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Technology and device for diethyl oxalate synthesis through vapor permeation dehydration process

A diethyl oxalate and osmotic dehydration technology, which is applied in the separation/purification of carboxylate, preparation of carboxylate, and preparation of organic compounds, etc., can solve the problems of water removal, etc., and achieve pollution elimination, high selectivity, and high efficiency. conversion rate effect

Inactive Publication Date: 2015-09-23
JIANGSU NINE HEAVEN HIGH TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The technical problem to be solved in the present invention is to overcome the diethyl oxalate synthesis process using the third component and the problem of water removal in the reaction process, and propose a process and device for the synthesis of diethyl oxalate in a steam permeation dehydration process

Method used

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  • Technology and device for diethyl oxalate synthesis through vapor permeation dehydration process

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Experimental program
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Effect test

Embodiment 1

[0019] In the reaction kettle, under the action of 0.01kg of concentrated sulfuric acid catalyst, 1 kg of oxalic acid and 3.5 L of absolute ethanol are used for esterification reaction. 40 mm, the rectification column is filled with 3 mm × 0.5 mm glass spring packing, the top of the rectification column is controlled at about 78 °C under normal pressure, and the heavy part of the vapor in the reactant returns to the reaction after passing through the rectification column In the still, the light components are condensed by the top condenser and sent to the top of the rectification column through the transfer pump as a reflux liquid, the reflux ratio is 5, and the other part enters the evaporator, is heated and vaporized by the evaporator to 110°C and enters the steam Permeable membrane for dehydration, the membrane module is 2 membranes with an area of ​​0.03 m 2 The single-tube NaA molecular sieve membrane components are connected in series, and the pressure on the permeate si...

Embodiment 2

[0021] In the reaction kettle, under the action of 0.03kg of p-toluene sulfonic acid as a catalyst, 2 kg of oxalic acid and 7 L of absolute ethanol were used for esterification reaction. It is about 40 mm, and the rectification column is filled with 3 mm×0.5 mm glass spring packing. Under the operating pressure of about 0.1 MPa, the top of the rectification column is controlled at about 100 ° C. After passing through the rectification column, the vapor in the reactant The heavy component is returned to the reaction kettle, and the light component is condensed by the top condenser, and part of the light component is sent to the top of the rectification column as reflux liquid through the transfer pump. The reflux ratio is 4, and the other part enters the evaporator, and is heated and vaporized by the evaporator Enter the steam permeation membrane at 120°C for dehydration, and the membrane module consists of 4 membranes with an area of ​​0.03 m 2 The single-tube T-type molecular...

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Abstract

The invention relates to a technology and device for diethyl oxalate synthesis through a vapor permeation dehydration process, and belongs to the technical field of pervaporation membrane separation application and organic compound synthesis technologies. The technology comprises the following steps: under the action of a catalyst, oxalic acid and ethyl alcohol are subjected to esterification reaction in a reaction kettle provided with a rectification column, and after steam generated during the reaction passes through the rectification column, heavy components return into the reaction kettle; light components are condensed, then, one part of the light components are sent to the top of the rectification column for refluxing, the other part of the light components enter a pervaporation membrane raw material solution side to be subjected to vapor permeation dehydration, and the obtained products are condensed to return into the reaction kettle. According to the invention, water in the esterification reaction process is continuously removed in the situation that an azeotropic dehydration agent causing pollution to the environment is not introduced, so that the reaction is facilitated, the conversion rate of the reaction is increased, the problem about the post-processing of the azeotropic dehydration agent and the problem of environment pollution of the azeotropic dehydration agent are avoided, and the production cost is reduced.

Description

technical field [0001] The invention relates to a process and a device for synthesizing diethyl oxalate in a steam permeation dehydration process, and belongs to the technical field of pervaporation membrane separation application and organic compound synthesis technology. Background technique [0002] Diethyl oxalate is an intermediate of medicine, plastics, dyes and other products, and can also be used as a solvent for cellulose and spices. In China, diethyl oxalate is mainly produced by direct oxalate esterification. In this method, benzene or toluene is used as the azeotropic water-carrying agent, and then the phases are separated and refluxed for dehydration until anhydrous is taken out from the reaction substance, and the benzene (toluene) and ethanol are distilled off to obtain the crude diethyl oxalate. However, this method uses benzene or toluene, which must be removed during the refining process of diethyl oxalate, and at the same time pollutes the environment....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/36C07C67/08C07C67/48
CPCC07C67/08C07C67/48C07C69/36
Inventor 余从立仲超顾学红庆祖森
Owner JIANGSU NINE HEAVEN HIGH TECH