Method and device for synthesizing ethyl lactate by using vapor permeation dehydration technology

A technology of ethyl lactate and osmotic dehydration, which is applied in the separation/purification of carboxylic acid esters, preparation of carboxylic acid esters, chemical instruments and methods, etc., can solve the problem that lactic acid cannot be recycled and reused, the amount of evaporation cannot be accurately controlled, and ethyl lactate Solve the problems of high water content in ester products, and achieve the effects of low organic matter content, high dehydration efficiency and short reaction time

Inactive Publication Date: 2016-12-14
JIANGSU NINE HEAVEN HIGH TECH
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Problems solved by technology

The production process does not do dehydration treatment, the conversion rate is low in the reaction process, and there are many side reactions
On the other hand, due to the high water content in the kettle liquid, during the refining process, after ethanol is distilled off, a part of ethyl lactate will produce lactic acid, and this lactic acid cannot be recycled and reused.
In the process of distilling water out under reduced pressure, the amount of distilled water cannot be accurately controlled, resulting in a large loss of ethyl lactate and a low yield
The ethyl lactate product obtained by this method has a high water content, and after a long storage time, the quality of ethyl lactate will decrease, affecting normal use
At the same time, the added value of ethyl lactate currently on the market is low, and the cost of the process is relatively high, and the benefit is relatively low

Method used

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  • Method and device for synthesizing ethyl lactate by using vapor permeation dehydration technology

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Experimental program
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Effect test

Embodiment 1

[0029] Such as figure 1As shown, 2.5kg of lactic acid (water content about 20%) was put into the reactor, and after vacuum distillation, the amount of distilled water was 0.4kg. After cooling slightly, 3.65L of absolute ethanol and 0.04kg of catalytic resin were put into it. After heating, the esterification reaction is carried out under the catalysis of the catalyst. The temperature in the reactor is 85~90°C, and the temperature at the top of the rectification column is controlled at about 76°C. The height of the rectification column is 0.8 m and the diameter of the column is about 37 mm, the rectification column is filled with 3 mm × 0.5 mm glass spring packing. The rising steam and the descending reflux liquid in the reactor conduct heat and mass transfer in the rectification column, part of the overhead distillate is used as the reflux liquid with a reflux ratio of 1.5, and the other part is used as the raw material liquid for the steam permeation dehydration process, eva...

Embodiment 2

[0031] like figure 1 As shown, 4kg of lactic acid (water content about 20%) was put into the reactor, and after vacuum distillation, the amount of distilled water was 0.53kg. After cooling down slightly, add 6.67L absolute ethanol and 0.032kg (accurately measured) concentrated sulfuric acid. After heating, the esterification reaction is carried out under the catalysis of the catalyst. The temperature in the reactor is 85~90°C, and the temperature at the top of the rectification column is controlled at about 76°C. The height of the rectification column is 0.8 m and the diameter of the column is about 37 mm. , the rectification column is filled with 3 mm × 0.5 mm glass spring packing. The rising steam and the descending reflux liquid in the reactor conduct heat and mass transfer in the rectification column, part of the overhead distillate is used as the reflux liquid, and the reflux ratio is 2, and the other part is used as the raw material liquid for the steam permeation dehyd...

Embodiment 3

[0033] like figure 1 As shown, 3kg of lactic acid (water content about 20%) was put into the reactor, and after vacuum distillation, the amount of distilled water was 0.45kg. After cooling down slightly, add 4.6L absolute ethanol and 0.024kg (accurately measured) concentrated sulfuric acid. After heating, the esterification reaction is carried out under the catalysis of the catalyst. The temperature in the reactor is 85~90°C, and the temperature at the top of the rectification column is controlled at about 76°C. The height of the rectification column is 0.8m and the diameter of the column is about 37 mm. , the rectification column is filled with 3 mm × 0.5 mm glass spring packing. The rising steam and the descending reflux liquid in the reactor conduct heat and mass transfer in the rectification column, part of the overhead distillate is used as the reflux liquid, and the reflux ratio is 2, and the other part is used as the raw material liquid for the steam permeation dehydra...

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Abstract

The invention relates to a method and a device for synthesizing ethyl lactate by using a vapor permeation technology and belongs to the technical fields of pervaporation membrane separation application and organic compound synthesis. The method comprises the following steps: performing reduced pressure distillation on lactic acid in a reaction kettle, and removing partial moisture in the lactic acid; adding ethyl alcohol and a catalyst according to a certain ratio, heating to a certain temperature, and enabling the reactants to mainly produce ethyl lactate and water under the catalytic action of the catalyst; performing heat transfer and mass transfer on rising vapor and descending reflux in the reaction kettle in the reaction process, distilling off the ethyl alcohol and water from the top of a rectifying column, and dehydrating by taking the distillate as a vapor permeation membrane dehydration material; carrying out distillate dehydration to obtain high-purity ethyl alcohol vapor, cooling and returning into the reaction kettle. According to the invention, the ethyl alcohol serves as a water-carrying agent, water carried in the raw materials and water produced in the reaction process can be continuously removed, the reaction is promoted to move to a direction of producing esters, the reaction conversion rate is improved, and the later water removal process is reduced.

Description

technical field [0001] The invention relates to a method and a device for synthesizing ethyl lactate using steam permeation dehydration technology, and belongs to the technical field of pervaporation membrane separation application and organic compound synthesis. Background technique [0002] Ethyl lactate is one of the important organic solvents, mainly used in spices and food. As a spice, the ester can be used to prepare rum, milk, butter, wine, fruit wine, coconut flavor essence, and used in food; it can also be used as a high-grade solvent for artificial pearls. At the same time, it is also the main organic solvent in the production of pesticides, and can also be used in coatings, inks and other fields. It is an environmentally friendly solvent with significant application prospects. In the production process, acid-catalyzed direct esterification is mainly used to produce ethyl lactate. This method directly reacts to reflux, and there is no dehydration process in the...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/54C07C67/48C07C69/68C07C51/44C07C59/08
CPCC07C67/08C07C51/44C07C67/48C07C67/54C07C69/68C07C59/08
Inventor 余从立相里粉娟郭海超纪祖焕
Owner JIANGSU NINE HEAVEN HIGH TECH
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