Device for recycling industrial grade diethoxymethane and method for recycling industrial grade diethoxymethane

A diethoxymethane and chemical industry technology, applied in the field of diethoxymethane preparation, can solve the problems of the by-product ethanol not being effectively used, the by-products affecting the environment, and the energy consumption of the process, etc., to improve the purity of the product , environmental protection, high conversion rate of ethanol

Inactive Publication Date: 2018-10-12
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since DEM forms azeotrope with ethanol and water, high reflux ratio (reflux ratio about 15-20:1) precision distillation method is used to extract DEM, the DEM content is only about 83-91%, and the process consumes a lot of energy
In order to obtain more than 99% DEM, there are currently two processing methods, one is to use sodium metal or alkali distillation to remove ethanol, and then obtai

Method used

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  • Device for recycling industrial grade diethoxymethane and method for recycling industrial grade diethoxymethane
  • Device for recycling industrial grade diethoxymethane and method for recycling industrial grade diethoxymethane
  • Device for recycling industrial grade diethoxymethane and method for recycling industrial grade diethoxymethane

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Experimental program
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Effect test

Embodiment 1

[0020] Such as figure 2 As shown, the method for refining and recycling industrial grade industrial grade diethoxymethane using the device of the present invention comprises the following steps:

[0021] (1) add extraction agent and industrial grade diethoxymethane (DEM) respectively by the industrial grade diethoxymethane feed inlet 30 of liquid-liquid extraction device and extractant inlet 5, this extractant and industrial grade The ratio of the DEM addition is 0.995:1, the starting motor 26 stirring speed 80rpm, by N 2 The gas cylinder adjusts the pressure P1 of the buffer bottle 33, and the pressure P2 of the catalytic conversion device 4 is controlled to be greater than the pressure P3 of the liquid-liquid extraction device 3. After the extraction reaction, the raffinate phase outlet 29 at the upper end of the liquid-liquid extraction device 3 obtains a concentration of Up to 99.07% DEM;

[0022] (2) The mixed solution containing extractant and ethanol flowing out from...

Embodiment 2

[0029] Adopt the device of the present invention to carry out the method for refining and recycling industrial grade technical grade diethoxymethane comprising the following steps:

[0030](1) add extraction agent and industrial grade diethoxymethane (DEM) respectively by the industrial grade diethoxymethane feed inlet 30 of liquid-liquid extraction device and extractant inlet 5, this extractant and industrial grade The ratio of the DEM addition is 0.8:1, the starting motor 26 stirring speed 80rpm, by N 2 The gas cylinder adjusts the pressure P1 of the buffer bottle 33, and the pressure P2 of the catalytic conversion device 4 is controlled to be greater than the pressure P3 of the liquid-liquid extraction device 3. After the extraction reaction, the raffinate phase outlet 29 at the upper end of the liquid-liquid extraction device 3 obtains a concentration of Up to 99.02% DEM;

[0031] (2) The mixed solution containing extractant and ethanol flowing out from the extraction pha...

Embodiment 3

[0033] Adopt the device of the present invention to carry out the method for refining and recycling industrial grade technical grade diethoxymethane comprising the following steps:

[0034] (1) add extraction agent and industrial grade diethoxymethane (DEM) respectively by the industrial grade diethoxymethane feed inlet 30 of liquid-liquid extraction device and extractant inlet 5, this extractant and industrial grade The ratio of the DEM addition is 1.5:1, the starting motor 26 stirring speed 80rpm, by N 2 The gas cylinder adjusts the pressure P1 of the buffer bottle 33, and the pressure P2 of the catalytic conversion device 4 is controlled to be greater than the pressure P3 of the liquid-liquid extraction device 3. After the extraction reaction, the raffinate phase outlet 29 at the upper end of the liquid-liquid extraction device 3 obtains a concentration of Up to 99.09% DEM;

[0035] (2) The mixed solution containing extractant and ethanol flowing out from the extraction ph...

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Abstract

The invention discloses a device for recycling industrial grade diethoxymethane and a method for recycling the industrial grade diethoxymethane, the device comprises an extraction conversion tower anda side line regeneration tower connected with the extraction conversion tower, and the extraction conversion tower comprises a liquid-liquid extraction device and a catalytic conversion device whichare integrally arranged up and down. The method is as follows: the industrial grade diethoxymethane and an extractant are added into the liquid-liquid extraction device for reaction, and then a mixedsolution containing the extractant is sent to the side line regeneration tower for reaction; the mixed solution containing the extractant obtained at the bottom of the side line regeneration tower iscirculated to the liquid-liquid extraction device, an ethanol mixed solution obtained at the top of the tower is circulated to the catalytic conversion device, and a mixture of a formaldehyde solutionand a catalyst is added to the catalytic conversion device for catalytic conversion reaction. The significant advantage of the device is that the device can not only effectively recycle the industrial grade diethoxymethane, but also realize catalytic conversion of ethanol; the process is simple and the environment is protected.

Description

technical field [0001] The invention belongs to the field of preparation of diethoxymethane, and in particular relates to a device for recycling industrial-grade diethoxymethane and a method for recycling it. Background technique [0002] Diethoxymethane (abbreviation: DEM) has strong stability to alkalis and oxidants. It can be used not only as a solvent in organic synthesis, as a solvent in batteries, as a fuel additive, etc., but also as a reagent for organic reactions, such as formaldehyde. Equivalents, substrates for carbonylation, etc. [0003] At present, the methods for synthesizing DEM mainly include halogenated hydrocarbon method, polyphosphoric acid method, inorganic salt method, acid catalysis method and chloramphenicol by-product method, and the reaction generates about 46-58% DEM mixture. Since DEM forms azeotrope with ethanol and water, high reflux ratio (reflux ratio about 15-20:1) precision distillation method is used to extract DEM, the DEM content is only...

Claims

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Application Information

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IPC IPC(8): C07C41/58C07C43/30
CPCC07C41/58C07C43/30Y02P20/584
Inventor 顾正桂曹晓艳凌鸿钰李硕黄鑫王春梅
Owner NANJING NORMAL UNIVERSITY
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