Continuous synthesis process of alpha-chloro-alpha-acetyl-gamma-butyrolactone

A synthesis process and acetyl technology, applied in the direction of organic chemistry, etc., can solve the problems of low utilization rate of chlorine gas, uneven distribution of chlorine gas, over temperature, etc., and achieve the effect of improving utilization rate of chlorine gas, avoiding excessive side reactions and continuous production.

Active Publication Date: 2013-11-13
江苏兄弟维生素有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The chlorination reaction process of α-acetyl-γ-butyrolactone is very mature, but it has the following disadvantages: the reaction time for chlorine passage is long, generally more than 10 hours; due to the small heat exchange area of ​​the reactor, the requirements for refrigerant Higher, otherwise the reaction temperature is difficult to be effectively controlled, and there may be overheating locally; the large cross-sectional area of ​​the reactor makes the distribution of

Method used

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  • Continuous synthesis process of alpha-chloro-alpha-acetyl-gamma-butyrolactone

Examples

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Effect test

Embodiment 1

[0021] Add 100g of α-acetyl-γ-butyrolactone, 280g of water, and 65g of sodium bicarbonate into a 500ml round-bottomed flask, start stirring and mix thoroughly, pour the premixed liquid into the constant pressure premixed liquid addition funnel 1, and use a laminated glass Condenser (with an overflow opening at a moderate position) is used as reactor 5, and the bottom of reactor 5 is connected to the chlorine gas inlet, and the outlet of said premixed solution dropping funnel 1 is extended into the bottom of said reactor 5 after dripping flowmeter 3, After passing through the material distribution pipe 4, it enters into the reaction kettle 5, chlorine gas enters the reaction kettle 5 through the chlorine gas distribution head 9 after being metered through the chlorine gas inlet pipe 8, and the overflow liquid in the reaction kettle 5 enters through the discharge pipe 10. The stratifier 11 performs stratification, the upper water layer is extracted through the water layer pipe 13...

Embodiment 2

[0024] Add 280g of α-acetyl-γ-butyrolactone, 650g of water, and 185g of sodium bicarbonate into a 1000ml round bottom flask, start stirring and mix thoroughly, pour the premixed liquid into the constant pressure premixed liquid addition funnel 1, and use a laminated glass Condenser (with an overflow opening at a moderate position) is used as reactor 5, and the bottom of reactor 5 is connected to the chlorine gas inlet, and the outlet of said premixed solution dropping funnel 1 is extended into the bottom of said reactor 5 after dripping flowmeter 3, After passing through the material distribution pipe 4, it enters into the reaction kettle 5, chlorine gas enters the reaction kettle 5 through the chlorine gas distribution head 9 after being metered through the chlorine gas inlet pipe 8, and the overflow liquid in the reaction kettle 5 enters through the discharge pipe 10. The stratifier 11 performs stratification, the upper water layer is extracted through the water layer pipe 13...

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Abstract

The invention relates to the technical field of chemical product preparation, and especially relates to a continuous synthesis process of alpha-chloro-alpha-acetyl-gamma-butyrolactone. The method comprises the steps that: alpha-acetyl-gamma-butyrolactone, water, and sodium bicarbonate are added into a same mixer; stirring is started, such that the materials are sufficiently mixed, and a premix liquid is prepared; the premix liquid is added into a constant-pressure premix liquid dropping funnel; through dropping flow meter metering, the liquid enters the bottom of a reaction kettle; chlorine gas is metered, and enters the bottom of the reaction kettle; a reaction temperature is controlled, such that a chlorination reaction is carried out; overflow liquid in the reaction kettle enters a stratification device through a discharge pipe, and stratification is carried out; upper-layer water layer is recovered through a water layer pipe, and a lower-layer finished product is recovered through a finished product pipe. According to the alpha-chloro-alpha-acetyl-gamma-butyrolactone continuous synthesis process, continuous production is realized, chlorine gas utilization rate is improved, product yield is improved, reaction rate is improved, and production capacity is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical products, in particular to a continuous synthesis process of α-chloro-α-acetyl-γ-butyrolactone. Background technique [0002] α-Chloro-α-acetyl-γ-butyrolactone is one of the important steps in the organic synthesis of vitamin B1. At present, all domestic companies or enterprises adopt batch-type chlorination reaction: add a certain amount of α-acetyl-γ-butyrolactone, water, sodium bicarbonate, control the temperature not to exceed 20°C under stirring, and feed measured chlorine gas into the bottom of the kettle. After the reaction is completed, let the layers stand for more than 10 hours, and then proceed Separation, the supernatant is α-chloro-α-acetyl-γ-butyrolactone. The chlorination reaction process of α-acetyl-γ-butyrolactone is very mature, but it has the following disadvantages: the reaction time for chlorine passage is long, generally more than 10 hours; due to the small h...

Claims

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Application Information

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IPC IPC(8): C07D307/33
Inventor 李健平李来成陈英明
Owner 江苏兄弟维生素有限公司
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