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A kind of industrial production method of n-ethylpyrrolidone

A technology of ethylpyrrolidone and ethylamine, which is applied in the field of fine chemical product preparation, can solve problems such as short reaction time, high equipment requirements, and unstable effects, and achieve the goal of avoiding the increase of side reactions, good product purity, and suppressing side reactions Effect

Active Publication Date: 2022-04-29
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the characteristics of short reaction time and high yield, but reducing the material at 240°C to 0-5°C in a short period of time requires high equipment requirements. At the same time, micro-reaction, as an emerging technology, has relatively high investment costs , the effect is not stable, also can find that its yield is the highest more than 90% from its embodiment, minimum only has 43.7%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] An industrial production method for N-ethylpyrrolidone, using gamma-butyrolactone and monoethylamine as raw materials, under the action of a catalyst, to synthesize N-ethylpyrrolidone, the total amount of catalyst in the two-stage reactor is 1000g, and the upper stage reacts 200g of container filling, 800g of filling of lower section reactor; comprise the following steps:

[0042] Step 1, 10kg of γ-butyrolactone and 1.74kg of 1,4-butanediol are continuously and evenly added to the stirring tank with a metering pump according to the ratio of 1000:174, and fully mixed, the catalyst is filled in the stirring tank, and the stirring The still has a jacket and a stirrer inside. Several tubes with holes are welded on the concentric discs of the stirrer. The tubes are filled with catalysts, and 1,4-butanediol passes through the columns. The outflow from the hole on the tube is fully mixed with the γ-butyrolactone in the stirring tank. Under the rotation of the agitator, the mix...

Embodiment 2

[0057] Repeat the processing condition of embodiment 1, the processing capacity of catalyst is tested, 1000g catalyst can handle 305kg gamma-butyrolactone altogether.

Embodiment 3

[0059] The industrial production method of a kind of N-ethylpyrrolidone described in this embodiment is different from Example 1 in that:

[0060] In step 2, the reaction temperature in the reaction stage is 120°C, the reaction pressure is 1.6MPa, and the material and the catalyst are fully reacted for 0.8h;

[0061] The molar ratio of monoethylamine to γ-butyrolactone is 1.05:1; the molar ratio of 1,4-butanediol to γ-butyrolactone is 0.3:1;

[0062] The weight percent composition of the catalyst is 23.5% Cu, 8.2% γ-Al 2 o 3 , 6.5%Ni, 2.3%Ag, 1.3%Bi, and the balance is carrier. The carrier is composed of component A and component B, the component A is silicon dioxide, and the component B is zinc oxide. For the preparation method, refer to Example 1, and details are not repeated here.

[0063] The yield of the terminal product obtained in this example is 99.47%, the purity is 99.99%, the water content is 40ppm, and the free amine content is 1.5ppm.

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Abstract

The invention provides an industrial production method of N-ethylpyrrolidone, which belongs to the technical field of preparation of fine chemical products, and comprises the following steps: Step 1, adding γ-butyrolactone into a stirred tank, and a tube is welded on the stirrer, The catalyst is filled in the tube, and the solvent flows out through the holes on the tube and fully mixed with γ-butyrolactone; step 2, the material flowing out of the stirred tank is fully mixed with monoethylamine and then sent to the tube reactor, and the feeder has Atomizing nozzle, after the solvent is atomized, it is fully mixed with the material from the upper reaction section, collected, and evenly enters the tubes of the lower reaction section after passing through the distributor; step 3, the product flowing out of the tube-and-tube reactor is sent to the stirring In the jacket of the kettle, after exchanging heat with the material in step 1, it flows out from the outlet of the jacket and enters the refining stage. The invention solves the shortcomings of high reaction temperature, high reaction pressure, high equipment requirements and low environmental protection benefit existing in the existing N-ethylpyrrolidone production.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, in particular to an industrial production method of N-ethylpyrrolidone. Background technique [0002] The patent document with the publication number CN105237456A discloses a production method of pyrrolidone products. It introduces the direct production of pyrrolidone by using 1,4-butanediol as a raw material through one-step reaction, and realizes 1 by using segmented reactors and combined catalysts. , 4-butanediol is converted into pyrrolidone series products in one reaction unit through dehydrogenation-amination reaction. After careful research and judgment, it was found that the method is completed in two reactors in one reaction unit. The first stage of the reaction is mainly based on the dehydrogenation of 1,4-butanediol to produce γ-butyrolactone, and the second stage of the reaction is Mainly synthesize pyrrolidones by amination of γ-butyrolactone. Since th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/267B01J23/89B01J37/34B01J37/10
CPCC07D207/267B01J23/8973B01J23/002B01J37/346B01J37/10B01J2523/00B01J2523/17B01J2523/18B01J2523/31B01J2523/41B01J2523/48B01J2523/54B01J2523/847B01J2523/27B01J2523/22
Inventor 宋国全吴彦彬李凯闫广学肖强杨理吴正岭李清霞
Owner MAIQI CHEM CO LTD
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