Continuous reaction rectifying synthesizing methylene diethyl ether technology

A diethoxymethane and reactive distillation technology, which is applied in sustainable manufacturing/processing, chemical industry, climate sustainability, etc., can solve the problems of long reaction period and unsatisfactory yield, and achieves fast reaction rate and high reaction rate. The effect of short cycle and high yield

Inactive Publication Date: 2006-08-30
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] The disadvantage of the traditional process is that the reaction cycle is long and the yield is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1, continuous reaction distillation synthesis of diethoxymethane process: 37-40% formaldehyde is continuously added to the reaction at a rate of V / V68ml / min, and 36-38% of hydrochloric acid catalyst is continuously added to the reaction at a rate of V / V8.4ml / min In the kettle, 95% ethanol is added from the 5th block (feed position can be adjusted) of the rectifying column, adding V / V is 101ml / min, after reaction rectification, the higher DEM and ethanol of the distillate are obtained at the top of the tower and Water, with glycerol as the extraction agent, is extracted through a liquid-liquid extraction tower, and the DEM content at the top of the extraction tower can reach more than 99.6%. The extractant and ethanol-water mixture are recovered and recycled through the regeneration tower. The ethanol and water at the top of the regenerated tower can be further recycled and processed. The temperature of the kettle and top of the reactive distillation unit is ...

Embodiment 2

[0021] Embodiment 2 is substantially the same as Example 1, but the catalyst is changed to sulfuric acid, and the extractant is changed to diethanolamine.

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PUM

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Abstract

A process for synthesizing diethoxymethane (DEM) by continuous reactive rectification includes such steps as continuously adding formaldehyde and acid catalyst to reactor, adding ethanol from reactifying column, respectively controlling the internal temp and the top temp of reactive rectifying tower to 80 deg.C and 65 deg.C, reactive reactifying to obtain distilate from tower, extracting by propanetriol or diethanolamine in liquid-liquid extracting tower to obtain DEM from tower top, and regenerating extractant, ethanol and water by regenerating tower for cyclic use. Its advantages are high speed and high output rate (more than 76%).

Description

technical field [0001] The invention relates to a process for synthesizing diethoxymethane through continuous reactive distillation. Background technique [0002] The traditional diethoxymethane (abbreviated as DEM) synthesis process adopts the following five methods: the dichloromethane method is the earliest method for synthesizing DEM, because the technology is backward and the yield is low, so this method has no industrialization; the dimethyl sulfoxide method , because dimethyl sulfoxide is unstable to acid, and heating will generate formaldehyde, so there is no industrialization; the calcium chloride method, the reaction yield can reach 86.5%, but due to the long reaction time, post-processing is inconvenient. So there is no industrialization; the acid catalyzed batch method has simple reaction operation and high yield (95%), but the reaction energy consumption is high and the production cycle is long; the chloramphenicol by-product method is the main way to produce DE...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/30C07C43/04C07C41/56
CPCY02P20/10
Inventor 顾正桂职慧珍
Owner NANJING NORMAL UNIVERSITY
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