A refining method and device for esterification synthesis of n-propyl acetate

A technology of n-propyl ester and refining method, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., which can solve the problems of complex extraction and separation process steps, difficult rectification and separation, and low purity of products , to achieve the effects of improving energy utilization, reducing the types of azeotropes, and simplifying the process

Active Publication Date: 2016-11-23
JIANGSU NINE HEAVEN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] What the present invention aims to solve is: the azeotrope existing in the refining method of n-propyl acetate esterification synthesis makes rectification and separation difficult and the problem of low product purity; and the steps in the extraction and separation process are complicated and need to add new The problem of low purity of components and products

Method used

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  • A refining method and device for esterification synthesis of n-propyl acetate
  • A refining method and device for esterification synthesis of n-propyl acetate
  • A refining method and device for esterification synthesis of n-propyl acetate

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Embodiment 1

[0056] The refining method of n-propyl acetate esterification synthesis, the device used is as figure 1 As shown, the operation process comprises the following steps: the crude product obtained by the esterification tank is sent to the esterification tower from the bottom of the tower in the vapor phase, and the n-propyl acetate is initially separated by rectification in the esterification tower, and the unreacted The raw materials are returned to the esterification tank from the bottom of the esterification tower to continue the reaction, and the crude ester composed of n-propyl acetate, water, and part of n-propanol is evaporated from the top of the esterification tower. In the above process, the amount of catalyst used is 0.5% of the weight percentage of the raw material acetic acid, the molar ratio of the raw material acetic acid and propanol is 1.5:1, and the temperature is controlled at 60°C; when the equilibrium of the esterification tower is established, the temperature...

Embodiment 2

[0062] The refining method of n-propyl acetate esterification synthesis, the device used is as figure 1 As shown, the operation process comprises the following steps: the crude product obtained by the esterification tank is sent to the esterification tower from the bottom of the tower in the vapor phase, and the n-propyl acetate is initially separated by rectification in the esterification tower, and the unreacted The raw material returns to the esterification kettle from the bottom of the esterification tower to continue the reaction, and the crude ester composed of n-propyl acetate, water, and part of n-propanol is steamed from the top of the esterification tower; 0.5%, the molar ratio of raw materials acetic acid and propanol is 1.5:1, and the temperature is controlled at 60°C; when the equilibrium of the esterification tower is established, the temperature of the tower bottom is controlled at 105°C, and the gas phase temperature at the top of the tower is 85°C. After being...

Embodiment 3

[0068] The refining method of n-propyl acetate esterification synthesis, the device used is as figure 1 As shown, the operation process comprises the following steps: the crude product obtained by the esterification tank is sent to the esterification tower from the bottom of the tower in the vapor phase, and the n-propyl acetate is initially separated by rectification in the esterification tower, and the unreacted The raw material returns to the esterification kettle from the bottom of the esterification tower to continue the reaction, and the crude ester composed of n-propyl acetate, water, and part of n-propanol is steamed from the top of the esterification tower; 0.5%, the molar ratio of raw materials acetic acid and propanol is 1.5:1, and the temperature is controlled at 60°C; when the equilibrium of the esterification tower is established, the temperature of the tower bottom is controlled at 105°C, and the gas phase temperature at the top of the tower is 85°C. After being...

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Abstract

The invention relates to a refining method and device for n-propyl acetate esterification synthesis. The refining method comprises the following steps: feeding a crude product obtained in an n-propyl acetate reaction section into an esterification tower, performing preliminary separation on the n-propyl acetate in the esterification tower through a rectifying mode, and evaporating out raw ester consisting of the n-propyl acetate, water and part of n-propyl alcohol from the tower top of the esterification tower; after condensing the raw ester through a tower-top condenser, feeding the condensed raw ester into a tower-top layering machine for layering, refluxing a lower-layer water-phase part to an esterification tower, completely extracting and feeding an upper-layer organic phase into a pervaporation membrane separator to perform separation, so as to obtain dehydrated raw ester; enabling water and a little n-propyl acetate in a solution at a feed liquid side to penetrate through the pervaporation membrane in the form of steam, so as to obtain a penetrating fluid, and returning the penetrating fluid to tower-top layering machine of the esterification tower and discharging the layered penetrating fluid from the water phase; re-feeding the dehydrated raw ester into a refining tower to obtain a n-propyl acetate finished product. According to the refining method, the recovery rate is high, the process is simple, the safety coefficient is high, the feed liquid circulation volume is small, the operation energy consumption is low, and a third component is not added.

Description

technical field [0001] The present invention relates to a refining method and device for esterification synthesis of n-propyl acetate, in particular to a method for synthesizing n-propyl acetate from refined acetic acid by pervaporation and esterification of n-propanol, belonging to the application field of pervaporation membranes . Background technique [0002] N-propyl acetate is a fine chemical raw material. As a mild and quick-drying agent, it is used in flexographic printing inks and gravure printing inks, especially in polyolefin and polyamide film printing. N-propyl acetate is also used as a solvent for nitrocellulose, chlorinated rubber, and heat-reactive Bakelite. It has a slightly fruity aroma and is therefore also used in spices. [0003] In the traditional process of esterifying acetic acid and n-propanol to synthesize refined n-propyl acetate, the n-propyl acetate, n-propanol, water and a small amount of acetic acid obtained in the n-propyl acetate reaction s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/48
CPCC07C67/08C07C67/48C07C67/52C07C67/54C07C69/14
Inventor 郭海超余从立庆祖森
Owner JIANGSU NINE HEAVEN HIGH TECH
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