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A kind of synthetic method of α-acetyl-γ-butyrolactone cracking to prepare cyclopropyl methyl ketone

A technology of cyclopropyl methyl ketone and synthesis method, which is applied in the direction of heterocyclic compound preparation and organic chemistry, can solve the problems of insufficient catalyst activity, high reaction temperature, low reaction yield, etc., achieve excellent catalytic cracking effect, reduce The effect of pyrolysis reaction temperature and high specific surface area

Active Publication Date: 2021-11-12
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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  • A kind of synthetic method of α-acetyl-γ-butyrolactone cracking to prepare cyclopropyl methyl ketone
  • A kind of synthetic method of α-acetyl-γ-butyrolactone cracking to prepare cyclopropyl methyl ketone
  • A kind of synthetic method of α-acetyl-γ-butyrolactone cracking to prepare cyclopropyl methyl ketone

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 synthesis method for preparing cyclopropyl methyl ketone by cracking α-acetyl-γ-butyrolactone, which comprises adding α-acetyl-γ-butyrolactone into a jet loop reactor based on Venturi effect Lactone raw materials, deoxygenation, filling inert gas replacement protection, turning on the external circulation pump for high-speed jet mixing and other steps, the invention adopts a new jet loop reactor based on the Venturi effect, which greatly promotes the process of each reactor in the reactor The mass transfer between reactant species enables the reaction to be under kinetic control, and sufficient mass transfer and reaction can be achieved between the organic phase and the catalyst raw material in the reaction system, which greatly improves the reaction efficiency and reduces the occurrence of side reactions. The combined catalyst adopted in the present application has high catalytic efficiency, high activity and high selectivity, which not only reduces the reaction temperature, but also reduces other side reactions of cracking at high temperature, reduces energy consumption and costs at the same time.

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 Patents(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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