A kind of method for continuously synthesizing n-methylpyrrolidone and n-ethylpyrrolidone

A technology of ethylpyrrolidone and methylpyrrolidone, which is applied in the field of continuous synthesis of N-methylpyrrolidone and N-ethylpyrrolidone using micro-reaction technology, can solve the problems of high reaction pressure, high safety risk, high catalyst cost, etc. The effect of improving efficiency

Active Publication Date: 2021-03-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The above-mentioned N-methylpyrrolidone and N-ethylpyrrolidone synthesis technologies have problems such as high reaction temperature, high reaction pressure, long reaction cycle, high safety risk, and high catalyst cost.

Method used

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  • A kind of method for continuously synthesizing n-methylpyrrolidone and n-ethylpyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Prepare 1.25M γ-butyrolactone solution 1 and 1.5M methylamine solution 2 with ethylene glycol as a solvent, and the two materials pass through metering pump 3 and metering pump 4 through one-way flow at 0.1ml / min and 0.1ml / min respectively. The valves 5 and 6 are sent to the micro-mixer 7 and then enter the micro-reactor system to start the reaction at normal temperature. After that, the reaction liquid enters the air bath temperature control zone 8. The temperature in the temperature control zone is controlled at 290°C. The reaction residence time in the zone is 13.3min, and the reacted material enters the cooling zone 9, and the cold fluid heat exchange is used to suppress the reaction. The residence time of the reaction suppression section is 42 seconds, and the pressure of the system is stabilized at 5.2 through the back pressure valve 10. MPa, the reaction product is collected at the outlet of the microreactor system, and the collected sample 11 is processed and ana...

Embodiment 2

[0019] Prepare 1.25M gamma-butyrolactone solution 1 and 1.5M ethylamine solution 2 with ethylene glycol as a solvent, and the two materials pass through metering pump 3 and metering pump 4 through one-way The valves 5 and 6 are sent to the micro-mixer 7 and then enter the micro-reactor system to start the reaction at normal temperature. After that, the reaction liquid enters the air bath temperature control zone 8. The temperature in the temperature control zone is controlled at 290°C. The reaction residence time in the zone is 13.3min, and the reacted material enters the cooling zone 9, and the cold fluid heat exchange is used to suppress the reaction. The residence time of the reaction suppression section is 42 seconds, and the pressure of the system is stabilized at 5.2 through the back pressure valve 10. MPa, the reaction product was collected at the outlet of the microreactor system, and the collected sample 11 was processed and then analyzed by gas chromatography and comb...

Embodiment 3

[0021] Use ethylene glycol as a solvent to prepare 2M γ-butyrolactone solution 1 and 2.8M methylamine solution 2, and the two materials pass through metering pump 3 and metering pump 4 through the check valve at flow rates of 0.1ml / min and 0.1ml / min respectively 5 and 6 are transported to the micro-mixer 7 and then enter the micro-reactor system to start the reaction at room temperature, and then the reaction liquid enters the air bath temperature control zone 8, the temperature in the temperature control zone is controlled at 290 ° C, and the two materials are in the temperature control zone The reaction residence time of the reaction is 13.3min, and the reacted material enters the cooling zone 9, and the cold fluid is used to exchange heat to suppress the reaction. The residence time of the reaction suppression section is 42 seconds, and the pressure of the system is controlled at 5.2MPa through the back pressure valve 10. , the reaction product was collected at the outlet of...

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Abstract

A method for continuously synthesizing N-methylpyrrolidone and N-ethylpyrrolidone, the method is carried out in a microreactor, and gamma-butyrolactone solution and corresponding alkylamine solution are continuously passed through a microreactor to synthesize N-methylpyrrolidone and N-ethylpyrrolidone. Wherein, the microreactor includes a reaction section and a reaction suppression section, and the reaction mixture is carried out under the condition that the residence time of the reaction mixture is 1 to 30 minutes, and wherein the γ-butyrolactone solution and the corresponding alkylamine solution Both use ethylene glycol as a solvent, the molar ratio of alkylamine and γ-butyrolactone in the reaction mixture is 1.0-1.6, and the concentration of the γ-butyrolactone solution is 0.5-2 mol / L. The invention can shorten the synthesis process time of N-methylpyrrolidone and N-ethylpyrrolidone from several hours to within 30 minutes, and meanwhile, the yield of the product reaches more than 90%.

Description

technical field [0001] The invention relates to a method for continuously synthesizing N-methylpyrrolidone and N-ethylpyrrolidone, in particular to a method for continuously synthesizing N-methylpyrrolidone and N-ethylpyrrolidone using micro-reaction technology. Background technique [0002] N-methylpyrrolidone and N-ethylpyrrolidone are important organic chemical solvents and additives, and have very important applications in many fields such as petrochemicals, medicine, cosmetics, food, coatings, and photosensitive materials. Among them, N-methylpyrrolidone / N-ethylpyrrolidone, as an organic solvent, is widely used in chemical industry production due to its advantages of outstanding solvency, stable chemical properties and non-corrosiveness. [0003] US Pat.6248902 uses gamma-butyrolactone and methylamine to continuously non-catalyze the synthesis of N-methylpyrrolidone under the pressure of 30.4-91.2 barg in the third-stage reaction section: a) the operating temperature of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 陈光文周峰焦凤军王克军
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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