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Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device

A technology of ethyl hexanoate and osmotic dehydration, which is used in the preparation of carboxylate, the preparation of organic compounds, the separation/purification of carboxylate, etc., to avoid secondary evaporation, simple sewage treatment, and easy system stability.

Inactive Publication Date: 2015-09-23
JIANGSU NINE HEAVEN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to overcome the problem of using the third component to remove the water generated in the reaction process in time in the synthesis reaction of ethyl caproate, and propose a coupling method of synthesis reaction of ethyl caproate and steam permeation dehydration craft

Method used

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  • Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device
  • Reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Such as figure 1 As shown, in the reactor, 1.5kg of hexanoic acid and 2.25L of absolute ethanol are subjected to esterification reaction under the catalyst of 0.0045kg of concentrated sulfuric acid. The temperature in the reactor is 80°C. At about 78°C, the height of the rectification column is 0.8 m, the diameter of the column is about 37 mm, and the rectification column is filled with glass spring packing with a size of 3 mm × 0.5 mm. The steam generated in the reaction kettle conducts heat and mass transfer with the reflux liquid in the rectification column. Part of the overhead distillate is used as the reflux liquid with a reflux ratio of 5, and the other part is used as the raw material liquid for the steam permeation dehydration process, which passes through the evaporator 6 After heating and vaporizing, it enters the membrane separation unit, and the pressure of the feed liquid side is controlled at about 0.25MPa. The membrane separation unit is composed of tw...

Embodiment 2

[0025] Such as figure 2 As shown, in the reaction kettle, 3kg of hexanoic acid and 4.5L of absolute ethanol are subjected to esterification reaction under the catalysis of 0.2kg p-toluene yellow acid catalyst, the temperature in the reaction kettle is 110°C, and the refined The temperature at the top of the distillation column is controlled at about 100 °C. The height of the rectification column is 0.8 m, the diameter of the column is about 37 mm, and the rectification column is filled with glass spring packing with a size of 3 mm × 0.5 mm. After the steam generated in the reaction kettle is partially condensed, the condensate is used as the reflux liquid, and the reflux ratio is 2. The uncondensed steam enters the membrane separation unit after being heated by the supplementary heater, and the operating pressure of the feed liquid side is about 0.3MPa. The membrane separation unit is composed of three single-tube NaA molecular sieve membrane modules connected in series, with...

Embodiment 3

[0027] Such as figure 1 As shown, in the reactor, 2kg of hexanoic acid and 1.6L of absolute ethanol are subjected to esterification reaction under the catalysis of 0.005kg of sodium bisulfate composite catalyst, the temperature in the reactor is 90°C, The temperature is controlled at about 78°C, the height of the rectification column is 0.8 m, the diameter of the column is about 37 mm, and the rectification column is filled with glass spring packing with a size of 3 mm×0.5 mm. The steam generated in the reaction kettle conducts heat and mass transfer with the reflux liquid in the rectification column. Part of the overhead distillate is used as the reflux liquid with a reflux ratio of 3, and the other part is used as the raw material liquid for the steam permeation dehydration process, which passes through the evaporator After heating and vaporizing, it enters the membrane separation unit, and the pressure of the feed liquid side is controlled at about 0.2MPa. The membrane se...

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Abstract

The invention relates to a reaction and steam osmotic dehydration coupled ethyl hexanoate synthesizing process and device and belongs to the technical field of pervaporation membrane separation application and organic compound synthesis. Hexanoic acid and ethyl ester inside a reaction still are heated to a certain reaction temperature, and then are subjected to reaction under the catalytic action of a catalyst to mainly generate ethyl hexanoate and water. Steam generated in the reaction still in the reaction process passes through a rectifying column and then is subjected to heat transfer and mass transfer with returned flow, ethyl alcohol and water are distilled off from the tower top of the rectifying column after transfer, the distillate serves as the dehydration raw material for the steam osmosis membrane, steam osmotic dehydration is conducted, and the dehydrated ethyl alcohol solution high in purity is cooled and returned to the reaction still. Under the condition of not introducing other water-carrying agents bad for the environment, water in the esterification reaction is continuously removed in the ethyl alcohol water carrying and dehydration process, the reaction is promoted to move toward the production of ester, the reaction conversion rate is increased, aftertreatment of water-carrying agents and environmental pollution are avoided, and the production cost is reduced.

Description

technical field [0001] The invention relates to an ethyl hexanoate synthesis process and device coupled with reaction and steam permeation dehydration, and belongs to the technical field of pervaporation membrane separation application and organic compound synthesis. Background technique [0002] Ethyl hexanoate is a common solvent and one of the important synthetic intermediates in the field of organic synthesis, which can be used to prepare flavors for food. The ester is a colorless liquid with koji, grape, and pineapple aromas, so it can also be used for flavoring tobacco and wine. In the production process, acid-catalyzed direct esterification is mainly used to produce ethyl hexanoate. This method usually uses benzene or toluene as a water-carrying agent. During the reaction process, it forms an azeotrope with ethanol and water and evaporates, then separates the phases and refluxes for dehydration. Benzene (toluene) and ethanol in the feed liquid in the reaction ket...

Claims

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Application Information

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IPC IPC(8): C07C69/24C07C67/08C07C67/48
CPCC07C67/08C07C67/48C07C69/24
Inventor 余从立杨龙顾学红庆祖森
Owner JIANGSU NINE HEAVEN HIGH TECH
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