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Method for separating acetic acid and water by complexation extraction and rectification

An extractive distillation and complexation technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of complex operation control, large amount of extractant, large amount of azeotrope, etc. The effect of improved volatility and good reliability

Inactive Publication Date: 2003-03-26
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ordinary rectification has a simple process flow and easy operation and control, but requires a large number of trays and consumes a lot of energy in the process; azeotropic distillation uses a small number of trays, but the amount of azeotrope is large, the configuration is complicated, and the process consumes a lot of energy. Operational control is more complicated; US5167774 and US4729818 have disclosed and adopted the method separation acetic acid of common extractive rectification and water, and the selection range of this method extractant is wide, and operation control is easy, but there is extractant Weaknesses such as large dosage, large number of trays, and large energy consumption

Method used

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  • Method for separating acetic acid and water by complexation extraction and rectification
  • Method for separating acetic acid and water by complexation extraction and rectification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Such as figure 1 As shown, the experimental process consists of an extractive distillation column 1 and a solvent recovery column 2. The extractive distillation tower has 30 theoretical trays (the number of trays is counted from top to bottom), and the tributylamine liquid mixture (mass fraction exceeding 15%) that contains a small amount of acetic acid is selected as the complex extraction agent, from the 4th theoretical plate The plate is added, and the flow rate is 10ml / min. The mixture of acetic acid and water is added from the 15th theoretical plate, and the composition is 71.13wt% of water, 28.87wt% of acetic acid, and the flow rate is 10ml / min. The extractive distillation tower is operated under normal pressure, the reflux ratio at the top of the tower is 1, the temperature at the top of the tower is controlled at 99.5°C-101.0°C, the mass fraction of water at the top product is 99.74%, and the mass fraction of acetic acid is 0.26% through gas chromatography analy...

Embodiment 2

[0022] Same as in Example 1, the experimental process consists of an extractive distillation tower and a solvent recovery tower. The extractive distillation tower has 30 theoretical trays (the number of trays is counted from top to bottom), and the tributylamine liquid mixture (mass fraction exceeding 10%) that contains a small amount of acetic acid is selected as the complex extraction agent, from the 4th theoretical plate The plate is added, and the flow rate is 10ml / min. The mixture of acetic acid and water is added from the 15th theoretical plate, and the composition is 71.13wt% of water, 28.87wt% of acetic acid, and the flow rate is 10ml / min. The extractive distillation tower is operated under normal pressure, the top reflux ratio is 0, the top temperature is controlled at 99.5°C-101.0°C, the top product is analyzed by gas chromatography, the mass fraction of water is 99.81%, and the mass fraction of acetic acid is 0.19% %, to meet the separation requirements. The soluti...

example 3

[0023] Same as in Example 1, the experimental process consists of an extractive distillation tower and a solvent recovery tower. The extractive distillation column has 30 theoretical trays (the number of trays is counted from top to bottom), and the tripentylamine liquid mixture (mass fraction exceeding 10%) that contains a small amount of acetic acid is selected as the complex extraction agent, from the 4th theoretical plate The plate is added, and the flow rate is 10ml / min. The mixture of acetic acid and water is added from the 15th theoretical plate, and the composition is 69.97wt% of water, 30.03wt% of acetic acid, and the flow rate is 10ml / min. The extractive distillation tower is operated under normal pressure, the reflux ratio at the top of the tower is 1, and the temperature at the top of the tower is controlled at 99.5°C-101.0°C. The mass fraction of water at the top product is 99.77% and the mass fraction of acetic acid is 0.23% through gas chromatography analysis. %...

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Abstract

THe invention provides a method for separating acetic acid and water by complexation, extraction and rectification process. Said invention utilizes the acting force between organic alkali and acetic acid, which is stronger than that of water, and greatly raises the relative volatilities of acetic acid and water so as to separate them. In the fractionating recrtifying tower with 10-50 theoretical plates it adopts tertiary amine organic alkali as complexation extracting agent, under the condition of normal pressure (or reduced pressure), its solvent ratio is 0.5-5 and refluxing ratio is 0-5, the water whose mass fraction is greater than 99.7% can be obtained from tower top, and in the solvent recovering tower with 5-40 the oretical plates, under the condition of reduced pressure and refluxing ratio of 0.5-5 the acetic acid whose mass fraction is greater than 95.0% can be obtained.

Description

Technical field: [0001] The invention relates to a method for separating acetic acid and water, in particular to separating acetic acid and water by means of extraction and rectification. Background technique: [0002] In the production process of acetic acid, because the relative volatility of acetic acid and water is close to 1, their separation is relatively difficult, and the methods of ordinary rectification and azeotropic rectification are generally used at home and abroad. Ordinary distillation has a simple process flow and easy operation and control, but requires a large number of trays and consumes a lot of energy in the process; azeotropic distillation uses a small number of trays, but the amount of azeotropic agent is large, the configuration is complicated, and the process consumes a lot of energy. Operational control is more complicated; US5167774 and US4729818 have disclosed and adopted the method separation acetic acid of common extractive rectification and wa...

Claims

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Application Information

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IPC IPC(8): C07C51/44C07C53/08
Inventor 雷志刚李成岳陈标华
Owner BEIJING UNIV OF CHEM TECH
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