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Method for preparing diethoxymethane from ethanol and paraformaldehyde

A technology of diethoxymethane and paraformaldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex post-treatment, long reaction cycle, low yield, etc. Short, easy to operate control, low energy consumption effect

Inactive Publication Date: 2011-09-14
YANGZHOU LIBANG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention overcomes the defects of long reaction cycle, low yield and complex post-treatment in the traditional process

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0009] 1. Weigh raw materials:

[0010] 1. Industrial ethanol with a mass fraction of 95%, 100kg.

[0011] 2. Industrial paraformaldehyde with a mass fraction of 92%, 60kg.

[0012] 3. Industrial sulfuric acid with a mass fraction of 98%, 10kg.

[0013] 2. Equipment preparation:

[0014] A first group of distillation towers is connected to the top of the reactor with a stirring device, a storage tank is connected to the top of the group of distillation towers, and a second group of distillation towers is connected to one side of the storage tank.

[0015] 3. Preparation process:

[0016] 1. Put ethanol and paraformaldehyde in a reaction kettle with a stirring device, heat the reaction kettle under stirring conditions, and add sulfuric acid when the temperature of the mixed liquid in the reaction kettle rises to 70±2°C, and the temperature in the kettle is 80 Under the condition of ~85°C (preferably 82-85°C), keep the reaction until the end.

[0017] 2. Continue to heat th...

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PUM

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Abstract

The invention discloses a method for preparing diethoxymethane from ethanol and paraformaldehyde, which relates to a synthesis method of chemical industry. The method comprises the following steps of: stirring ethanol and paraformaldehyde in a reaction kettle, adding sulfuric acid when heating to reach 70+ / -2 DEG C, preserving heat and undergoing a reaction at the temperature of 75-85 DEG C for 0.5-1 hour; and heating and distilling by using a rectifying tower, collecting distillate with the boiling range of 70-88 DEG C under the condition that the reflux ratio is (1-3):1, standing the distillate, distilling supernate and collecting distillate serving as diethoxymethane at the temperature of 80-88 DEG C. Ethanol directly reacts with paraformaldehyde under the condition that sulfuric acid is taken as a catalyst, so that a process is simplified, and a large amount of post-treatment equipment investment can be particularly saved; the method is easy to operate and control; and compared with the prior art, the method has the advantages of higher primary transformation ratio, short reaction time, low energy consumption and product purity of up to 99.6 percent.

Description

technical field [0001] The invention relates to a synthesis method in the chemical industry, in particular to the technical field of a method for preparing diethoxymethane. Background technique [0002] Diethoxymethane (DEM), also known as formaldehyde diethyl acetal, is an excellent organic solvent and can also be used as ethoxymethylation reagent, methyleneation reagent and carbonylation reaction substrate, etc. There are many ways to synthesize DEM. In addition to the by-product of chloramphenicol, ethanol and formaldehyde solution are generally used as raw materials, inorganic acid (31% hydrochloric acid), organic acid (p-toluenesulfonic acid), solid acid (strong acid type cation) Resin) etc. as the catalyst, obtained by catalytic distillation. Since this method has a large amount of water in the reaction process, the conversion rate is low. In addition, diethoxymethane, ethanol, and water form azeotrope, which makes purification difficult and directly affects the puri...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/50
Inventor 吴洪侯玉祥
Owner YANGZHOU LIBANG CHEM
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