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Method for catalyzing and synthesizing alpha-pyrrolidone by using granular solid superacid

A solid super acid, pyrrolidone technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry and other directions, can solve the problems of low reaction conversion rate and yield, increase the difficulty of product purification, and high temperature. Simple processing, excellent catalytic activity and high product yield

Inactive Publication Date: 2015-04-08
TONGREN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) The reaction pressure is high and the temperature is high, which puts forward high requirements for the design of the equipment
[0006] (2) The reaction conversion rate and yield are low, and a small amount of raw material GBL and intermediate 1-hydroxybutyramide have not reacted completely. Since the boiling point difference between the raw material GBL and the product α-pyrrolidone is very small, this increases the purification of the product Difficulty, to obtain high-purity-pyrrolidone products can only be processed by adding alkali to remove GBL and then distill
[0007] (3) Most of them are batch reactions, and it is difficult to obtain high space-time yields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add catalyst: put Φ=4~6mm granular SO in the fixed bed 4 2- / M x o y 150g of quasi-solid superacid catalyst;

[0023] (2) Heating: Heating to raise the temperature to 260-280°C;

[0024] (3) Introduce nitrogen: at a space velocity of 70cm 3 / min Feed nitrogen into the fixed bed, so that the catalyst is always in a state of nitrogen protection;

[0025] (4) Mixing of raw materials: Mix 1,4-butyrolactone (GBL) and ammonia water at a molar ratio of GBL:ammonia water=1:1.2 at -25°C;

[0026] (5) Input the mixed solution of GBL and ammonia water: input the mixed aqueous solution of GBL and ammonia water to the fixed bed at a weight space velocity of 0.5g / min;

[0027] (6) Product formation: GBL and ammonia water are dehydrated under the continuous catalysis of a hot catalyst to generate α-pyrrolidone;

[0028] (7) Product post-treatment: After the above reaction, the mixed gas of α-pyrrolidone and water discharged from the outlet of the fixed bed is condensed by a...

Embodiment 2

[0030] (1) Add catalyst: put Φ=4~6mm granular SO in the fixed bed 4 2～ / M x o y 200g of quasi-solid superacid catalyst;

[0031] (2) Heating: Heating to raise the temperature to 220-240°C;

[0032] (3) Introduce nitrogen: at a space velocity of 70cm 3 / min Feed nitrogen into the fixed bed, so that the catalyst is always in a state of nitrogen protection;

[0033] (4) Mixing of raw materials: Mix 1,4-butyrolactone (GBL) and ammonia water at a molar ratio of GBL:ammonia water=1:1.5 at -25°C;

[0034] (5) Input the mixed solution of GBL and ammonia water: input the mixed aqueous solution of GBL and ammonia water to the fixed bed at a weight space velocity of 0.4g / min;

[0035] (6) Product formation: GBL and ammonia water are dehydrated under the continuous catalysis of a hot catalyst to generate α-pyrrolidone;

[0036] (7) Product post-treatment: After the above reaction, the mixed gas of α-pyrrolidone and water discharged from the outlet of the fixed bed is condensed by a...

Embodiment 3

[0038] (1) Add catalyst: put Φ=4~6mm granular SO in the fixed bed 4 2～ / M x o y 180g of quasi-solid superacid catalyst;

[0039] (2) Heating: Heating to raise the temperature to 260-280°C;

[0040] (3) Introduce nitrogen: at a space velocity of 70cm 3 / min Feed nitrogen into the fixed bed, so that the catalyst is always in a state of nitrogen protection;

[0041] (4) Mixing of raw materials: Mix 1,4-butyrolactone (GBL) and ammonia water at a molar ratio of GBL:ammonia water=1:2 at -25°C;

[0042] (5) Input the mixed solution of GBL and ammonia water: input the mixed aqueous solution of GBL and ammonia water to the fixed bed at a weight space velocity of 0.5g / min;

[0043] (6) Product formation: GBL and ammonia water are dehydrated under the continuous catalysis of a hot catalyst to generate α-pyrrolidone;

[0044] (7) Product post-treatment: After the above reaction, the mixed gas of α-pyrrolidone and water discharged from the outlet of the fixed bed is condensed by a c...

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PUM

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Abstract

The invention discloses a method for catalyzing and synthesizing alpha-pyrrolidone by using granular solid superacid. The method is characterized by taking 1,4-butyrolactone (GBL) and ammonium hydroxide as raw materials, gasifying the raw materials at the normal pressure under the nitrogen protection, reacting the raw materials in a fixed bed filled with a solid superacid catalyst, condensing, collecting, dewatering and rectifying a reaction product to obtain alpha-pyrrolidone with a content which reaches over 99.5%, wherein the monomer conversion rate in the raw materials is near 100%; the yield reaches over 95%. The method has the advantages of being simple in catalyzing process, high in yield and purity of product, low in cost and continuous in production; the industrial production is greatly facilitated.

Description

technical field [0001] The present invention relates to a synthesis method of high-efficiency and high-quality organic solvents, in particular to a method of catalytic synthesis using 1,4-butyrolactone (GBL) and ammonia water as raw materials and granular solid superacid as catalyst at normal pressure fixed bed α-pyrrolidone method. Background technique [0002] α-pyrrolidone, formula C 4 h 7 NO is an efficient and excellent organic solvent, and it is also an important chemical raw material. It is widely used in medicine, textiles, dyes, paints, cosmetics and other industries, such as the manufacture of Naofukang, nylon 4, polyvinylpyrrolidone, Artificial blood, etc. The current synthesis methods of α-pyrrolidone include 1-butanolamine oxidative dehydration method, 1,4-succinic acid ammoniation reduction method, 1-chlorobutyryl chloride ammoniation method, 1,4-butyrolactone ammoniation method, etc. But at present, the only industrialized production method is the aminatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267B01J27/053
CPCC07D207/267
Inventor 张玲钰李修刚杨晓红王霞
Owner TONGREN UNIV