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Method and device for synthesizing alpha-chloro-alpha-acetyl-gamma-butyrolactone for co-production of methyl formate

A technology of methyl formate and acetyl, which is applied in the field of synthesizing α-chloro-α-acetyl-γ-butyrolactone to co-produce methyl formate, which can solve the difficulty in the treatment of carbon dioxide and chlorine tail gas and the inability to synthesize hydrochloric acid Utilization, low utilization rate of chlorine gas, etc., to avoid local overheating, improve reaction safety, and avoid excessive chlorine gas concentration

Active Publication Date: 2019-03-01
江苏兄弟维生素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Then, in the existing synthesis process, a large amount of carbon dioxide will be generated during the reaction process, which will cause the raw material chlorine to be carried, resulting in waste of raw materials, low utilization rate of chlorine gas, and greater safety risks
At the same time, it is difficult to treat the obtained carbon dioxide and chlorine tail gas
Moreover, in the reaction process, the obtained by-product hydrochloric acid cannot be comprehensively utilized, and a large amount of sodium bicarbonate needs to be consumed, resulting in waste of raw and auxiliary materials

Method used

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  • Method and device for synthesizing alpha-chloro-alpha-acetyl-gamma-butyrolactone for co-production of methyl formate
  • Method and device for synthesizing alpha-chloro-alpha-acetyl-gamma-butyrolactone for co-production of methyl formate
  • Method and device for synthesizing alpha-chloro-alpha-acetyl-gamma-butyrolactone for co-production of methyl formate

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Experimental program
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Embodiment 1

[0065] The method for synthesizing α-chloro-α-acetyl-γ-butyrolactone of the present embodiment to co-produce methyl formate comprises the following steps:

[0066] (1) Get 96g of α-acetyl-γ-butyrolactone, mass fraction of 45% sodium formate aqueous solution 180g, 54g of chlorine continuously into the micropipe reactor, react at 15-16°C, control the reaction of the reactants in the micropipe The residence time in the container is 20-30s. After the reaction, the obtained reaction solution contains the main product α-chloro-α-acetyl-γ-butyrolactone, water, formic acid and sodium chloride;

[0067] (2) The reaction solution after reaction is sent to the flash evaporator from the discharge end of the micropipe reactor, and is directly flashed under the negative pressure condition of -0.05~-0.1MPa, which can separate the slight excess chlorine gas, and after continuous chlorine discharge Obtain the reaction solution 330g after chlorine discharge;

[0068] (3) The reaction solution ...

Embodiment 2

[0072] The method for synthesizing α-chloro-α-acetyl-γ-butyrolactone of the present embodiment to co-produce methyl formate comprises the following steps:

[0073] (1) Get 96g of α-acetyl-γ-butyrolactone, mass fraction of 35% sodium formate aqueous solution 231g, 54g of chlorine continuously into the micropipe reactor, react at 15-16°C, control the reaction of the reactant in the micropipe The residence time in the container is 20-30s. After the reaction, the obtained reaction solution contains the main product α-chloro-α-acetyl-γ-butyrolactone, water, formic acid and sodium chloride;

[0074] (2) After the reaction, the reaction solution is sent to the flash evaporator from the discharge end of the micropipe reactor, and is directly flashed under the negative pressure condition of -0.05Pa~-0.1MPa, which can separate the slight excess chlorine gas and discharge chlorine continuously After obtaining the reaction solution after chlorine discharge;

[0075] (3) The reaction solu...

Embodiment 3

[0079] The method for synthesizing α-chloro-α-acetyl-γ-butyrolactone of the present embodiment to co-produce methyl formate comprises the following steps:

[0080] (1) Get 96g of α-acetyl-γ-butyrolactone, mass fraction of 30% sodium formate aqueous solution 270g, 54g of chlorine continuously into the micropipe reactor, react at 15-16°C, control the reaction of the reactant in the micropipe The residence time in the container is 20-30s. After the reaction, the obtained reaction solution contains the main product α-chloro-α-acetyl-γ-butyrolactone, water, formic acid and sodium chloride;

[0081] (2) The reaction solution after reaction is sent to the flash evaporator from the discharge end of the micropipe reactor, and is directly flashed under the negative pressure condition of -0.05~-0.1MPa, which can separate the slight excess chlorine gas, and after continuous chlorine discharge Obtain the reaction solution after chlorine discharge;

[0082] (3) The reaction solution after th...

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Abstract

The invention relates to the technical field of preparation of chemical products, in particular to a method and device for synthesizing alpha-chloro-alpha-acetyl-gamma-butyrolactone for co-productionof methyl formate. The method for synthesizing the alpha-chloro-alpha-acetyl-gamma-butyrolactone for the co-production of the methyl formate comprises the following steps of mixing alpha-acetyl-gamma-butyrolactone and a sodium formate aqueous solution, introducing chlorine gas for reaction and layering a reaction solution, wherein the lower layer substance is alpha-chloro-alpha-acetyl-gamma-butyrolactone, and making the upper layer substance to have esterification reaction with methanol to obtain the methyl formate. According to the method, the generation of gas like carbon dioxide is avoidedin the synthesis process, and the utilization rate of chlorine gas can be effectively improved. At the same time, a by-product can continuously react with methanol to produce the methyl formate afterthe certain reaction, and the by-product produced in the production process is fully utilized to meet the process demand, the production cost is greatly improved, and the environmental protection property is improved.

Description

technical field [0001] The invention relates to the technical field of preparation of chemical products, in particular to a method and a device for synthesizing α-chloro-α-acetyl-γ-butyrolactone and coproducing methyl formate. Background technique [0002] The synthesis of α-chloro-α-acetyl-γ-butyrolactone is one of the important steps in the synthesis of vitamin B1. In the prior art, the synthesis of α-chloro-α-acetyl-γ-butyrolactone mostly adopts batch reaction, and α-acetyl-γ-butyrolactone, water, sodium bicarbonate are mixed under stirring conditions Under temperature control, chlorine gas was introduced to carry out the reaction. [0003] Then, in the existing synthesis process, a large amount of carbon dioxide will be generated during the reaction process, which will cause the raw material chlorine to be carried, resulting in waste of raw materials, low utilization rate of chlorine gas, and greater safety risks. At the same time, it is difficult to treat the obtained...

Claims

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Application Information

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IPC IPC(8): C07D307/33C07C67/08C07C69/06
CPCC07C51/02C07C67/08C07D307/33C07C69/06C07C53/02
Inventor 陈英明徐晓海李褦成严建斌
Owner 江苏兄弟维生素有限公司
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