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Synthetic method for preparing cyclopropyl methyl ketone by cracking alpha-acetyl-gamma-butyrolactone

A technology for the synthesis of cyclopropylmethyl ketone, which is applied in the preparation of heterocyclic compounds and organic chemistry, can solve the problems of low reaction yield, high reaction temperature, and strong corrosion, so as to promote the mass transfer process and improve Reaction efficiency, the effect of ensuring uniformity

Active Publication Date: 2019-04-12
JIANGSU YUXIANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction temperature of this route is too high, which is difficult for general enterprises to achieve. At the same time, the reaction yield is low, generally lower than 90%, and the product content is also low, containing more cracking by-products, which is caused by insufficient catalyst activity.
[0007] The existing catalytic cracking method of α-acetyl-γ-butyrolactone has more or less defects, or the product yield is low, or the corrosion is too strong in the reaction process, or the cost is too high
Existing technical routes need to be improved in terms of environmental friendliness and cost

Method used

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  • Synthetic method for preparing cyclopropyl methyl ketone by cracking alpha-acetyl-gamma-butyrolactone
  • Synthetic method for preparing cyclopropyl methyl ketone by cracking alpha-acetyl-gamma-butyrolactone
  • Synthetic method for preparing cyclopropyl methyl ketone by cracking alpha-acetyl-gamma-butyrolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) In the injection loop reactor based on the Venturi effect, add the α-acetyl-γ-butyrolactone raw material, remove oxygen and fill it with inert gas for replacement protection, and turn on the external circulation pump 3 for high-speed injection mixing.

[0033] (2) Turn on the heat exchanger 2, control the temperature at 140°C, slowly add the α-acetyl-γ-butyrolactone raw material and the catalyst through the material inlet 5 into the injection loop reactor, and spray and mix through the injection mixer 1 And realize sufficient catalytic cracking reaction. Catalyst 1.0kg (sodium chloride: ZIF-8=1:0.05), the particle size of the catalyst is less than 2000 microns.

[0034] (3) From the top of the reaction kettle, the pyrolysis product cyclopropyl methyl ketone is continuously condensed and extracted from the cyclopropyl methyl ketone extraction outlet 6, and the waste material is discharged from the sewage outlet 4. At the same time, the raw material of α-acetyl-γ-but...

Embodiment 2

[0036] (1) In the injection loop reactor based on the Venturi effect, add the α-acetyl-γ-butyrolactone raw material, remove oxygen and fill it with inert gas for replacement protection, and turn on the external circulation pump 3 for high-speed injection mixing.

[0037] (2) Turn on the heat exchanger 2, control the temperature at 100°C, slowly add the α-acetyl-γ-butyrolactone raw material and the catalyst through the material inlet 5 into the injection loop reactor, and spray and mix through the injection mixer 1 And realize sufficient catalytic cracking reaction. Catalyst 1.0kg (sodium iodide: ZIF-8=1:0.5), the particle size of the catalyst is less than 500 microns.

[0038] (3) From the top of the reaction kettle, the pyrolysis product cyclopropyl methyl ketone is continuously condensed and extracted from the cyclopropyl methyl ketone extraction outlet 6, and the waste material is discharged from the sewage outlet 4. At the same time, the raw material of α-acetyl-γ-butyrol...

Embodiment 3

[0040] (1) In the injection loop reactor based on the Venturi effect, add the α-acetyl-γ-butyrolactone raw material, remove oxygen and fill it with inert gas for replacement protection, and turn on the external circulation pump 3 for high-speed injection mixing.

[0041](2) Turn on the heat exchanger 2, control the temperature at 130°C, slowly add the α-acetyl-γ-butyrolactone raw material and the catalyst through the material inlet 5 into the injection loop reactor, and spray and mix through the injection mixer 1 And realize sufficient catalytic cracking reaction. Catalyst 1.0kg (potassium iodide: ZIF-8=1:0.1), the particle size of the catalyst is less than 1000 microns.

[0042] (3) From the top of the reaction kettle, the pyrolysis product cyclopropyl methyl ketone is continuously condensed and extracted from the cyclopropyl methyl ketone extraction outlet 6, and the waste material is discharged from the sewage outlet 4. At the same time, the raw material of α-acetyl-γ-buty...

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Abstract

The invention discloses a synthetic method for preparing cyclopropyl methyl ketone by cracking alpha-acetyl-gamma-butyrolactone, which comprises the following steps of: adding alpha-acetyl-gamma-butyrolactone material in a venturi-based jet loop reactor, deoxidizing and filling inert gases for replacement and protection, turning on an outside circulating pump for high-speed jet mix, and the like.By the adoption of the synthetic method for preparing the cyclopropyl methyl ketone by cracking the alpha-acetyl-gamma-butyrolactone, a new type of the venture-based jet loop reactor is adopted, so that mass transfer among various reaction species in the reactor is greatly promoted, a reaction is controlled dynamically, and sufficient mass transfer and reaction are achieved between organic phase and catalyst feedstock in a reaction system, the reaction efficiency is greatly improved and occurrence of a side reaction is reduced. Combined catalyst adopted has high catalytic efficiency, high activity and high selectivity, not only reduce the reaction temperature, but also reduce other side reactions of pyrolysis at high temperature, reduce energy consumption and cost.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a synthesis method for preparing cyclopropyl methyl ketone by cracking alpha-acetyl-gamma-butyrolactone. Background technique [0002] α-acetyl-γ-butyrolactone, referred to as ABL, has a molecular formula of C6H8O3 and a molecular weight of 128.13. It is a colorless and transparent liquid. It is an important intermediate in the synthesis of vitamin B, and an intermediate in the synthesis of 3,4-disubstituted pyridine and 5-(β-hydroxyethyl)-4-methylthiazole. Its structure is as follows: [0003] [0004] In recent years, the cracking and decarboxylation method of α-acetyl-γ-butyrolactone has been developed abroad, and cyclopropyl methyl ketone can be prepared, which can be used more widely. Cyclopropyl methyl ketone is a methyl ketone with a relatively special structure. It is an important intermediate for the synthesis of new broad-spectrum antibacteria...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/59C07C49/293
CPCC07C45/59C07C2601/02C07C49/293
Inventor 张治国徐官根徐林斌黄剑程红伟
Owner JIANGSU YUXIANG CHEM
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