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Method for preparing sec-butyl alcohol

A technology of sec-butanol and sec-butyl acetate, which is applied in the field of preparation of sec-butanol, can solve the problems of low conversion rate, low purity, inability to separate sec-butanol and sec-butyl acetate, etc., and improve the conversion rate , the effect of meeting the material requirements

Active Publication Date: 2017-05-10
HUNAN ZHONGCHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the single-pass conversion rate of n-butene is low, only about 6%, and the requirements for raw materials are relatively strict. If the n-butene content of the C4 raw material used in the direct hydration process is greater than 90%, it may be directly hydrated to SBA, if the B-B grade fraction with lower n-butene content is directly reacted, the project cost will be increased due to its low conversion rate and high circulation rate, so extractive distillation or molecular sieve separation should be carried out first, and pre-purification should be carried out to achieve the maximum reduction. purpose of production cost
In this invention, the process is relatively long, and the obtained methyl acetate product is a crude ester product with a mass fraction of about 82% and low purity. However, in the sec-butanol refining tower, since sec-butanol and sec-butyl acetate can form an azeotrope , the boiling point of the azeotrope is 99.6 ° C, and the boiling point of sec-butanol is 99.5 ° C, so, in this column, sec-butanol and sec-butyl acetate cannot be separated well, and high-purity sec-butanol cannot be obtained basically alcohol

Method used

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  • Method for preparing sec-butyl alcohol

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Experimental program
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Effect test

Embodiment 1

[0064] The sec-butyl acetate raw material 2 is sent into the hydrolysis reactor 3 with the speed of 30t / h, wherein, the sec-butyl acetate is a commercially available product purchased, and the industrial purity is 99.54%, and water 1 is added simultaneously, wherein, water and acetic acid The molar ratio of sec-butyl ester is 1.05:1, the temperature of the reactor is 60°C, and the reaction pressure is 1.0MPa. The mixture 4 of sec-butanol, water and sec-butyl acetate obtained through hydrolysis reaction is at a speed of 34.9t / h Send into the deacidification tower 9, the deacidification tower is a plate tower, the number of theoretical plates is 60, the feed port of the deacidification tower is set at the 35th tray, and the side line of the deacidification tower is provided with 2 side reactors 7 and 11 are respectively located at the 20th and 30th theoretical plates of the deacidification tower. The reaction temperature of the control side reactor is 80°C, the reaction pressure ...

Embodiment 2

[0067]The sec-butyl acetate raw material 2 is sent into the hydrolysis reactor 3 with the speed of 64t / h, and the sec-butyl acetate raw material is obtained from Chinese patent application CN103980115A step (1) containing sec-butyl acetate, C8 olefins and unreacted acetic acid The bottom product, wherein, the mass content of sec-butyl acetate is 46.87%, the mass content of acetic acid is 43.45%, the mass content of C8 olefins is 8.63%, and the mass content of sec-butanol is 1.05%. Water 1 is added to the hydrolysis reactor at the same time, wherein the molar ratio of water to sec-butyl acetate is 0.5:1, the temperature of the reactor is 70°C, and the reaction pressure is 0.6MPa. The sec-butanol and water obtained through the hydrolysis reaction , the mixture 4 of acetic acid, C8 olefin and sec-butyl acetate is sent into the deacidification tower with the speed of 66.3t / h, and the deacidification tower is a plate tower, and the number of theoretical plates is 40, and the feed in...

Embodiment 3

[0070] The sec-butyl acetate raw material 2 is sent into the hydrolysis reactor 3 with the speed of 30t / h, wherein, the sec-butyl acetate is a commercially available product purchased, and the industrial purity is 99.67%, and water 1 is added simultaneously, wherein, water and acetic acid The molar ratio of sec-butyl ester is 1.2:1, the temperature of the reactor is 80°C, and the reaction pressure is 0.7MPa. The mixture 4 of sec-butanol, water and sec-butyl acetate obtained through hydrolysis reaction is at a speed of 35.6t / h Send into the deacidification tower 9, the deacidification tower is a plate tower, the number of theoretical plates is 50, the feed port of the deacidification tower is arranged at the 30th tray, and the side line of the deacidification tower is provided with 3 side reactors , respectively located at the 20th, 25th, and 29th theoretical plates of the deacidification tower, the reaction temperature of the control side reactor is 100°C, the reaction pressure...

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Abstract

The invention provides a method for preparing sec-butyl alcohol. The method comprises the steps of (1) mixing sec-butyl acetate and water, then putting the mixture into a hydrolysis reactor, and carrying out hydrolysis reaction so as to obtain a mixture of the sec-butyl alcohol, the water and the sec-butyl acetate; (2) after the reaction is finished, sending the obtained mixture to the lower part of a deacidification tower, and enabling separated acetic acid to fall into the bottom of the tower; (3) sending a mixture of the sec-butyl acetate and the sec-butyl alcohol to a sec-butyl alcohol refining tower, adding an entrainer water, enabling an azeotrope of the water, the sec-butyl acetate and part of the sec-butyl alcohol to be evaporated to the top of the tower, carrying out condensation and then enabling a product to be recycled back to a reaction system so as to enable most sec-butyl alcohol to fall into the bottom of the tower, and collecting the sec-butyl alcohol from the bottom of the tower to obtain a product sec-butyl alcohol. After the method is used for preparing the sec-butyl alcohol, the single-pass conversion rate of the sec-butyl acetate is 60% or above, the separated sec-butyl alcohol is high in purity, and the purity reaches 99% or higher; furthermore, the purity of the acetic acid obtained at the bottom of the deacidification tower is also higher and reaches 96% or higher; the yield of the sec-butyl alcohol separated by the method is higher and reaches 65% or above. The method is simple in process and operation, and lower in energy consumption.

Description

technical field [0001] The invention relates to a method for preparing sec-butanol, in particular to a method for preparing sec-butanol by hydrolysis of sec-butyl acetate. Background technique [0002] Secondary butanol (SBA), also known as second butanol, methyl ethyl carbinol, other butanol, 2-butanol, is a colorless, transparent, flammable liquid with a wine-like smell. SBA is used as a solvent in industry, co-solvent with methanol, can be used as a component to increase the octane number of gasoline, and can also be used to produce plasticizers, mineral dressing agents, herbicides, sec-butyl esters, etc., but the most important application is The production of methyl ethyl ketone accounts for about 90% of the total consumption. At present, the relatively mature methods in the industry include the indirect hydration method of n-butene and the direct hydration method of n-butene. The traditional process for preparing sec-butanol is sulfuric acid indirect hydration, which...

Claims

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Application Information

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IPC IPC(8): C07C31/12C07C29/09C07C29/80C07C29/82
CPCC07C29/095C07C29/80C07C29/82C07C31/12
Inventor 胡先念黄能武王坤李星肖云飞刘良会刘郁东张小明申文义
Owner HUNAN ZHONGCHUANG CHEM
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