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Method and device for preparing and separating sec-butyl alcohol by sec-butyl acetate hydrolysis

A technology of sec-butyl acetate and sec-butanol, which is applied in the fields of hydrolysis preparation, carboxylate/lactone preparation, chemical instruments and methods, etc., can solve the problems of tower bottom alcohol, unstable operation, and sec-butanol content that cannot reach the standard And other issues

Active Publication Date: 2019-03-19
HUNAN ZHONGCHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, because the acetic acid that the lower part of deacidification tower extracts will return the reactor of sec-butyl acetate plant to recycle, so the content of sec-butanol needs to be controlled at the bottom of the tower and cannot exceed 0.1%, and the sec-butanol content is too high, It will affect the catalyst of the sec-butyl acetate reactor, leading to catalyst deactivation, but it is often difficult to control during operation, and a large amount of alcohol often appears at the bottom of the tower, and the content of sec-butanol in the bottom material often cannot reach the standard
At the same time, in order to completely azeotrope sec-butyl acetate and sec-butanol to the top of the tower, a large amount of entrainer water needs to be added, which increases the load of the deacidification tower, resulting in higher energy consumption of the deacidification tower; If it is too large, the operation is also unstable, so that the content of sec-butanol in the material drawn from the side line is not high and the content is unstable. After being sent to the sec-butanol refining tower, the sec-butanol, sec-butyl acetate and water mixture are separated to obtain sec-butanol Alcohol is less, even can not be well separated

Method used

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  • Method and device for preparing and separating sec-butyl alcohol by sec-butyl acetate hydrolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The sec-butyl acetate raw material is mixed with water according to the mass ratio of 1:1.5 and then sent to the hydrolysis reactor, and the reaction is carried out at a pressure of 0.8 MPa and a temperature of 90° C. to obtain sec-butyl alcohol, water, acetic acid and sec-butyl acetate Mixture; The reacted mixture is sent to the sec-butanol azeotropic rectification tower for separation, and the number of theoretical plates of the sec-butanol azeotropic rectification tower is 60, and the feed inlet is arranged at the 30th theoretical plate place, and the sec-butanol azeotropic rectification tower The operating conditions of the butanol azeotropic distillation tower are: normal pressure, tower top temperature 90°C, the top of the sec-butanol azeotropic rectification tower is a mixture of sec-butyl acetate, sec-butanol and water, which enters sec-butanol after condensation Alcohol azeotropic distillation tower top reflux tank, the oil phase after stratification is refluxed...

Embodiment 2

[0041] The sec-butyl acetate raw material is mixed with water according to the mass ratio of 1:10 and sent to the hydrolysis reactor, and reacted at a pressure of 1.5MPa and a temperature of 150°C to obtain sec-butyl alcohol, water, acetic acid and sec-butyl acetate Mixture; The reacted mixture is sent to the sec-butanol azeotropic rectification tower for separation, and the number of theoretical plates of the sec-butanol azeotropic rectification tower is 75, and the feed inlet is arranged at the 37th theoretical plate place, and the sec-butanol azeotropic rectification tower The operating conditions of the butanol azeotropic distillation tower are: normal pressure, tower top temperature 110°C, the top of the sec-butanol azeotropic rectification tower is a mixture of sec-butyl acetate, sec-butanol and water, which enters sec-butanol after condensation Alcohol azeotropic distillation tower top reflux tank, the oil phase after stratification is refluxed with a mixture of sec-buty...

Embodiment 3

[0043] The sec-butyl acetate raw material is mixed with water according to the mass ratio of 1:1 and sent to the hydrolysis reactor, and reacted at a pressure of 0.6 MPa and a temperature of 60° C. to obtain sec-butyl alcohol, water, acetic acid and sec-butyl acetate Mixture; The mixture after the reaction is sent into the sec-butanol azeotropic rectification tower to separate, and the number of theoretical plates of the sec-butanol azeotropic rectification tower is 45, and the feed inlet is arranged at the 23rd theoretical plate place, and the sec-butanol azeotropic rectification tower The operating conditions of the butanol azeotropic distillation tower are: normal pressure, tower top temperature 60°C, the top of the sec-butanol azeotropic rectification tower is a mixture of sec-butyl acetate, sec-butanol and water, which enters sec-butanol after condensation Alcohol azeotropic distillation tower top reflux tank, the oil phase after stratification is refluxed with a mixture o...

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Abstract

The invention discloses a method for preparing and separating sec-butyl alcohol by sec-butyl acetate hydrolysis. The method includes the steps: (1) mixing sec-butyl acetate raw materials and water, conveying mixture into a hydrolysis reactor, and performing hydrolysis reaction to obtain mixture of the sec-butyl alcohol, the water, acetic acid and sec-butyl acetate; (2) conveying the reacted mixture into a sec-butyl alcohol azeotropic distillation tower for separation, condensing and layering a tower top product into an oil phase to obtain mixture reflux of the sec-butyl acetate and the sec-butyl alcohol; (3) conveying side draw materials of the sec-butyl alcohol azeotropic distillation tower into a sec-butyl alcohol refining tower for refining, condensing and layering the tower top product, refluxing one part of the oil phase, returning the other part of the oil phase to the hydrolysis reactor for reaction, returning a water phase to the middle of the sec-butyl alcohol refining tower,supplementing water and acquiring high-purity sec-butyl alcohol at the bottom of the sec-butyl alcohol refining tower; (4) conveying raw materials at the bottom of the sec-butyl alcohol azeotropic distillation tower into a sec-butyl acetate recovery tower for azeotropic separation, acquiring sec-butyl acetate and water mixture at the top of the sec-butyl acetate recovery tower, and acquiring high-purity acetic acid at the bottom of the sec-butyl acetate recovery tower.

Description

technical field [0001] The invention relates to a method and a device for separating sec-butanol from sec-butyl acetate hydrolysis reaction products. Background technique [0002] In the prior art, most of the techniques for preparing sec-butanol from sec-butyl acetate are to send the material after the hydrolysis reaction of sec-butyl acetate into the sec-butanol azeotropic rectification tower for separation, and the sec-butanol azeotropic rectification tower The mixture of sec-butanol, sec-butyl acetate and water is extracted from the top, and the sec-butanol is extracted from the side line and enters the sec-butanol refining tower for refining. The bottom of the tower is a mixture of acetic acid, sec-butanol, and sec-butyl acetate. separate. [0003] In the previous sec-butanol azeotropic distillation tower, in order to make sec-butanol and sec-butyl acetate azeotrope to the top of the tower, a large amount of water was added as an entrainer. Low, and no matter how much...

Claims

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Application Information

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IPC IPC(8): C07C31/12C07C29/09C07C29/82C07C29/80C07C53/08C07C51/09C07C51/46
CPCC07C29/095C07C29/80C07C29/82C07C51/09C07C51/46C07C31/12C07C53/08
Inventor 王伟华刘郁东李霁黄能武
Owner HUNAN ZHONGCHUANG CHEM
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