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Continuous catalysis and rectification technology for synthesizing diethoxymethane

A diethoxymethane, catalytic distillation technology, applied in the chemical industry, sustainable manufacturing/processing, organic chemistry, etc., can solve the problems of low product purity, long production cycle, complicated operation, etc., to achieve high product purity, The effect of long production cycle and complicated operation

Active Publication Date: 2011-10-05
石家庄一科发化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional synthesis methods of diethoxymethane mainly include: dichloromethane method, dimethyl sulfoxide method, calcium chloride method, acid catalyzed batch method, chloramphenicol by-product method, but these production methods have high energy consumption and short production cycle Long, complicated operation, and the product has low purity and is not easy to separate, so the traditional production method of diethoxymethane is not suitable for continuous industrial production

Method used

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  • Continuous catalysis and rectification technology for synthesizing diethoxymethane
  • Continuous catalysis and rectification technology for synthesizing diethoxymethane

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Effect test

Embodiment 1

[0039] The continuous distillation synthesis process flow chart of diethoxymethane is as follows figure 1 shown. The catalytic reaction rectification tower is divided into the first-stage catalytic reaction rectification tower T101 and the second-stage catalytic reaction rectification tower T102. The reaction sections of the two-stage catalytic reaction rectification towers are filled with solid acid catalysts, and 30% formaldehyde enters through pipeline 1. To the top of T101, flow is 2.12g / min, and ethanol enters the bottom of T102 through pipeline 6, and flow is 2.00g / min, and the mol ratio of ethanol and formaldehyde is 2.051, and T101 overhead extract (diethoxymethane , unreacted ethanol and water) condenses through condenser 4, enters reflux tank, part returns T101 tower through pipeline 3, as the reflux of this reaction, reflux flow is 17ml / min, part is discharged as product through pipeline 10, and it is composed of : 2.835% of water, 1.490% of ethanol, 95.675% of die...

Embodiment 2

[0042] The continuous distillation synthesis process flow chart of diethoxymethane is as follows figure 1shown. The catalytic reaction rectification tower is divided into the first-stage catalytic reaction rectification tower T101 and the second-stage catalytic reaction rectification tower T102. The reaction sections of the two-stage catalytic reaction rectification towers are filled with solid acid catalysts, and 30% formaldehyde enters through pipeline 1. To the top of T101, flow is 2.12g / min, and ethanol enters the bottom of T102 through pipeline 6, and flow is 2.14g / min, and the mol ratio of ethanol and formaldehyde is 2.194, and T101 overhead extract (diethoxymethane , unreacted ethanol and water) are condensed through the condenser 4, enter the reflux tank, part returns to the T101 tower through the pipeline 3, and part is discharged as the product through the pipeline 10, and the discharge is composed of: water 2.670%, ethanol 7.236%, diethoxy Methyl methane 90.094%, f...

Embodiment 3

[0045] The continuous distillation synthesis process flow chart of diethoxymethane is as follows figure 1 shown. The catalytic reaction rectification tower is divided into the first-stage catalytic reaction rectification tower T101 and the second-stage catalytic reaction rectification tower T102. The reaction sections of the two-stage catalytic reaction rectification towers are filled with solid acid catalysts, and 30% formaldehyde enters through pipeline 1. To the top of T101, flow is 2.12g / min, and ethanol enters the bottom of T102 through pipeline 6, and flow is 2.00g / min, and the mol ratio of ethanol and formaldehyde is 2.051, and T101 overhead extract (diethoxymethane , unreacted ethanol and water) condenses through condenser 4, enters reflux tank, part returns T101 tower through pipeline 3, as the reflux of this reaction, reflux flow is 17ml / min, part is discharged as product through pipeline 10, and it is composed of : 2.835% of water, 1.490% of ethanol, 95.675% of die...

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Abstract

The invention discloses a continuous catalysis and rectification technology for synthesizing diethoxymethane. According to the invention, formaldehyde and ethanol are adopted as raw materials, and a two-stage linkage catalysis rectifying tower composed of a first-stage reaction rectifying tower and a second-stage reaction rectifying tower is employed. Solid acid catalysts are loaded in both the first-stage and the second-stage reaction rectifying towers. The technology comprises the steps that: (A) formaldehyde is delivered to the first-stage reaction rectifying tower, while ethanol is delivered to the second-stage reaction rectifying tower; (B) formaldehyde discharged from the bottom of the first-stage reaction rectifying tower is delivered to the second-stage reaction rectifying tower, where formaldehyde is subject to a reaction with ethanol; and waste water is discharged from the bottom of the second-stage reaction rectifying tower; (C) material obtained from the top of the second-stage reaction rectifying tower is delivered to the first-stage reaction rectifying tower, where the obtained material is subject to a reaction with formaldehyde; and diethoxymethane, which is a target product, is obtained from the top of the first-stage reaction rectifying tower; (D) the steps from (A) to (C) are repeatedly circulated. The technology has advantages of short processing period, high selectivity, high yield, high product purity, and simple operation. Therefore, the technology is suitable for continuous industrial production.

Description

technical field [0001] The invention relates to a continuous catalytic rectification synthesis process of diethoxymethane. Background technique [0002] Diethoxymethane is an industrial environment-friendly solvent with excellent performance and an important pharmaceutical intermediate, which is widely used in organic synthesis, coating ink and fuel additive. It is used as a reaction solvent in organic synthesis, such as alkylation and acylation reactions; it is used as a solvent for neoprene adhesives, making the adhesives more stable in storage, good in brushing performance, and high in peel strength; it is used as the equivalent of formaldehyde , can be used as a substitute for formaldehyde, making the reaction safer, and easy to handle without water. [0003] The traditional synthesis methods of diethoxymethane mainly include: dichloromethane method, dimethyl sulfoxide method, calcium chloride method, acid catalyzed batch method, chloramphenicol by-product method, but t...

Claims

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Application Information

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IPC IPC(8): C07C43/30C07C41/50C07C41/58
CPCY02P20/10
Inventor 王纲司君华刘新泰黄胜飘
Owner 石家庄一科发化工科技有限公司
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