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A kind of rectification-steam permeation coupled method and device for producing diethyl maleate

A technology of diethyl maleate and steam, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., to achieve the effects of improving dehydration efficiency, avoiding secondary pollution, and high resource recovery rate

Active Publication Date: 2015-11-18
JIANGSU NINE HEAVEN HIGH TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is: need to use the problem of the 3rd component in the production process of diethyl maleate in the prior art, propose a kind of rectification-steam permeation coupling production method of diethyl maleate and device

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  • A kind of rectification-steam permeation coupled method and device for producing diethyl maleate

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Experimental program
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Effect test

Embodiment 1

[0024] In the reaction kettle, 0.04kg of concentrated sulfuric acid is used as a catalyst, and maleic acid (1.2kg) and absolute ethanol (3L) are subjected to esterification reaction. For preliminary separation, the height of the rectification column is 1m, the diameter of the column is 37mm, and it is filled with 3mm*0.5mm glass spring packing; the heavy component in the rectification column is refluxed to the reactor, and the light component is discharged from the top, which mainly contains ethanol And water, light component steam is reheated to 100°C by a supplementary heater and enters the steam permeable membrane module for dehydration. The membrane module has a membrane area of ​​0.03m 2 The single-tube NaA molecular sieve membrane module, the permeate side pressure is controlled at 300Pa, and the dehydrated ethanol is returned to the reactor from the top of the rectification column and the top of the reactor respectively. The ratio of ethanol entering the rectification co...

Embodiment 2

[0026] In the reactor, use ferric ammonium sulfate dodecahydrate as catalyst (0.3kg) to carry out esterification reaction of maleic acid (1.2kg) and absolute ethanol (3L), the temperature in the reactor is 120°C, the steam generated at the top of the reactor Preliminary separation is carried out through the rectification column. The height of the rectification column is 1m, the diameter of the column is 37mm, and it is filled with 3mm*0.5mm glass spring packing. It mainly contains ethanol and water. The light component steam is heated to 115°C by a supplementary heater and enters the steam permeable membrane module for dehydration. The membrane module has a membrane area of ​​0.03m 2 The single-tube T-type molecular sieve membrane module, the permeate side pressure is controlled at 300Pa, the dehydrated ethanol is returned to the reactor from the top of the rectification column and the top of the reactor respectively, and the ratio of ethanol entering the rectification column t...

Embodiment 3

[0029] In the reactor, use concentrated sulfuric acid as catalyst (0.4kg) to carry out the esterification reaction between maleic acid (24kg) and absolute ethanol (60Lg). For preliminary separation, the height of the rectification column is 2.5m, the diameter of the column is 100mm, and the filling is 6mm×6mm×0.1mm with stainless steel multi-layer rectangular wire mesh packing; the heavy components after rectification are returned to the reactor, and the light components are discharged from the top , which mainly contains ethanol and water, and the light component steam is reheated to 100°C through the supplementary heater and enters the steam permeation membrane module for dehydration. The membrane module consists of 4 stages of 0.25m 2Tubular NaA molecular sieve membrane modules with membrane area are formed in series, and the permeate side pressure is controlled at 1000Pa. The ethanol after dehydration is returned to the reactor from the top of the rectification column and t...

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Abstract

The invention relates to a method and device for producing diethyl maleate by virtue of rectification and steam osmosis coupling, belonging to the technical field of separation and application of pervaporation membranes. The method comprises the following steps: in a reaction kettle, heating maleic acid and ethanol under the action of a catalyst to generate diethyl maleate and water, enabling a gaseous mixture above the reaction kettle to flow through a rectification column under the driving of pressure difference, performing heat exchange on the gaseous mixture and a reflux liquid to ensure that ethanol and water mixed gas can flow out from the top of the rectification column, replenishing heat for the ethanol and water mixed gas, putting the ethanol and water mixed gas into steam osmosis membrane equipment, then performing dehydration, condensing dehydrated ethanol, and conveying ethanol to the reaction kettle from the top of the rectification column. A process method disclosed by the invention ensures that water in an esterification reaction system is continuously removed under the condition that other impurities are not introduced, so that the reaction can be promoted to the generation direction of diethyl maleate, and the conversion rate of the reaction can be effectively improved; and an overall esterification reaction and steam osmosis coupling system is less in floor area, is easy to amplify, and is low in energy consumption.

Description

technical field [0001] The invention relates to a rectification-steam permeation coupled method and device for producing diethyl maleate, belonging to the technical field of steam permeation membrane separation applications. Background technique [0002] Esterification generally refers to the process in which alcohols and phenols react with oxygen-containing acids (including organic and inorganic acids) to form esters and water. The esterification process is an equilibrium reaction. When the reaction reaches equilibrium, the conversion rate is low. If the water in the product is removed, the conversion rate can be further increased, thereby increasing the yield of the ester. In the existing production process of diethyl maleate, benzene is used as a water-carrying agent, and benzene, ethanol and water can be used to form a three-component minimum azeotropic liquid, and the organic phase returns to the reaction system after the azeotropic liquid is separated. , so that the w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/60
CPCC07C67/08C07C69/60
Inventor 顾学红仲超余从立庆祖森
Owner JIANGSU NINE HEAVEN HIGH TECH
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