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Method and device for preparing sec butanol

A technology of sec-butanol and sec-butyl acetate, which is applied in the field of preparing sec-butanol by double-catalyzed rectification process, can solve the problems of long process, increased engineering cost, low conversion rate, etc., and achieve energy consumption reduction, cost saving, easy The effect of the operation

Active Publication Date: 2017-03-22
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 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. 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 and device for preparing sec butanol
  • Method and device for preparing sec butanol

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Second-butyl acetate 1 is sent into primary catalytic rectification tower 6 with the speed of 6.38t / h, and methyl alcohol 5 is added simultaneously, wherein, the theoretical plate number of primary catalytic rectification tower is 25, methanol and acetic acid secondary The molar ratio of butyl ester is 1.05:1, the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 57°C, and the temperature at the bottom of the tower is 99°C. Second-butanol falls into the bottom of the tower and is recovered as product 11 at a rate of 7.77t / h , the unreacted methanol and the reaction product methyl acetate are steamed from the top of the tower, and after being condensed by the condenser 7, part of it is used as the top reflux 9 of the first-stage catalytic rectification tower, wherein the reflux ratio is 1:1, and part 12 is 7.56t / The speed of h is sent to the secondary catalytic rectification tower 14, while adding excess sec-butyl acetate 13,...

Embodiment 2

[0041] Second-butyl acetate 1 is sent into primary catalytic rectification tower 6 with the speed of 3.48t / h, and ethanol 5 is added simultaneously, wherein, the theoretical plate number of primary catalytic rectification tower is 30, and ethanol and secondary acetic acid The molar ratio of butyl ester is 1.1:1, the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 77°C, and the temperature at the bottom of the tower is 100°C. Second-butanol falls into the bottom of the tower and is recovered as product 11 at a rate of 8.14t / h , the unreacted ethanol and the reaction product ethyl acetate are steamed from the top of the tower, and after being condensed by the condenser 7, the part 9 is used as the top reflux of the first-stage catalytic distillation column, wherein the reflux ratio is 2:1, and the part 12 is 9.26t / The speed of h is sent to the secondary catalytic rectification tower 14, while adding excess sec-butyl acetate 13, the...

Embodiment 3

[0048] Second-butyl acetate 1 is sent into primary catalytic rectification tower 6 with the speed of 6.96t / h, and isopropanol 5 is added simultaneously, wherein, the theoretical plate number of primary catalytic rectification tower is 40, and isopropanol The molar ratio of alcohol to sec-butyl acetate is 1.2:1, the pressure at the top of the tower is normal pressure, the temperature at the top of the tower is 89°C, the temperature at the bottom of the tower is 99.5°C, and the sec-butanol falls into the bottom of the tower at a rate of 8.88t / h as Product 11 is taken out, unreacted isopropanol and reaction product isopropyl acetate are steamed from the top of the tower, and part 9 after being condensed by the condenser 7 is used as the top reflux of the first-stage catalytic rectification tower, wherein the reflux ratio is 3:1, Part 12 is sent into secondary catalytic rectification tower 14 with the speed of 11.4t / h, adds excessive sec-butyl acetate 13 simultaneously, and alcohol...

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Abstract

The present invention provides a method and a device for preparing sec butanol, and the method is as follows: (1) sec-butyl acetate is introduced into a first-stage catalytic distillation column, excessive C1-C3 alcohols are added simultaneously for ester exchange, the sec butanol as a product falls into a tower kettle to collect, and the unreacted C1-C3 alcohols and reaction product acetic acid C1-C3 esters partly are sent into a second-stage catalytic distillation column for further reaction separation; (2) excessive sec-butyl acetate is added into the second-stage catalytic distillation column, the acetic acid C1-C3 esters are distilled off from the top of the column, and then congealed to partly reflux to the top of the second-stage catalytic distillation column and partly use as a product to collect; and (3) the sec butanol obtained by the step (2) and the unreacted sec-butyl acetate are returned to the first-stage catalytic distillation column for further reaction separation. The purity of the sec butanol obtained by the method is high above 99.9%, the purity of the separated acetic acid C1-C3 esters is more than 99%, at the same time, the method has the advantages of simple process and easy operation, compared with the process of butylene hydration for preparing the sec butanol, energy consumption is greatly reduced, and cost is saved.

Description

technical field [0001] The invention relates to a method and device for preparing sec-butanol, in particular to a method and device for preparing sec-butanol through a double catalytic rectification process. 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 sul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/12C07C29/128C07C29/80B01D3/14
CPCB01D3/146C07C29/1285C07C29/80C07C31/12Y02P20/10
Inventor 黄能武申文义刘良会王坤孙李林刘郁东张小明
Owner HUNAN ZHONGCHUANG CHEM
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