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Method and device for preparing ethyl tert-alkyl ether by distillation - extraction coupling separation and purification

A technology for separation and purification of ethyl tertiary alkyl ether, applied in the field of purification and preparation of ethyl tertiary alkyl ether, can solve the problems of high energy consumption separation method under operating conditions, reduction of commercial value, etc., and achieves improved utilization rate, high commercial value, and reduced cost effect

Inactive Publication Date: 2012-06-13
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] These several types of methods described have their own advantages and disadvantages, but the common defect that they exist is: there are strict requirements on the content of some components of the material entering the de-butanizer distillation tower (especially ETBE, which requires entering the "de-butanizer" The water content in the material is at most 1% by weight, the content of tert-butanol (TBA) is at most 1% by weight (see CN1127243A and US 5,607,557A, etc.)), and / or adopt adsorption separation, pervaporation membrane separation, azeotropic Separation and other special separation methods
Such harsh operating conditions and / or high energy consumption separation methods lead to a reduction in the commercial value of the existing separation and purification methods for preparing ethyl tertiary alkyl ethers

Method used

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  • Method and device for preparing ethyl tert-alkyl ether by distillation - extraction coupling separation and purification
  • Method and device for preparing ethyl tert-alkyl ether by distillation - extraction coupling separation and purification
  • Method and device for preparing ethyl tert-alkyl ether by distillation - extraction coupling separation and purification

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Effect test

Embodiment 1

[0067] Process reference figure 1 , ethanol containing about 5% by weight of azeotropic water and recovered ethanol was mixed with isoamylene containing C 5 The material after the etherification reaction of hydrocarbons in the reaction zone R is used as the material of the to-be-separated mixture of ethyl tert-alkyl ether (line 3), and is separated in the first distillation column C1 after heat exchange to 65°C.

[0068] The first distillation column C1 has 80 trays in total, the feeding position is the 24th tray, the operating pressure at the top of the column is 4 bar, the reflux ratio is 1.5, and the temperature at the top of the column is 85°C. Collect unreacted mixed C from the top of the first distillation column C1 5 Hydrocarbon fraction (line 5), obtain TAEE-containing fraction (one of the products, pipeline 4) from the bottom of the first distillation tower C1, the side line feed position is the 45th tray, and the material at about 132 ° C taken out from the liquid p...

Embodiment 2

[0075] Process reference figure 1 , ethanol containing about 5% by weight of azeotropic water and recovered ethanol was mixed with C 4 The material after the etherification reaction of hydrocarbons in the reaction zone R is used as the mixture material (line 3) to be separated of ethyl tertiary alkyl ether, and the material from the extraction tower C 3 The overhead raffinate (line 11) is combined and then fed to the first distillation column C1.

[0076] The first distillation column C1 has 80 trays in total, the feed temperature is 65°C, the feed position is the 40th tray, the operating pressure at the top of the tower is 8 bar, the reflux ratio is 0.75, and the temperature at the top of the tower is 65°C. The first distillation column C1 top collects the unreacted mixture C 4 For the hydrocarbon fraction (line 5), the side feed position is the 64th tray, and the material (line 6) at about 135°C taken out from the liquid phase is cooled to 65°C and then enters the second d...

Embodiment 3

[0082] Process reference figure 1 , ethanol containing about 5% by weight of azeotropic water and recovered ethanol was mixed with C 4 The material after the etherification reaction of hydrocarbons in the reaction zone R is used as the to-be-separated mixture material (line 3) of ethyl tert-alkyl ether, which is combined with the raffinate (line 11) from the top of the extraction tower C3 and then used as the first distillation Feed to column C1.

[0083] The first distillation column C1 has 80 trays in total, the feed temperature is 65°C, the feed position is the 40th tray, the operating pressure at the top of the tower is 8 bar, the reflux ratio is 0.75, and the top temperature is 65°C. Collect unreacted mixed C from the top of the first distillation column C1 4 Hydrocarbon fraction (pipeline 5), the side feed position is the 64th tray, and the material (pipeline 6) at about 135°C taken out from the liquid phase is cooled to 65°C and then enters the second distillation tow...

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Abstract

The invention provides a method and a device for preparing ethyl tert-alkyl ether by distillation - extraction coupling separation and purification. The method uses a mixture to be separated of ethyl tert-alkyl ether prepared by etherification of ethanol with water content of at least more than 1 weight percentage and at most 15 weight percentage and isoolefine with at least four carbon atoms as a raw material, and the method is carried out by a distillation - extraction coupling separation method. The method and the device are beneficial to increase the utilization rate of an isoolefine resource, and the circulation volume of tertiary alcohol harmful to a reaction zone is greatly reduced in the whole process of separation and purification. At the same time, the method and the device can reduce the cost, can especially adopt the ethanol with water content of more than 1 weight percentage and at most 15 weight percentage belonging to the renewable resource as the raw material of etherification, can obtain qualified ethyl tert-alkyl ether products, and can coproduce corresponding atomic alcohol (including especially corresponding tertiary alcohol), therefore having a high commercialvalue (function / cost).

Description

technical field [0001] The present invention relates to a method and device for preparing ethyl tertiary alkyl ether, in particular to a method and device for purifying and preparing ethyl tertiary alkyl ether. The method for purifying and preparing ethyl tertiary alkyl ether is carried out by distillation-extraction coupled separation method. Background technique [0002] The development of bio-based fuels based on ethanol (EtOH) produced by fermentation has attracted more and more attention from many countries in the world. [0003] However, fuel ethanol is currently the most important bio-based alcohol ether fuel. One of the key issues of its energy consumption and cost constraints is that if you want to remove about 5% by weight of azeotropic water to below 1% by weight, you need to use constant boiling water. Distillation, extractive distillation, adsorption, pervaporation membrane separation and other special separation methods, and usually need to add a small amount ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/04C07C41/34B01D11/04B01D3/14
CPCC07C41/42
Inventor 张武平张文里周山花田恒水张涵璐诸富根江兆顾京君
Owner EAST CHINA UNIV OF SCI & TECH