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Method for preparing methylal

A technology of dimethoxymethane and methanol is applied in the field of preparation of chemical raw material dimethoxymethane, which can solve the problems of complicated operation process, insufficient reaction, short contact time, etc., and achieves high equilibrium conversion rate and easy product separation. , the effect of fast response

Inactive Publication Date: 2010-01-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the entire reaction system of catalytic rectification is in a flowing state, the contact time between formaldehyde and methanol in the reaction section is too short to fully react, and formaldehyde contains a large amount of water, which prevents the reaction from proceeding.
And because this process, like the continuous reaction synthesis process, has specific requirements on temperature, pressure and catalyst, the operation process is relatively complicated
Therefore, the process also has deficiencies

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The raw materials are based on the molar ratio of paraformaldehyde and methanol 0.55:1, wherein the paraformaldehyde is CH 2 In terms of O, sulfuric acid is used as a catalyst, the amount of catalyst is 0.05g / g methanol, the organic solvent is toluene, the reaction is carried out in a batch reactor, the reaction temperature is 40 ° C, and the reaction time is 3 hours to obtain dimethoxymethane . The conversion rate of the reactant methanol is 62.2%, and the selectivity of the product dimethoxymethane is 96.7%.

Embodiment 2

[0045] The raw materials are based on the molar ratio of paraformaldehyde and methanol 0.55:1, wherein the paraformaldehyde is CH 2 In terms of O, sulfuric acid is used as a catalyst, the amount of catalyst is 0.05g / g methanol, the organic solvent is toluene, the reaction is carried out in a batch reactor, the reaction temperature is 60 ° C, and the reaction time is 2 hours to obtain dimethoxymethane . The conversion rate of the reactant methanol is 84.6%, and the selectivity of the product dimethoxymethane is 97.9%.

Embodiment 3

[0047] The raw materials are based on the molar ratio of paraformaldehyde and methanol 0.75:1, wherein the paraformaldehyde is CH 2In terms of O, sulfuric acid is used as a catalyst, the amount of catalyst is 0.05g / g methanol, the organic solvent is toluene, the reaction is carried out in a batch reactor, the reaction temperature is 60 ° C, and the reaction time is 2 hours to obtain dimethoxymethane . The conversion rate of the reactant methanol is 76.7%, and the selectivity of the product dimethoxymethane is 93.4%.

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Abstract

The invention provides a method for preparing methylal. The method comprises the following steps of: taking methanol and paraformaldehyde as raw materials and acid as a catalyst; putting the raw materials and the catalyst in an organic solvent for reaction; reacting with stirring in a mode of batch reaction to prepare methylal; and by separating the methylal, obtaining an azeotrope of methanol and methylal or high-purity methylal. The method has the advantages of high reaction speed and high conversion rate, and can be applied in the field of organic chemical engineering.

Description

technical field [0001] The invention relates to a preparation method of chemical raw material dimethoxymethane. Background technique [0002] Dimethoxymethane is mainly used to produce high-concentration formaldehyde by oxidation method, and it can also replace formaldehyde for condensation reaction, such as the reaction of diphenol or diphenylamine compounds with dimethoxymethane to form diphenol methane or diphenylamine methane compounds. Direct use of formaldehyde solution has greater advantages. It has recently been found that dimethoxymethane as an additive to methanol gasoline can significantly improve its low-temperature starting performance, and has been widely used in methanol-containing vehicle fuels. Dimethoxymethane can also be used as an environment-friendly benzene-free solvent with a purity of more than 85%. It can be widely used in medicine, ink, and paint solvents to make benzene-free banana water, adhesives for shoes, electronic equipment cleaners, air Fr...

Claims

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Application Information

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IPC IPC(8): C07C43/303C07C41/56
Inventor 许春梅张明森柯丽冯静
Owner CHINA PETROLEUM & CHEM CORP
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