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Preparation method of n-propyl propionate

A technology of n-propyl propionate and propionic acid, which is applied in the field of preparation of n-propyl propionate, can solve the problems of low catalytic effect of the catalyst, unsatisfactory products, difficult handling of by-products, etc., so as to prevent overheating and improve product quality. Stable, easy-to-control effects

Inactive Publication Date: 2018-12-04
TIANJIN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at proposing a kind of preparation method of n-propyl propionate, to solve the problems such as the existing preparation method of n-propyl propionate does not meet the requirements, the catalytic effect of the catalyst is low, the by-products are not easy to handle, and the method is simple to operate, Has good economic benefits

Method used

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  • Preparation method of n-propyl propionate

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preparation example Construction

[0028] A preparation method for n-propyl propionate, comprising the following steps:

[0029] Add excess propionic acid and n-propanol to the reactive distillation tower equipped with a catalyst, under the action of the catalyst, an esterification reaction occurs to generate n-propyl propionate, the by-product is water, and the top of the reactive distillation tower contains propionic acid Mixture of n-propyl ester and water;

[0030] The mixture containing n-propyl propionate and water is sent to the phase separator after being condensed, the water phase is extracted, the mass fraction is 0.98-0.998, part of the oil phase is refluxed, and a part is extracted to obtain n-propyl propionate product, The mass score is greater than 0.999;

[0031] Excess propionic acid is extracted from the reactor of the reactive distillation tower, the mass fraction of propionic acid is 0.92-0.94, and returned to the feedstock inlet of propionic acid of the reactive distillation tower to contin...

Embodiment

[0043] 10,000 tons / year of n-propyl propionate production, in which the raw material composition and related parameters are as follows:

[0044] Raw material propionic acid: mass fraction is 0.999, feed rate is 888Kg / h; raw material n-propanol: mass fraction is 0.999, feed rate is 600Kg / h.

[0045] The pressure at the top of the reactive distillation column is 30KPa, the temperature at the top of the column is 81.4°C, the mass ratio of reflux to propionic acid feed is 6.78, and the mass ratio of reflux to n-propyl propionate output is 5.25.

[0046] Obtain n-propyl propionate and water mixture at the top of the reactive distillation tower, through the phase separator phase separation, obtain the n-propyl propionate that mass fraction is 0.99965, and the by-product water that mass fraction is 0.9983; Propionic acid with a mass fraction of 0.9275 is extracted from the tower reactor and returned to the feed inlet of propionic acid to continue to react with n-propanol.

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Abstract

The invention provides a preparation method of n-propyl propionate. The method comprises the following steps: S1, adding excessive propionic acid and n-propanol into a reactive rectification tower provided with a catalyst, and carrying out reactive rectification to obtain a heterogeneous reaction product containing n-propyl propionate and water at the top of the reactive rectification tower; S2, conveying the heterogeneous reaction product containing n-propyl propionate and water into a phase splitter, extracting the obtained water phase, refluxing a part of the obtained oil phase, and extracting the remaining part of the oil phase to obtain n-propyl propionate; and S3, extracting propionic acid from the bottom of the reactive rectification tower, returning the propionic acid to the propionic acid raw material inlet of the reactive rectification tower, and continuously reacting the propionic acid with n-propanol. The excessive propionic acid added into the reactive rectification towermakes the n-propanol completely reacted, a gas phase obtained at the tower top is condensed and undergoes phase splitting to obtain the product n-propyl propionate and a byproduct water, and the remaining propionic acid is extracted from the tower bottom, and is reused. Reduced pressure operation is adopted to effectively reduce the reaction temperature, prevent the temperature runaway phenomenonof a catalyst and make the catalyst have a good effect; and the method has the advantages of easiness in product separation, good product quality and low device investment.

Description

technical field [0001] The invention relates to the field of chemical reactive distillation, in particular to a preparation method of n-propyl propionate. Background technique [0002] N-propyl propionate is a fine chemical with a wide range of uses. As a selective solvent, it is widely used in coatings, printing inks, fragrances, cleaning agents, food industry seasonings, etc. It can replace some aromatic hydrocarbons that cause air pollution compound solvent. With the rapid development of the world economy and the enhancement of human awareness of environmental protection, the consumption of n-propyl propionate is increasing, and the requirements for its purity are also getting higher and higher. For example, the battery industry requires more than 99.9% of its purity. [0003] The esterification reaction of propionic acid and n-propanol synthesizes n-propyl propionate, and at the same time produces water as a by-product. This reaction is a reversible equilibrium reaction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/24C07C67/08C07C67/54
CPCC07C67/08C07C67/54C07C69/24Y02P20/10
Inventor 王红星郑广强邱挺李飞刘伯潭盖晓龙
Owner TIANJIN UNIV OF SCI & TECH
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