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Method for preparing acetal by using glyoxal

A technology of glyoxal and acetal, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as energy loss and equipment cost increase, failure to meet energy saving and emission reduction, and complex reaction operations, etc., to achieve The effect of improving efficiency, increasing yield and reducing production cost

Inactive Publication Date: 2010-03-24
上海华谊(集团)上硫化工有限公司
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Problems solved by technology

[0007] In the above method, physical methods are used to remove the water in the reaction system, which leads to the increase of energy loss and equipment cost, and the reaction operation is relatively complicated, which does not meet the requirements of energy saving and emission reduction

Method used

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  • Method for preparing acetal by using glyoxal

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Effect test

Embodiment 1

[0020] Under the reduced pressure condition of 0.05-0.09MPa, 58g of 40 mass% glyoxal aqueous solution was concentrated, and the concentration temperature was 60-80°C, and the obtained 33.1g of 70 mass% glyoxal aqueous solution, 256g of methanol, 48g of methyl formate and 5.0g of 98 mass % sulfuric acid together and heated to reflux for 24 hours at a reflux temperature of 80°C. Wherein the raw material composition is methanol: methyl formate: glyoxal (molar ratio)=20:2:1. The product was analyzed by gas chromatography, and the crude yields of monoacetal and diacetal based on the glyoxal used were 55.93% and 24.86%.

Embodiment 2

[0022] Under the reduced pressure condition of 0.05~0.09MPa, 58g of 40 mass% glyoxal aqueous solution was concentrated, and the concentration temperature was 60~80°C, and the obtained 33.1g of 70 mass% glyoxal aqueous solution, 256g of formic acid, 240g of methyl formate and 5.0g of 98 mass % sulfuric acid together and heated to reflux for 20 hours at a reflux temperature of 90°C. Wherein the raw material composition is methanol:methyl formate:glyoxal (molar ratio)=20:10:1. The product was analyzed by gas chromatography, and the crude yields of monoacetal and diacetal based on the glyoxal used were 60.78% and 28.75%.

Embodiment 3

[0026] Under the condition of reduced pressure of 0.05-0.09MPa, 58g of 40 mass% glyoxal aqueous solution was concentrated, and the concentration temperature was 60-80°C. The obtained 33.1g of 70 mass% glyoxal aqueous solution, 192g of methanol, 48g of methyl formate and 10.9 g of methanesulfonate The acid was heated to reflux together for 24 hours, and the reflux temperature was 80°C. Wherein the raw material composition is methanol:methyl formate:glyoxal (molar ratio)=15:2:1. The product was analyzed by gas chromatography, and the crude yields of monoacetal and diacetal based on the glyoxal used were 45.55% and 25.76%.

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Abstract

The invention relates to a method for preparing acetal by using glyoxal, which is characterized in that glyoxal water solution and alkyl alcohol are taken as raw materials; meanwhile, ester corresponding to the alkyl alcohol is added into the raw materials, and the mixture is continuously stirred under the condition that acid catalyst exists for liquid phase reaction; the heating backflow time is20-30h, the backflow reaction temperature is 70-90 DEG C, the backflow reaction pressure is normal pressure, and the products of monoacetal and diacetal of the glyoxal can be obtained; and the molar ratio between the alkyl alcohol and the glyoxal is 5-20:1, and the molar ratio between the ester corresponding to the alkyl alcohol and the glyoxal is 2-10:1. The method improves the efficiency for preparing the monoacetal and the diacetal by condensation reaction between the glyoxal and the alkyl alcohol, saves the energy and reduces the production cost.

Description

Technical field: [0001] The invention relates to a method for preparing acetal from glyoxal, in particular to a method for preparing glyoxal acetal products from glyoxal, alcohol and ester as raw materials. Background technique: [0002] Glyoxal acetal product is a kind of important organic synthesis intermediate, and its usual preparation method is to use glyoxal and monohydric alcohol (R-OH) to prepare glyoxal acetal product under the effect of acid catalyst, but reaction It is very complicated. In addition to the formation of monoacetal and diacetal, the reaction product also has many oligomers and cyclic by-products. The acetal reaction is a reversible reaction, water is one of the reaction products, and glyoxal itself is also an aqueous solution, so in order to complete the reaction, water in the reaction system is generally removed to improve the reaction efficiency. The main chemical reaction equation is as follows : [0003] [0004] US2360959 describes a proces...

Claims

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Application Information

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IPC IPC(8): C07C43/303C07C41/56
Inventor 李楠季云娣周月红郑碧照曹亮
Owner 上海华谊(集团)上硫化工有限公司
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