Method for recycling acetic acid in dilute acetic acid

A technology of dilute acetic acid and acetic acid, which can be used in solvent extraction of liquid solutions, separation/purification of carboxylic acid compounds, organic chemistry, etc., and can solve problems such as low separation efficiency

Active Publication Date: 2008-05-07
SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is that there is a problem of low separation efficiency in the process of reclaiming acetic acid in dilute acetic acid solution in the prior art, and a new method for reclaiming acetic acid in dilute acetic acid solution is provided

Method used

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  • Method for recycling acetic acid in dilute acetic acid
  • Method for recycling acetic acid in dilute acetic acid
  • Method for recycling acetic acid in dilute acetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The extraction tower is filled with 3 mm × mm θ ring wire mesh packing, with an effective height of 1.2 meters, which is equivalent to 11 theoretical plates. The weight percentage of acetic acid in the dilute acetic acid solution is 6.8%, the percentage of water is 93.2%, and the extraction agent Percentage by weight: mixed amine (tributylamine and tripentylamine account for 35% and 65% by weight respectively, hereinafter the same) is 32.5%, n-octanol is 48.7%, kerosene fraction above 160°C is 18.8% , the dilute acetic acid solution and the extractant both enter the top and bottom of the extraction tower at a flow rate of 0.70 kg / h, the extraction temperature is 35°C, the air compressor pressure is 150kPa, and the pulse frequency of the solenoid valve is 0.05 seconds-1. After the operation is stable, the extraction phase And the temperature of raffinate phase is 40 ℃ and 37 ℃ respectively, and analysis obtains the composition of extract phase and raffinate phase and sees...

Embodiment 2

[0025] Keep other conditions of the extraction tower as in Example 1, change the composition of the extractant, the mixed amine weight content is 21.2%, the n-octanol weight content is 42.6%, the kerosene weight content is 36.2%, the analysis obtains the extraction phase and the raffinate phase The composition is shown in the table below. After being separated by the whole technological process, the recovery rate of acetic acid is 92%.

[0026] Extraction tower extraction result

[0027]

Embodiment 3

[0029] Keep other conditions of the extraction tower as in Example 1, change the extraction temperature to 60° C., and analyze the composition of the extract phase and raffinate phase as shown in the table below. After being separated by the whole technological process, the recovery rate of acetic acid is 85%.

[0030] Extraction tower extraction result

[0031]

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Abstract

The invention relates to a method for recycling acetic acid from diluted acetic acid, and aims at solving the problem that the recycling of acetic acid in the hydrolysis of furfural and methyl acetate as well as the Fischer-Tropsch combined production is difficult. The invention comprises the steps as follows: a) diluted acetic acid is extracted by a pulse filling extracting tower, the extractionphase containing extracting agent, the acetic acid and little water for the tower top is acquired, and the residual extraction phase of water containing micro acetic acid from the tower kettle is acquired; b) the extraction phase in an extracting agent recycling tower is conveyed; c) acetic acid 1 is fed into an azeotropic rectifying tower which utilizes one kind of benzene, cyclohexane, ethyl acetate, isopropyl acetate and butyl acetate as the extrainer, two-phase mixture of the extrainer and the water at a phase separator at the top of the tower is acquired, the water is extracted out from the tower top, and the retrainer returns into the tower. The utility model has the technical proposal of producing pure acetic acid at the tower top, solves the problems above, and adapts the industrial productions including recycling of acetic acid from wasted aldehyde water and extracting and refining acetic acid in the methyl acetate hydrolysis technique.

Description

technical field [0001] The invention relates to a method for recovering acetic acid in dilute acetic acid solution. Background technique [0002] Acetic acid-water mixture is usually separated by rectification, extractive rectification, azeotropic rectification and other methods, but when these methods are used for the separation of dilute acetic acid, the energy consumption is too large. Therefore, the commonly used method for the treatment of dilute acetic acid aqueous solution is as follows: [0003] 1. Sodium acetate method: Use sodium hydroxide to neutralize acetic acid in dilute acid solution to generate sodium acetate, then use it as a low-pressure boiler water supply to evaporate its concentration to 15% to 25%, and finally add concentrated sulfuric acid to the concentrated salt converted to acetic acid. [0004] The drawback of this method is that the quality of the sodium acetate that reclaims is poor, and sodium hydroxide is expensive, uneconomical. Currently, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/48C07C53/08B01D11/04
Inventor 钟禄平肖剑陈秀宏钟思青顾军民张惠明
Owner SHANGHAI RES INST OF PETROCHEMICAL TECH SINOPEC
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