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Method for separating isobutanol and ethyl isobutyrate azeotrope by continuous extractive distillation

A technology of ethyl isobutyrate and extractive distillation, which is applied in extractive distillation, chemical instruments and methods, preparation of carboxylate, etc., can solve problems such as unseen data, and achieve the effect of reducing cost, saving cost and simple process

Inactive Publication Date: 2015-06-10
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many articles and patents on extractive distillation, but there is no published information on extractive distillation and separation of isobutanol-ethyl isobutyrate azeotropic system

Method used

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  • Method for separating isobutanol and ethyl isobutyrate azeotrope by continuous extractive distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A method for continuous extraction and rectification separation of isobutanol and ethyl isobutyrate azeotrope, its process flow diagram is as follows figure 1 shown. The number of theoretical plates in the extractive distillation column 3 is 55. Use 95wt% ethylene glycol and 5wt% [Emim][OAc] as the extractant, add it from the third theoretical plate (the number of plates is from top to bottom, nozzle 1), and the flow rate is 1.8kg / hr. The mixture of isobutanol and ethyl isobutyrate is added from the 42nd theoretical plate (pipe port 2), the flow rate is 1kg / hr, the mass fraction of isobutyric acid is 52%, 3 is operated under normal pressure, and the tower top The reflux ratio is 7:1, the temperature at the top of the tower is 110~115°C, and the temperature at the bottom of the tower is 140~150°C. The product at the top of the tower is analyzed by gas chromatography, and the ethyl isobutyrate product with a purity higher than 99.8% is obtained.

[0025] The bottom of t...

Embodiment 2

[0027] The two-column process flow of the extractive distillation column goes through Example 1. 85wt% ethylene glycol and 15wt% [Emim][OAc] were used as the extractant, fed from the third theoretical plate, and the flow rate was 2.2kg / hr. The mixture of isobutanol and ethyl isobutyrate is added from the 42nd theoretical plate, the flow rate is 1kg / hr, and the composition is the same as in Example 1. The rectification column 3 operates under normal pressure with a reflux ratio of 5.0:1. At this time, the temperature at the top of the tower is 110~113°C, and the temperature at the bottom of the tower is 130~140°C. The overhead product is analyzed by gas chromatography to obtain an ethyl isobutyrate product with a purity higher than 99.7%.

[0028] The operating conditions of the solvent recovery tower are the same as in Example 1, and the bottom of the tower is returned to the extractive distillation tower 3 for recycling, and other conditions are the same as in Example 1.

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Abstract

The invention relates to a method for separating an isobutanol and ethyl isobutyrate azeotrope by continuous extractive distillation. Glycol and 1-ethyl-3-methylimidazolium acetate [Emim] [OAc] which is an ionic liquid are used as extracting agents to carry out extractive distillation; high-purity ethyl isobutyrate is obtained on the top of an extractive distillation tower, high-purity isobutanol is obtained on the top of a solvent recovery tower, and high-concentration glycol is obtained on the bottom of the solvent recovery tower; and the extracting agents can flow back to a solvent tank to serves as the supplement to the solvent.

Description

technical field [0001] The invention relates to a method for continuous extraction and rectification to separate isobutanol and ethyl isobutyrate azeotrope, which mainly involves the extraction and rectification of isobutanol and ethyl isobutyrate azeotrope. Background technique [0002] Extractive distillation is a special distillation separation technology, suitable for azeotropic systems that cannot be separated by ordinary distillation separation methods. The most important thing in extractive distillation is the choice of extractant. The choice of extraction agent mainly depends on the selectivity of the selected solvent to be separated from A and B components, so that the relative volatility of A and B components will increase. The extractant is generally added from the upper part of the tower, and the material is added from the middle and lower part of the tower. [0003] Ionic liquid is a new type of green medium, which has the advantages of non-volatile, strong co...

Claims

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Application Information

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IPC IPC(8): C07C27/32C07C31/12C07C29/84C07C69/24C07C67/54C07B63/00B01D3/40
CPCC07C29/80C07C29/84C07C67/54C07C31/12C07C69/24
Inventor 姜占坤刘顺江孙国新
Owner UNIV OF JINAN
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