Method for preparing methylal by combining reaction rectification and extraction

A technology of dimethoxymethane and reactive distillation, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long cycle, many procedures, high energy consumption, etc., and achieve purity and yield High, simple process effect

Inactive Publication Date: 2007-12-26
NANJING NORMAL UNIVERSITY
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Problems solved by technology

In short, the preparation of high-purity DMM requires many procedures, long cycle and high energy consumption.

Method used

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  • Method for preparing methylal by combining reaction rectification and extraction

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Embodiment 1

[0015] Embodiment 1, with reference to Fig. 1: preparation raw material methanol, formaldehyde solution (containing formaldehyde 37%~40%) mass ratio is 0.9: 1; The mass ratio of extraction agent ethylene glycol and raw material is 1.2: 1; Catalyst p-toluenesulfonic acid mass ratio 5% of the raw material. Raw materials (methanol, formaldehyde) and reagents (ethylene glycol and p-toluenesulfonic acid) are fed into the tower at a mass flow rate of 15mL / min, and the bottom of the tower is discharged at the same flow rate into the solvent recovery tower. The DMM content in the obtained product reaches more than 99.5%, and the yield reaches more than 85%. The specific operating conditions are shown in Table 1, and the separation results are shown in Table 2.

[0016] The steps are: the raw material ① (methanol and formaldehyde solution) enters the extraction reaction rectification tower through a metering pump through the feed port, and the feed port of the raw material is set at t...

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Abstract

This invention relates to a method for preparing dimethoxymethane by combination of rectification and extraction. The method comprises: adding raw materials, extractant and catalyst at a certain ratio into a rectification column from different parts at a weight flow rate of 15 mL / min, reacting to obtain high-purity dimethoxymethane at the overhead and mixed liquids at the bottom, sending the mixed liquids to a solvent recovery column, recovering the extracting solvent, and recycling. The weight ratio of methanol to 37-40% formaldehyde solution (raw materials) is 0.9:1. The weight ratio of extractant ethylene glycol to raw materials is 1.2:1. The addition amount of catalyst is 5% of raw materials. The method adopts only one column to finish the preparation of dimethoxymethane. The concentration of dimethoxymethane is up to 99.5%, and the yield is up to 85% or higher. The method has such advantages as simple process, high product purity and yield, and low energy consumption (saved by 50% compared with combined method of reaction rectification and extraction rectification).

Description

technical field [0001] The invention relates to a method for preparing dimethoxymethane by combining reactive distillation and extraction. The synthesis and extraction and purification of dimethoxymethane are completed in the same reactive distillation tower. Background technique [0002] Dimethoxymethane (DMM) is an important solvent and oxygen-containing additive. At this stage, the research on the synthesis of DMM mainly focuses on: using solid acid as a catalyst, using a certain proportion of methanol and formaldehyde as raw materials, and synthesizing it by reactive distillation. Among them, the reactive distillation method is divided into batch operation and continuous operation. The batch operation is that the raw materials and the catalyst are added to the reactor at one time, the reaction cycle is long, and the concentration of the obtained methylal is not high. The continuous operation is to add solid acid catalyst in many places on the reactive distillation colu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/303C07C41/50
Inventor 顾正桂管小伟
Owner NANJING NORMAL UNIVERSITY
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