CN113548996B - Synthesis process of N-ethyl pyrrolidone - Google Patents
Synthesis process of N-ethyl pyrrolidone Download PDFInfo
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- CN113548996B CN113548996B CN202110993744.8A CN202110993744A CN113548996B CN 113548996 B CN113548996 B CN 113548996B CN 202110993744 A CN202110993744 A CN 202110993744A CN 113548996 B CN113548996 B CN 113548996B
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- monoethylamine
- butyrolactone
- gamma
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- ethyl pyrrolidone
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Chemistry (AREA)
- Pyrrole Compounds (AREA)
Abstract
The invention discloses a synthesis process of N-ethyl pyrrolidone, which comprises the following steps: (1) Raw materials of gamma-butyrolactone and monoethylamine are added into a preheater for preheating through a metering pump; (2) After preheating, uniformly mixing the gamma-butyrolactone and the monoethylamine to obtain a mixed material; (3) Continuously heating the mixed material, reacting for 1.5-2 hours after heating, and fully reacting to obtain a reaction product; (4) The reaction product is cooled to 40-60 ℃ firstly, then subjected to depressurization treatment, and finally enters a deamination tower to remove excessive monoethylamine and water. The synthesis process of N-ethyl pyrrolidone adopting the structure has the advantages of short reaction time, no need of using a catalyst, low cost, low pressure drop and normal pressure after the reaction is finished, and improvement of the safety of the reaction.
Description
Technical Field
The invention relates to the technical field of fine chemical product preparation, in particular to a synthesis process of N-ethyl pyrrolidone.
Background
N-ethyl pyrrolidone is an important organic chemical solvent and an auxiliary agent, and has very important application in the fields of petrochemical industry, medicines, cosmetics, foods, coatings, photosensitive materials and the like. Among them, N-ethyl pyrrolidone is widely used in chemical industrial production due to its superior dissolving capacity, stable chemical properties, and non-corrosiveness.
In the prior art, the N-ethyl pyrrolidone synthesis technology has the problems of high reaction pressure, long reaction period, high safety risk, high catalyst cost and the like.
Disclosure of Invention
The invention aims to provide a synthesis process of N-ethyl pyrrolidone, which has short reaction time, does not need to use a catalyst, reduces cost, reduces normal pressure by high pressure after the reaction is finished, and improves the safety of the reaction.
The invention provides a synthesis process of N-ethyl pyrrolidone, 1. The synthesis process of N-ethyl pyrrolidone is characterized in that: the method comprises the following steps:
(1) Raw materials of gamma-butyrolactone and monoethylamine are added into a preheater for preheating through a metering pump;
(2) After preheating, uniformly mixing the gamma-butyrolactone and the monoethylamine to obtain a mixed material;
(3) Continuously heating the mixed material, reacting for 1.5-2 hours after heating, and fully reacting to obtain a reaction product;
(4) The reaction product is cooled to 40-60 ℃ firstly, then subjected to depressurization treatment, and finally enters a deamination tower to remove excessive monoethylamine and water;
the reaction principle is as follows:
preferably, in the step (1), the molar ratio of the gamma-butyrolactone to the monoethylamine is 1:1-1:1.5.
Preferably, in the step (1), the gamma-butyrolactone is pumped out of the storage tank by a gamma-butyrolactone metering pump to a pressure of 7.0-8.0 MPa.
Preferably, in the step (1), the monoethylamine is pumped out of the storage tank by a monoethylamine metering pump to a pressure of 7.0-8.0 MPa.
Preferably, in step (1), the preheater is heated to 150 ℃.
Preferably, in step (2), the mixing is performed in a static mixer.
Preferably, in the step (3), the temperature rise is performed in an inner tube of the jacketed reactor, the temperature of the heat conduction oil in an outer tube of the jacketed reactor is 260-270 ℃, and the temperature rise of the mixed material is 230-280 ℃.
Preferably, in the step (4), the cooling is that the reaction product is cooled by a product cooler after heat exchange of a raw material exchange heat exchanger.
Therefore, the synthesis process of N-ethyl pyrrolidone adopting the structure has short reaction time, does not need to use a catalyst, reduces the cost, reduces the normal pressure by high pressure after the reaction is finished, and improves the safety of the reaction.
The technical scheme of the invention is further described in detail through examples.
Detailed Description
The present invention will be further described with reference to examples in which various chemicals and reagents are commercially available unless otherwise specified.
Example 1
Pumping out the gamma-butyrolactone serving as a reaction raw material through a gamma-butyrolactone metering pump, boosting the pressure to 7.5MPa, and sending the gamma-butyrolactone into a preheater for preheating; pumping the other reaction raw material monoethylamine out by a monoethylamine metering pump, boosting the pressure to 7.5MPa, merging the monoethylamine metering pump and GBL, then sending the monoethylamine into a preheating pre-heater to be heated to 150 ℃, uniformly mixing the monoethylamine with the gamma-butyrolactone by a static mixer, heating the mixed material by heat conduction oil at 260 ℃ outside the tube after the mixed material enters the inner tube of a jacket tube type reactor, and carrying out reaction for 1.6 hours to ensure that the temperature of the material reaches 250 ℃. The reaction product is cooled to 40 ℃ by a product cooler after heat exchange by a raw material/product heat exchanger, enters a constant pressure tank, passes through a flow limiting orifice plate under the control of liquid, causes the material to be subjected to high pressure drop to normal pressure, and then enters a deamination tower to remove excessive monoethylamine and water, thus obtaining qualified N-ethyl pyrrolidone.
The product obtained in this example has a yield of 98.17% and a purity of 98.99%.
Example 2
Pumping out the gamma-butyrolactone serving as a reaction raw material through a gamma-butyrolactone metering pump, boosting the pressure to 7.0MPa, and sending the gamma-butyrolactone into a preheater for preheating; pumping the other reaction raw material monoethylamine out by a monoethylamine metering pump, boosting the pressure to 7.0MPa, merging the monoethylamine metering pump and GBL, then sending the monoethylamine into a preheating pre-heater to be heated to 150 ℃, uniformly mixing the monoethylamine with the gamma-butyrolactone by a static mixer, wherein the molar ratio of the gamma-butyrolactone to the monoethylamine is 1:1, heating the mixed material by heat conducting oil at 270 ℃ outside the tube after the mixed material enters the inner tube of a jacket tube type reactor, and reacting for 1.8 hours to ensure the sufficient reaction. The reaction product is cooled to 50 ℃ by a product cooler after heat exchange by a raw material/product heat exchanger, enters a constant pressure tank, passes through a flow limiting orifice plate under the control of liquid, causes the material to be subjected to high pressure drop to normal pressure, and then enters a deamination tower to remove excessive monoethylamine and water, thus obtaining qualified N-ethyl pyrrolidone.
The product obtained in this example has a yield of 98.87% and a purity of 99.19%.
Therefore, the synthesis process of N-ethyl pyrrolidone adopting the structure has the advantages of short reaction time, no need of using a catalyst, low cost, high pressure drop and low normal pressure after the reaction is finished, high safety of the reaction, and high yield and purity of the product.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (2)
1. The synthesis process of the N-ethyl pyrrolidone is characterized by comprising the following steps of:
(1) Raw materials of gamma-butyrolactone and monoethylamine are added into a preheater for preheating through a metering pump; the preheater is heated to 150 ℃; the molar ratio of the gamma-butyrolactone to the monoethylamine is 1:1-1:1.5; the gamma-butyrolactone is pumped out of the storage tank from the storage tank after being boosted to 7.0-8.0 MPa by a gamma-butyrolactone metering pump; the monoethylamine is boosted to 7.0-8.0 MPa by a monoethylamine metering pump and is pumped out of the storage tank;
(2) After preheating, uniformly mixing the gamma-butyrolactone and the monoethylamine to obtain a mixed material;
(3) Continuously heating the mixed material, reacting for 1.5-2 hours after heating, and fully reacting to obtain a reaction product; the temperature rise is carried out in an inner pipe of the jacketed reactor, the temperature of heat conduction oil in an outer pipe of the jacketed reactor is 260-270 ℃, and the temperature rise temperature of the mixed material is 250-260 ℃;
(4) The reaction product is cooled to 40-60 ℃ firstly, then subjected to depressurization treatment, and finally enters a deamination tower to remove excessive monoethylamine and water; the cooling is that the reaction product is cooled by a product cooler after heat exchange of a raw material exchange heat exchanger;
the reaction principle is as follows:
2. the process for synthesizing N-ethyl pyrrolidone according to claim 1, wherein the process comprises the steps of: in step (2), the mixing is performed in a static mixer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104725293A (en) * | 2015-02-11 | 2015-06-24 | 沈阳化工大学 | Continuous production method of alpha-pyrrolidone |
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| WO2007131929A1 (en) * | 2006-05-16 | 2007-11-22 | Basf Se | Process for continuously preparing n- ethyl-2-pyrrolidone (nep) |
| CN107474003B (en) * | 2017-09-29 | 2021-03-05 | 中国科学院大连化学物理研究所 | Method for continuously synthesizing N-methyl pyrrolidone and N-ethyl pyrrolidone |
| CN110183370B (en) * | 2019-06-28 | 2022-04-29 | 迈奇化学股份有限公司 | Industrial production method of N-ethyl pyrrolidone |
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