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Alpha-chloro-acetyl-gamma-butyrolactone continuous flow microchannel reaction generation process

A technology of channel reaction and generation process, applied in chemical/physical/physical chemical reactors, organic chemistry, chemical/physical/physical chemical processes, etc., can solve problems such as long reaction time, and achieve product purity and quality improvement and stability production, avoiding overused effects

Pending Publication Date: 2022-05-06
PANASIA OLAUGHLIN BIO TECH WUHAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction time of this process is long, generally 2-6 hours, and the crude product contains more polychlorinated substances, the purity of the crude product is generally 85% to 90%, and the yield after rectification is about 85%.

Method used

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  • Alpha-chloro-acetyl-gamma-butyrolactone continuous flow microchannel reaction generation process
  • Alpha-chloro-acetyl-gamma-butyrolactone continuous flow microchannel reaction generation process

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Feed the raw material α-acetyl-γ-butyrolactone at 100g / h, chlorine gas 55.3g / h, (α-acetyl-γ-butyrolactone: chlorine gas=1:1) into the microchannel reactor at the same time , react at 20°C, 0.5Mpa, and a residence time of 90 seconds. After collecting the reaction liquid at the outlet, adjust the pH to 7-8 with saturated sodium bicarbonate solution. The lower water layer was separated, and the organic layer entered a rectification under vacuum tower with an operating pressure of 2 mmHg to obtain the product α-chloro-acetyl-γ-butyrolactone with a purity of 99.3% (gas chromatography analysis) and a total yield of 95.4%.

Embodiment 2

[0033] Feed the raw material α-acetyl-γ-butyrolactone at 100g / h, chlorine gas 55.3g / h, (α-acetyl-γ-butyrolactone: chlorine gas=1:1) into the microchannel reactor at the same time , react at 30°C, 0.5Mpa, and a residence time of 75 seconds. After collecting the reaction liquid at the outlet, adjust the pH to 7-8 with saturated sodium bicarbonate solution. The lower water layer was separated, and the organic layer entered a rectification under vacuum tower with an operating pressure of 2 mmHg to obtain the product α-chloro-acetyl-γ-butyrolactone with a purity of 99.1% (gas chromatography analysis) and a total yield of 94.2%.

Embodiment 3

[0035] Feed the raw material α-acetyl-γ-butyrolactone at 100g / h, chlorine gas 55.3g / h, (α-acetyl-γ-butyrolactone: chlorine gas=1:1) into the microchannel reactor at the same time , react at 20°C, 0.5Mpa, and a residence time of 40 seconds. After collecting the reaction liquid at the outlet, adjust the pH to 7-8 with 10% sodium hydroxide solution. The lower water layer was separated, and the organic layer entered a rectification under vacuum tower with an operating pressure of 2 mmHg to obtain the product α-chloro-acetyl-γ-butyrolactone with a purity of 99.1% (gas chromatography analysis) and a total yield of 93.7%.

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Abstract

The invention discloses an alpha-chloro-acetyl-gamma-butyrolactone continuous flow microchannel reaction generation process which specifically comprises the following steps: S1, simultaneously introducing raw materials alpha-acetyl-gamma-butyrolactone and chlorine into a microchannel reactor by using a pump, the method comprises the following steps: S1, carrying out a continuous condensation reaction in a microchannel reactor to generate an alpha-chloro-acetyl-gamma-butyrolactone crude product, and S3, neutralizing with an alkaline solution, and allowing an organic layer to enter a reduced pressure rectifying tower. According to the alpha-chloro-acetyl-gamma-butyrolactone continuous flow micro-channel reaction generation process, a process technology and reaction equipment which take a continuous flow high-flux micro-channel reaction system as a core are applied to the reaction of alpha-acetyl-gamma-butyrolactone and chlorine, so that the selectivity is improved, continuous, safe, efficient and stable production is realized, and the production cost is reduced. The purity and quality of the product are remarkably improved, and the danger in the using process of the reaction materials is greatly reduced through the continuous flow high-flux micro-channel technology.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to an alpha-chloro-acetyl-gamma-butyrolactone continuous flow microchannel reaction generation process. Background technique [0002] Name: α-Chloro-acetyl-γ-butyrolactone [0003] Molecular formula: C6H7ClO3 [0004] Appearance: colorless liquid [0005] Molecular weight: 157.26 [0006] CAS number: 2986-00-7 [0007] Density: 1.33g / cm 3 [0008] Boiling point: 306.1°C, 760mmHg [0009] Refraction point: 1.479 [0010] Uses: α-Chloro-acetyl-γ-butyrolactone is the main raw material for the preparation of vitamin B1 and chlorophyll compounds. It can also be used in the pharmaceutical industry to manufacture anti-angina drugs such as protracted heart pain. It is used in the flavor industry to prepare soybeans with Fragrant and meaty aroma raw material thiothiazole. At present, the demand for α-chloro-acetyl-γ-butyrolactone in domestic and foreign markets is increas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01J19/00
CPCC07D307/33B01J19/0093
Inventor 朱小力谭亚菲
Owner PANASIA OLAUGHLIN BIO TECH WUHAN CO LTD
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