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Esterification reaction-pervaporation membrane separation integrated method for producing methyl 3-hydroxypropionate

A technology of pervaporation membrane and hydroxypropionic acid, which is applied in chemical instruments and methods, separation/purification of carboxylic acid esters, preparation of organic compounds, etc., and can solve the problem of combined membrane technology that has not involved 3-hydroxypropionate reaction, etc. problems, to achieve the effects of small membrane area, increased yield, and improved production process

Inactive Publication Date: 2013-04-03
NANCHANG UNIV
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  • Application Information

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Problems solved by technology

[0009] The esterification reaction-pervaporation membrane integration technology mentioned in the above-mentioned documents is used for either butyl acetate or ethyl lactate or isoacetate at a higher reaction temperature or at a higher ratio of the membrane area to the volume of the reaction solution. The esterification reaction of liquid raw materials such as propyl ester has not been involved in the application of combined membrane technology in the esterification reaction of the production process of 3-hydroxypropionic acid

Method used

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  • Esterification reaction-pervaporation membrane separation integrated method for producing methyl 3-hydroxypropionate
  • Esterification reaction-pervaporation membrane separation integrated method for producing methyl 3-hydroxypropionate
  • Esterification reaction-pervaporation membrane separation integrated method for producing methyl 3-hydroxypropionate

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Embodiment 1

[0023] see figure 1 , 3-Hydroxypropionic acid methylation reaction-pervaporation membrane separation integrated process flow is:

[0024] Preparation of binary reaction liquid of 3-hydroxypropionic acid and methanol→esterification reaction→pervaporation membrane separation→termination of methyl esterification reaction. The method of the invention starts from the 3-hydroxypropionic acid raw material, undergoes an esterification reaction-pervaporation membrane separation and integration process, and finally obtains high-purity methyl 3-hydroxypropionate liquid for the production of 3-hydroxypropionic acid.

[0025] exist figure 2 The esterification reaction-pervaporation membrane separation is performed in the experimental setup of the shown integrated process. Take 80 mL of methanol (density 0.792 g / mL), inject it into a three-necked flask with a stirrer and a reflux condenser, turn on the stirrer, and then inject 82 g of 3-hydroxypropionic acid (methanol and 3-hydroxypropio...

Embodiment 2

[0030]According to the operation of Example 1, wherein, only changing the effective membrane area of ​​the pervaporation membrane and the reaction liquid volume ratio is 0.063cm -1 , the vacuum on the downstream side of the membrane was 600pa. When the methyl esterification reaction ended, HPLC analysis showed that 93.86% of the 3-hydroxypropionic acid in the reaction solution was converted into 3-hydroxypropionic acid methyl ester, and 152mL of light yellow 3-hydroxypropionic acid was obtained. Methyl propionate solution.

Embodiment 3

[0032] According to the operation of Example 1, wherein only the mass ratio of methanol to 3-hydroxypropionic acid is changed to 1.04, and the vacuum degree downstream of the membrane is 650 Pa, HPLC experiments show that 97.2% of 3-hydroxypropionic acid in the reaction solution is converted into 3-hydroxypropionic acid acid methyl ester. 149 ml of a pale yellow methyl 3-hydroxypropionate solution are obtained.

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Abstract

The invention relates to an esterification reaction-pervaporation membrane separation integrated method for producing methyl 3-hydroxypropionate. The method comprises a process of performing esterification reaction between methanol and 3-hydroxypropionic acid to generate methyl 3-hydroxypropionate, wherein the process comprises the following steps: (1) mixing 3-hydroxypropionic acid and methanol in an esterification reactor, heating, then adding a catalyst, and reacting; and (2) pumping the obtained reaction solution into a pervaporation membrane separation device, dewatering the reaction liquid through the membrane, circularly returning the reaction solution into the esterification reactor, and further performing esterification reaction, thus obtaining the high-purity methyl 3-hydroxypropionate product after the esterification reaction is completed. According to the method provided by the invention, the area of the used membrane is small, the raw material solution / catalyst mass ratio and the reaction temperature are low, the purity and yield of methyl 3-hydroxypropionate can be greatly increased, the process is simple, and the course is stable. Thus, the invention can be easily used in the large-scale production of methyl 3-hydroxypropionate.

Description

technical field [0001] The invention relates to the application of pervaporation membrane technology in the esterification industry, in particular to a method for producing methyl 3-hydroxypropionate by adopting an esterification reaction-pervaporation membrane separation integration process. Background technique [0002] 3-Hydroxypropionic acid (Chemical Index Number (CAS) 503-66-2, formula C 3 h 6 o 3 , chemical structure HOCH 2 CH 2 COOH, molecular weight 90.08), is a three-carbon achiral organic acid, which is isomers with lactic acid, and is an important platform compound that has emerged in recent years. It is colorless, odorless, oily liquid at room temperature, miscible with water, alcohol, ether and other solvents, and can be widely used in the production of coatings, adhesives, water treatment chemicals and personal care products; it can also be dehydrated to produce acrylic acid, oxidized Formation of malonic acid, esterification to form esters, reduction to ...

Claims

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Application Information

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IPC IPC(8): C07C69/732C07C67/08C07C67/48
Inventor 朱建航余振中张帆
Owner NANCHANG UNIV
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