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Method for preparing butyraldehyde glycol acetal

A technology of butyraldehyde ethylene glycol and ethylene glycol, which is applied in the field of preparation of butyraldehyde ethylene glycol acetal, can solve the problems of low yield, many side reactions, dark product color and the like, and achieves the effects of high yield and simple process

Inactive Publication Date: 2011-06-01
尹华芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has many side reactions, low yield, darker product color, serious equipment corrosion, complex post-treatment, and a large amount of waste acid is produced at the same time, causing environmental pollution and other shortcomings.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The catalyst is solid superacid SO 4 - / Fe 3 o 4 -Al 2 o 3 -ZnO;

[0015] Dissolve 20 g of ferric nitrate, 15 g of aluminum chloride, and 10 g of zinc chloride in 200 g of absolute ethanol, stir for 2 hours, add 50 ml of glacial acetic acid dropwise at room temperature and under stirring conditions, and continue stirring after adding to obtain a nearly transparent solution. Add 50ml of ammonium persulfate solution under strong stirring, continue to stir, and place the mixed solution in a 70°C water bath for sol-gel conversion. After the gel is aged, put it in a drying oven at 70°C for 16 hours to obtain a xerogel. After crushing, roast at 300°C for 6 hours to obtain the desired solid acid catalyst sample.

[0016] Preparation of Butyraldehyde Glycol Acetal

[0017] In a three-neck flask equipped with a water separator, a reflux condenser, and a thermometer, 72 g of butyraldehyde, 93 g of ethylene glycol, 3.6 g of catalyst, and 72 g of water-carrying agent cyclohe...

Embodiment 2

[0019] The catalyst is solid superacid SO 4 - / Fe 3 o 4 -Al 2 o 3 -ZnO

[0020] Dissolve 20 g of ferric nitrate, 10 g of aluminum chloride, and 5 g of zinc chloride in 200 g of absolute ethanol, stir for 1 hour, add 60 ml of glacial acetic acid dropwise at room temperature and under stirring conditions, and continue stirring after the addition to obtain a nearly transparent solution. Add 50ml of ammonium persulfate solution under strong stirring, continue to stir, and place the mixed solution in a 70°C water bath for sol-gel conversion. After the gel is aged, put it in a drying oven at 90°C for 24 hours to obtain a xerogel. After crushing, roast at 600°C for 2 hours to obtain the desired solid acid catalyst sample.

[0021] Preparation of Butyraldehyde Glycol Acetal

[0022] In a three-necked flask equipped with a water separator, a reflux condenser, and a thermometer, 72 g of butyraldehyde, 124 g of ethylene glycol, 14.4 g of catalyst, and 216 g of water-carrying cyclo...

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Abstract

The invention relates to a method for preparing butyraldehyde glycol acetal, which comprises: adding butyraldehyde, glycol, a catalyst and a cyclohexane water-carrying agent in turn into a neck flask in which a water segregator, a reflux condenser tube and a temperature meter are arranged; heating, refluxing and stirring till no water is separated out; and after the reaction is finished and the reactants cool down to room temperature, filtering to remove a catalyst; separating a coarse product, washing the coarse product with water and saturated salt solution in turn, and drying the coarse product with anhydrous magnesium sulfate; distilling at normal pressure, collecting a fraction at 130 to 134 DEG C to obtain colorless transparent liquid which is butyraldehyde glycol acetal with a fruit flavor. The catalyst is solid super strong acid SO4- / Fe3O4-Al2O3-ZnO. The method has the characteristics of high yield, easy operation and the like.

Description

technical field [0001] The invention relates to a preparation method of butyraldehyde glycol acetal. Background technique [0002] Butyraldehyde glycol acetal is a stable colorless liquid with fresh fruity aroma and is often used as an intermediate in organic synthesis. Widely used in the production of food, wine, beverages and cosmetics, it is a new product researched and developed in the past 20 years. [0003] The traditional synthesis method of butyraldehyde glycol aldehyde fragrances is obtained by direct condensation of aldehydes and alcohols under the catalysis of inorganic acids (such as concentrated sulfuric acid, etc.) or organic acids (such as p-toluenesulfonic acid, etc.). However, this method has many side reactions, low yield, dark product color, serious equipment corrosion, complex post-treatment, and produces a large amount of waste acid, causing environmental pollution and other shortcomings. [0004] Therefore, scientific research workers are trying to fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/12B01J27/053
Inventor 尹华芳
Owner 尹华芳
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