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A method for purifying 2,2-dimethoxyacetaldehyde

A technology of dimethoxyacetaldehyde and reaction liquid, which is applied in the field of separation and purification of fine chemicals, can solve the problems not clearly mentioned, high energy consumption, large reflux ratio, etc., to reduce energy consumption, improve production efficiency, The effect of reducing the reflux ratio

Active Publication Date: 2017-12-22
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the method for obtaining high-purity 2,2-dimethoxyacetaldehyde is not clearly mentioned in the current patent literature, and the raw materials for the preparation of 2,2-dimethoxyacetaldehyde are mainly ethylene, glyoxal and 1 , 1,1,1-tetramethoxyethane, etc. Therefore, according to different raw materials, there are many synthetic routes for 2,2-dimethoxyacetaldehyde
Wherein taking glyoxal as raw material is a kind of synthetic technique (The Monoacetalization of Glyoxal: A Direct of 2,2-dimethoxy and Diethoxy Ethanals, Synthetic Communication, 1988, 18 (2), 1343-1348) generally adopted at home and abroad. It has the advantages of simple process and high yield, but the boiling point of the by-product is similar to that of 2,2-dimethoxyacetaldehyde, resulting in only 75% of the content of 2,2-dimethoxyacetaldehyde, and high reflux is required for purification Compared with or larger theoretical plate number, the energy consumption is extremely high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 2000g of the 2,2-dimethoxyacetaldehyde reaction solution prepared by reacting glyoxal with methanol was subjected to ordinary atmospheric distillation, and the 2,2-dimethoxyacetaldehyde reaction solution was heated to 85°C until no longer End when there is a distillate, the remaining solution 800g is used as rectification raw material, the mass percent composition of 2,2-dimethoxyacetaldehyde detected by gas chromatography is 60%, the mass percentage of 2,2-dimethoxyacetaldehyde 480g, add 600g of extractant water, mix evenly, add to the tower still of the rectifying tower, the theoretical plate number of the rectifying tower is 30, be that 90Kpa in absolute vacuum, the reaction liquid temperature of tower still begins to refine Distillation, control the reflux ratio to 0.6:1, collect the fraction before 40-50°C, continue heating to 80°C, control the reflux ratio to 10:1, collect the fraction at 50-60°C to obtain 2,2-dimethoxyacetaldehyde 326g, the gas chromatography det...

Embodiment 2

[0016] 2000g of the 2,2-dimethoxyacetaldehyde reaction solution obtained by reacting glyoxal with methanol was subjected to normal pressure distillation, and the 2,2-dimethoxyacetaldehyde reaction solution was heated to 90°C until no longer End when a fraction is distilled off, the remaining solution 720g is used as rectification raw material, the mass percent composition of 2,2-dimethoxyacetaldehyde detected by gas chromatography is 65%, the mass percentage of 2,2-dimethoxyacetaldehyde is 468g, add extractant water 600g, mix uniformly, add the tower still of rectifying tower, the theoretical plate number of rectifying tower is 30, be that 90Kpa, tower still reaction liquid temperature start refining under the condition of 60 ℃ in absolute vacuum degree Distillation, control the reflux ratio to 0.6:1, collect the fraction before 40-50°C, continue heating to 80°C, control the reflux ratio to 10:1, collect the fraction at 50-60°C to obtain 2,2-dimethoxyacetaldehyde 323g, the pur...

Embodiment 3

[0018] 2000g of the 2,2-dimethoxyacetaldehyde reaction solution prepared by reacting glyoxal with methanol was subjected to ordinary atmospheric distillation, and the 2,2-dimethoxyacetaldehyde reaction solution was heated to 85°C until no longer End when there is a distillate, the remaining solution 800g is used as rectification raw material, the mass percent composition of 2,2-dimethoxyacetaldehyde detected by gas chromatography is 60%, the mass percentage of 2,2-dimethoxyacetaldehyde is 480g, add 720g of extractant water, mix well, add the tower still of rectifying tower, the theoretical plate number of rectifying tower is 30, be that 90Kpa, tower still reaction liquid temperature start refining under the condition of 60 ℃ in absolute vacuum degree Distillation, control the reflux ratio to 0.6:1, collect the fraction before 40-50°C, continue heating to 80°C, control the reflux ratio to 10:1, collect the fraction at 50-60°C to obtain 2,2-dimethoxyacetaldehyde 335g, the gas ch...

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Abstract

The invention discloses a method for purifying 2,2-dimethoxy acetaldehyde, and belongs to the technical field of separating and purifying fine chemicals. According to the method, a 2,2-dimethoxy acetaldehyde reaction solution is used as an initial raw material and subjected to normal pressure distillation, then water is added, and extractive distillation is conducted to obtain a high-purity 2,2-dimethoxy acetaldehyde solution, wherein the purity is higher than 98%. The method has the advantages that the operation process is simple, and the purified product is high in purity.

Description

technical field [0001] The invention belongs to the technical field of separation and purification of fine chemicals, and relates to a separation and purification method for obtaining high-purity 2,2-dimethoxyacetaldehyde. Background technique [0002] 2,2-Dimethoxyacetaldehyde is a colorless, low-toxic, non-volatile aldehyde, which contains a highly reactive aldehyde group and an acetal group that is less reactive but can be easily converted into an aldehyde group , is often used in reactions such as ring closing, prolonging the parent chain structure, and introducing aldehyde groups in synthetic chemistry. As an important fine intermediate, it is widely used in the resin industry, fragrance industry, and pharmaceutical industry. [0003] However, the method for obtaining high-purity 2,2-dimethoxyacetaldehyde is not clearly mentioned in the current patent literature, and the raw materials for the preparation of 2,2-dimethoxyacetaldehyde are mainly ethylene, glyoxal and 1 ,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/198C07C45/82C07C45/83
CPCC07C45/82C07C45/83C07C47/198
Inventor 陈涛卫天琪杨翠凤林双政徐泽刚
Owner XIAN MODERN CHEM RES INST