (en) * | 2010-12-23 | 2011-04-06 | 上海化学试剂研究所 | Method for improving quality of industrial N-methylpyrrolidone |
| CN108794371A (en) * | 2017-04-27 | 2018-11-13 | 迈奇化学股份有限公司 | A kind of process for purification of N-Methyl pyrrolidone product |
| CN107464964A (en) * | 2017-08-03 | 2017-12-12 | 百川化工(如皋)有限公司 | From the method for lithium ion battery recovery N methyl pyrrolidones |
| CN108299266A (en) * | 2018-01-30 | 2018-07-20 | 宁波大学 | The preparation method of high purity N-methyl pyrrolidone |
| CN110183369A (en) * | 2019-05-23 | 2019-08-30 | 安徽京控环境技术服务有限公司 | A method of the separating-purifying N-Methyl pyrrolidone from useless paint stripper |
Non-Patent Citations (1)
| Title |
|---|
| 化工百科全书编辑委员会编: "《化工百科全书》", 30 September 1993, 化学工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111792685B (en) | System and method for continuously recycling NMP from NMP wastewater | |
| CN108558602A (en) | Double thick double smart four tower quadruple effect energy-saving distillings production alcohol fuel systems and its application method | |
| CN109336803A (en) | A kind of method and its system of NMP devil liquor recovery production super-clean high-purity solvent | |
| CN107032959A (en) | A kind of heat pump and the methanol rectification method of multiple-effect coupling | |
| CN105779129A (en) | Method for preparing Artemisia apiacea volatile oil from Artemisia apiacea waste mother liquor, method for preparing byproduct and obtained byproduct | |
| CN110404285A (en) | Four column distillations and UF membrane integrated system and its method for distilling ethyl alcohol | |
| CN101979381B (en) | Method for refining crude quinoline by continuous rectification | |
| CN114588650B (en) | Combined hydrochloric acid resolving process | |
| CN103396297B (en) | Thermal coupling energy saving system and operation method for recovering organism from propylene epoxidation reaction wastewater | |
| CN112142618A (en) | Low-concentration dimethyl formamide wastewater recovery system and method | |
| CN107032555A (en) | A kind of method for handling oil-containing coal gasification waste water | |
| CN111925301B (en) | Method for recovering acetonitrile from waste solvent | |
| CN111138336A (en) | Efficient, energy-saving and environment-friendly continuous production process of ultra-clean high-purity N-methyl pyrrolidone | |
| CN203419863U (en) | Thermal coupling energy-saving system for reclaiming organic matters from propylene epoxidation waste water | |
| CN208649168U (en) | Double thick double smart four tower quadruple effect energy-saving distillings produce alcohol fuel system | |
| CN111170823B (en) | Method for simultaneously extracting phenol and naphthalene from tar | |
| CN205024120U (en) | Methanol recovery device | |
| CN213327409U (en) | Purification device of isopropyl alcohol | |
| CN203060873U (en) | Continuous rectifying tower for N-methylaniline | |
| CN212152190U (en) | Coal tar three-tower continuous deep processing system | |
| CN115108958A (en) | NMP purification method | |
| KR20120022020A (en) | Refine alcohol distillation system | |
| CN106276799B (en) | A kind of preparation method and device of electronic grade high-purity chlorine | |
| CN113813625A (en) | Device and method for recovering light alcohol by combining MVR with recovery tower | |
| CN112250575A (en) | Method for recovering propylene glycol methyl ether acetate from semiconductor diluent waste liquid |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200512 |
|
| RJ01 | Rejection of invention patent application after publication |