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Method for recovering dilute acetic acid through extraction by cyclohexyl acetate

A technology of cyclohexyl acetate and dilute acetic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve the problems of low acetic acid recovery rate and long process flow

Active Publication Date: 2017-06-20
SINOPEC SHANGHAI ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The technical problem to be solved by the present invention is the problem of long process flow and low recovery rate of acetic acid in the prior art, and a new method for extracting and reclaiming dilute acetic acid with cyclohexyl acetate is provided

Method used

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  • Method for recovering dilute acetic acid through extraction by cyclohexyl acetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The invention utilizes cyclohexyl acetate, an intermediate product of the cyclohexanone plant, as an extractant, and extracts and rectifies the dilute acetic acid produced by the cyclohexanone plant to separate the acetic acid from water to recover the acetic acid for reuse. The production scale of the cyclohexanone plant is 100,000 tons / year.

[0031] Such as figure 1 Shown, the dilute acetic acid feed (5) of cyclohexanone plant by-product enters the top of the extraction tower (1), and the intermediate product cyclohexyl acetate feed (6) of the cyclohexanone plant enters the bottom of the extraction tower (1). The acetic acid in the dilute acetic acid (5) is extracted by the stream through the countercurrent extraction method. The raffinate waste water (8) flows out from the bottom of the extraction tower (1) and is sent out. The extraction phase (7) is discharged from the top of the extraction tower (1), returns to the acetic acid separation tower (2), and is fed f...

Embodiment 2

[0035] According to the conditions and steps described in Example 1, only the production scale of the cyclohexanone plant was changed to 200,000 tons / year.

[0036] The process parameters are as follows: the operating temperature of the extraction tower is 50 ° C, the operating pressure is 0.46 MPaA, the mass ratio of the dilute acetic acid feed at the top of the extraction tower to the cyclohexyl acetate feed at the bottom of the extraction tower = 1:6.3, and the dilute The acetic acid concentration of acetic acid feed is 49% (mass), and temperature is 50 ℃, and pressure is 0.56MPaA, and the temperature of cyclohexyl acetate feed at the bottom of extraction tower tower is 50 ℃, and pressure is 0.61MPaA, and acetic acid separating tower tower top operation The temperature is 118°C, the operating temperature at the bottom of the tower is 186°C, the operating pressure is 0.16MPaA, the reflux ratio is 6.7, the temperature of the feed stream of the acetic acid separation tower is 1...

Embodiment 3

[0039] According to the conditions and steps described in Example 1, only the production scale of the cyclohexanone plant was changed to 400,000 tons / year.

[0040] The process parameters are as follows: the operating temperature of the extraction tower is 32 ° C, the operating pressure is 0.21 MPaA, the mass ratio of the dilute acetic acid feed at the top of the extraction tower to the cyclohexyl acetate feed at the bottom of the extraction tower = 1:8.9, and the dilute The acetic acid concentration of acetic acid feed is 39% (mass), and temperature is 32 ℃, and pressure is 0.38MPaA, and the temperature of cyclohexyl acetate feed at the bottom of extraction column is 32 ℃, and pressure is 0.41MPaA, and acetic acid separating tower top operation The temperature is 111°C, the operating temperature at the bottom of the tower is 176°C, the operating pressure is 0.14MPaA, the reflux ratio is 9.1, the temperature of the feed stream of the acetic acid separation tower is 131°C, and t...

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Abstract

The invention relates to a method for recovering dilute acetic acid through extraction by cyclohexyl acetate. The method is mainly used for solving the problems in the prior art that process flows are long and the recovery ratio of acetic acid is low. According to the method, by adopting the technical scheme that the method for recovering dilute acetic acid through extraction by cyclohexyl acetate comprises the steps of firstly, carrying out extraction on a byproduct, i.e., dilute acetic acid of a cyclohexanone device by taking cyclohexyl acetate as an extractant, then, carrying out rectifying separation so as to obtain acetic acid, and carrying out recovery and reutilization, wherein the content of acetic acid in raffinate phase wastewater of an extraction tower is lower than 100ppm, the content of cyclohexyl acetate in the raffinate phase wastewater of the extraction tower is lower than 1.0%, the rate of consumption of the extractant is lower than 0.10%, the content of acetic acid in the tower top of an acetic acid separating tower is not lower than 95.0%, the content of acetic acid in the tower bottom of the acetic acid separating tower is lower than 100ppm, and the recovery ratio of acetic acid is not lower than 99.0%, the problems are solved in a relatively good manner, so that the method can be applied to the industrial production of recovery of dilute acetic acid.

Description

technical field [0001] The invention relates to a method for extracting and recovering dilute acetic acid with cyclohexyl acetate. Background technique [0002] Acetic acid is an important light industry and chemical raw material, widely used in organic synthesis industry. In the process of producing cyclohexanone by esterification and hydrogenation, dilute acetic acid solution with a by-product concentration of less than 50% needs to adopt reasonable process operation means to concentrate the acetic acid and recycle it for utilization. [0003] Ordinary rectification method has mature technology and simple process. Although acetic acid and water do not form azeotrope in this method, the relative volatility of acetic acid and water is close to 1, so the required number of theoretical plates and reflux ratio are relatively large, and the energy consumption is relatively large. Large and expensive to produce. Moreover, under high temperature conditions, the material requirem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/48C07C53/08
CPCC07C51/42C07C51/48C07C53/08
Inventor 杨军顾静苒祁冰严政王东何琨张斌李真泽
Owner SINOPEC SHANGHAI ENG