CN113651744A - Process for removing impurities in high-purity N-methyl pyrrolidone - Google Patents
Process for removing impurities in high-purity N-methyl pyrrolidone Download PDFInfo
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- CN113651744A CN113651744A CN202110733333.5A CN202110733333A CN113651744A CN 113651744 A CN113651744 A CN 113651744A CN 202110733333 A CN202110733333 A CN 202110733333A CN 113651744 A CN113651744 A CN 113651744A
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- China
- Prior art keywords
- methyl pyrrolidone
- screening device
- purity
- removing impurities
- molecular screening
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000012535 impurity Substances 0.000 title claims abstract description 13
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000012528 membrane Substances 0.000 claims abstract description 20
- 238000012216 screening Methods 0.000 claims abstract description 16
- 238000005373 pervaporation Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000007873 sieving Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000007098 aminolysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000001944 continuous distillation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- -1 nitrogen heterocyclic compound Chemical class 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
Abstract
The invention discloses a process for removing impurities in high-purity N-methyl pyrrolidone, which comprises the following steps: preheating N-methyl pyrrolidone in a preheater at the flow rate of 30-100ml/min, carrying out pervaporation through a molecular screening device at the pressure of 40-500Pa, and collecting N-methyl pyrrolidone with methylamine and moisture removed after passing through a screen membrane circulating pipeline of the molecular screening device; after multiple times of circulating filtration, high-purity N-methyl pyrrolidone is obtained; the method has the advantages of simple and convenient operation, low energy consumption, good effect and wide industrial production prospect.
Description
Technical Field
The invention relates to the technical field of N-methyl pyrrolidone production, in particular to a process for removing impurities in high-purity N-methyl pyrrolidone.
Background
N-methylpyrrolidone (NMP) belongs to nitrogen heterocyclic compound, and is mainly applied to petrochemical industry, plastic industry, medicine, pesticide, dye, lithium ion battery manufacturing industry and other industries. In the microelectronic industry and the semiconductor industry, N-methyl pyrrolidone can be used for cleaning agents of precision instruments or circuit boards, photoresist removing liquid, solvents for LCD liquid crystal material production, electrode auxiliary materials of lithium batteries and the like. Due to the rapid development of the IT industry, especially along with the development of miniaturization and high-speed processing of integrated circuits, the requirements for methylamine and moisture in the sesmic 8 standard of N-methylpyrrolidone are strict, namely, the content of methylamine is less than 5ppm, and the content of moisture is less than 0.03%.
In the prior art, the N-methyl pyrrolidone is prepared by aminolysis of gamma-butyrolactone serving as a raw material and methylamine, and inevitable impurities such as methylamine, moisture and the like exist. In the existing N-methyl pyrrolidone purification technology, the method for removing methylamine and moisture mainly adopts continuous distillation or micro-boiling distillation; however, the method has high investment cost and complex process operation, and is difficult to popularize and apply.
Disclosure of Invention
The invention aims to provide an impurity removal process to overcome the defects of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
a process for removing impurities in high-purity N-methyl pyrrolidone comprises the following steps:
preheating N-methyl pyrrolidone in a preheater at the flow rate of 30-100ml/min, carrying out pervaporation through a molecular screening device at the pressure of 40-500Pa, and collecting N-methyl pyrrolidone with methylamine and moisture removed after passing through a screen membrane circulating pipeline of the molecular screening device; after multiple times of circulating filtration, the high-purity N-methyl pyrrolidone is obtained.
Preferably, the preheating temperature of the N-methyl pyrrolidone is 85-130 ℃, and the temperature of the N-methyl pyrrolidone in the molecular sieving device is kept above 85 ℃.
Preferably, the sieve membrane circulation pipeline is spirally arranged in the molecular screening device, and the sieve membrane holes of the sieve membrane circulation pipeline can only pass methylamine molecules and water molecules.
Preferably, the discharge port of the molecular screening device is connected to the raw material tank through a membrane pump; and is communicated with the discharge tank through a valve.
Preferably, the waste port of the molecular sieving apparatus is connected to the canister by a valve.
Compared with the prior art, the invention has the beneficial effects that:
in the method, N-methyl pyrrolidone is subjected to pervaporation, methylamine and moisture in the N-methyl pyrrolidone can be effectively removed through one-step simple cyclic operation, the purity of the obtained N-methyl pyrrolidone is more than or equal to 99.8 percent, the content of methylamine is lower than 5ppm, the moisture content is less than 0.03 percent, and the obtained N-methyl pyrrolidone completely meets the SEMIC8 standard; the method has the advantages of simple operation, low energy consumption, good effect and wide industrial production prospect.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view of the preparation process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Referring to fig. 1, the present invention provides a technical solution:
a process for removing impurities in high-purity N-methyl pyrrolidone comprises the following steps:
preheating N-methyl pyrrolidone in a preheater 2 at the flow rate of 30-100ml/min, carrying out pervaporation through a molecular screening device 3 at the pressure of 40-500Pa, and collecting N-methyl pyrrolidone with methylamine and moisture removed after passing through a sieve membrane circulating pipeline of the molecular screening device 3; after multiple times of circulating filtration, the high-purity N-methyl pyrrolidone is obtained.
Preferably, the preheating temperature of the N-methylpyrrolidone is 85-130 ℃, and the temperature of the N-methylpyrrolidone in the molecular sieving device 3 is kept above 85 ℃.
Preferably, the sieve membrane circulation pipeline is spirally arranged in the molecular sieving device 3, and the sieve membrane holes of the sieve membrane circulation pipeline can only pass methylamine molecules and water molecules.
Preferably, the discharge port of the molecular sieving device 3 is connected to the raw material tank 1 through a membrane pump 4; and communicates with the discharge tank 5 through a valve 6.
Preferably, the waste port of the molecular sieving apparatus 3 is connected to a waste tank 7 through a valve 6.
In the embodiment:
5000ml of industrial grade N-methyl pyrrolidone is placed in a raw material tank 1, preheated to 90 ℃ through a preheater 2 at the flow rate of 50ml/min, then subjected to pervaporation through a molecular screening device 3, the pressure of the molecular screening device 3 is controlled to be 500Pa, feed liquid passes through a screen membrane circulating pipeline, returns to the raw material tank 1 through a membrane pump 4, and is screened for methylamine molecules and water molecules through the screen membrane pores of the screen membrane circulating pipeline. After 120min, sampling and analyzing from a valve 6, wherein the content of methylamine in the feed liquid is 3.5ppm, the content of water is 0.006 percent, and the detection result meets the SEMIC8 standard; the separated methylamine molecules and water molecules are collected in a waste tank 7 through a valve 6.
In the method, N-methyl pyrrolidone is subjected to pervaporation, methylamine and moisture in the N-methyl pyrrolidone can be effectively removed through one-step simple cyclic operation, the purity of the obtained N-methyl pyrrolidone is more than or equal to 99.8 percent, the content of methylamine is lower than 5ppm, the moisture content is less than 0.03 percent, and the obtained N-methyl pyrrolidone completely meets the SEMIC8 standard; the method has the advantages of simple operation, low energy consumption, good effect and wide industrial production prospect.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. A process for removing impurities in high-purity N-methyl pyrrolidone is characterized by comprising the following steps: the method comprises the following steps:
preheating N-methylpyrrolidone in a preheater (2) at the flow rate of 30-100ml/min, carrying out pervaporation through a molecular screening device (3) at the pressure of 40-500Pa, and collecting N-methyl pyrrolidone with methylamine and moisture removed after passing through a sieve membrane circulating pipeline of the molecular screening device (3); after multiple times of circulating filtration, the high-purity N-methyl pyrrolidone is obtained.
2. The process according to claim 1 for removing impurities from high purity N-methylpyrrolidone, wherein: the preheating temperature of the N-methyl pyrrolidone is 85-130 ℃, and the temperature of the N-methyl pyrrolidone in the molecular screening device (3) is kept above 85 ℃.
3. The process according to claim 1 for removing impurities from high purity N-methylpyrrolidone, wherein: the sieve membrane circulating pipeline is spirally arranged in the molecular screening device (3), and the sieve membrane holes of the sieve membrane circulating pipeline can only pass methylamine molecules and water molecules.
4. The process according to claim 1 for removing impurities from high purity N-methylpyrrolidone, wherein: the discharge hole of the molecular screening device (3) is connected to the raw material tank (1) through a membrane pump (4); and is communicated with the discharge tank (5) through a valve (6).
5. The process according to claim 1 for removing impurities from high purity N-methylpyrrolidone, wherein: the waste port of the molecular screening device (3) is connected to a waste tank (7) through a valve (6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110733333.5A CN113651744A (en) | 2021-06-30 | 2021-06-30 | Process for removing impurities in high-purity N-methyl pyrrolidone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110733333.5A CN113651744A (en) | 2021-06-30 | 2021-06-30 | Process for removing impurities in high-purity N-methyl pyrrolidone |
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| CN113651744A true CN113651744A (en) | 2021-11-16 |
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| CN202110733333.5A Pending CN113651744A (en) | 2021-06-30 | 2021-06-30 | Process for removing impurities in high-purity N-methyl pyrrolidone |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696182A (en) * | 2009-09-10 | 2010-04-21 | 北京益利精细化学品有限公司 | Purifying method of N-methylpyrrolidone |
| CN101973921A (en) * | 2010-09-29 | 2011-02-16 | 上海化学试剂研究所 | Method for removing methylamine and moisture in N-methyl pyrrolidone |
| CN102399179A (en) * | 2010-09-17 | 2012-04-04 | 上海化学试剂研究所 | Production process for ultra-pure N-methylpyrrolidone |
| CN108299266A (en) * | 2018-01-30 | 2018-07-20 | 宁波大学 | The preparation method of high purity N-methyl pyrrolidone |
-
2021
- 2021-06-30 CN CN202110733333.5A patent/CN113651744A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696182A (en) * | 2009-09-10 | 2010-04-21 | 北京益利精细化学品有限公司 | Purifying method of N-methylpyrrolidone |
| CN102399179A (en) * | 2010-09-17 | 2012-04-04 | 上海化学试剂研究所 | Production process for ultra-pure N-methylpyrrolidone |
| CN101973921A (en) * | 2010-09-29 | 2011-02-16 | 上海化学试剂研究所 | Method for removing methylamine and moisture in N-methyl pyrrolidone |
| CN108299266A (en) * | 2018-01-30 | 2018-07-20 | 宁波大学 | The preparation method of high purity N-methyl pyrrolidone |
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