Method for producing high-purity sec-butyl alcohol through joint of fixed bed and reaction rectification

A fixed-bed reactor, reactive distillation technology, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., can solve the problem of low conversion rate, achieve stable product quality and improve production Scale, the effect of improving the hydrolysis conversion rate

Inactive Publication Date: 2018-05-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the problem that the conversion rate is not high in the existing sec-butyl acetate fixed-bed hydrolysis technology, the invention provides a method for the joint production of high-purity sec-butanol by fixed bed-reactive distillation, its reaction conditions are mild, sec-butyl acetate The hydrolysis conversion rate can reach more than 82%

Method used

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  • Method for producing high-purity sec-butyl alcohol through joint of fixed bed and reaction rectification
  • Method for producing high-purity sec-butyl alcohol through joint of fixed bed and reaction rectification
  • Method for producing high-purity sec-butyl alcohol through joint of fixed bed and reaction rectification

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Effect test

Embodiment 1

[0031] The feed molar ratio of sec-butyl acetate to water is 2, the fixed bed temperature is 110°C; the reflux ratio of the reactive distillation column is 2, and the operating pressure is 0.2MPa; the operating pressure in the vacuum distillation column is 5kPa, and the reflux ratio is 2 ; The operating pressure in the pressurized rectification tower is 0.6MPa, and the reflux ratio is 2.

[0032] In this example, the hydrolysis conversion rate of sec-butyl acetate was 71.55%, the purity of sec-butanol was 99.97%, and the yield of sec-butanol was 91.23%.

Embodiment 2

[0034] The feed molar ratio of sec-butyl acetate to water is 5, the fixed bed temperature is 110°C; the reflux ratio of the reactive distillation column is 8, and the operating pressure is 0.3MPa; the operating pressure in the vacuum distillation column is 10kPa, and the reflux ratio is 5 ; The operating pressure in the pressurized rectification tower is 1.0MPa, and the reflux ratio is 5.

[0035] In this example, the hydrolysis conversion rate of sec-butyl acetate was 82.91%, the purity of sec-butanol was 99.97%, and the yield of sec-butanol was 95.52%.

Embodiment 3

[0037] The feed molar ratio of sec-butyl acetate to water is 5, the fixed bed temperature is 110°C; the reflux ratio of the reactive distillation column is 10, and the operating pressure is 0.5MPa; the operating pressure in the vacuum distillation column is 50kPa, and the reflux ratio is 8 ; The operating pressure in the pressurized rectification tower is 1.3MPa, and the reflux ratio is 8.

[0038] In this example, the hydrolysis conversion rate of sec-butyl acetate was 83.37%, the purity of sec-butanol was 99.93%, and the yield of sec-butanol was 96.77%.

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Abstract

The invention discloses a method for producing high-purity sec-butyl alcohol through joint of a fixed bed and reaction rectification. Water and sec-butyl acetate are adopted as raw materials, preliminary catalytic hydrolysis is performed in a fixed bed reactor, further catalytic hydrolysis is performed in a reactive distillation column, a sec-butyl alcohol is generated, then, oil-water separationand three-step transformation rectification of decompression, pressurization and decompression are performed, and the high-purity sec-butyl alcohol is obtained. The reaction conditions are mild, the sec-butyl acetate hydrolysis conversion rate is high, and the byproduct acetic acid can be recycled for sec-butyl production.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a fixed-bed-reactive distillation combined method for producing high-purity sec-butanol. Background technique [0002] Sec-butanol is an important organic intermediate in the chemical industry, mainly used for the preparation of methyl ethyl ketone, in addition, sec-butanol can also be used as mineral processing agent, surfactant, antioxidant, etc. At present, the methods for producing sec-butanol include n-butene catalytic hydration, hydrogenation, transesterification, hydrolysis and so on. Wherein, the hydrolysis method is to use a solid acid catalyst such as a cation exchange resin to catalyze the hydrolysis of sec-butyl acetate and water to generate sec-butanol. With the maturity of the process of producing sec-butyl acetate through the addition of acetic acid and n-butene, the production capacity of sec-butyl acetate has increased year by year, but in recent yea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/00C07C31/12C07C29/09C07C29/80C07C29/76C07C29/86C07C51/09C07C51/44C07C51/42C07C51/48C07C53/08
CPCC07C29/095C07C29/76C07C29/80C07C29/86C07C51/09C07C51/42C07C51/44C07C51/48C07C31/12C07C53/08Y02P20/10
Inventor 李玲邱挺曾志杰廖雅霏韩云溪杨金杯叶长燊王晓达黄智贤王红星林小城杨臣陈锦溢王清莲
Owner FUZHOU UNIV
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