ETHYL STEARATE synthesis
- Product Name:ETHYL STEARATE
- CAS Number:111-61-5
- Molecular formula:C20H40O2
- Molecular Weight:312.53
Yield:111-61-5 98.7%
Reaction Conditions:
with trimethyloctylammonium methanesulfonate;toluene-4-sulfonic acid at 60; under 760.051 Torr; for 6 h;
Steps:
19 Example 19
According to the flow of Figure 1, the following processing is performed:2.5 mol of octadecanoic acid, 2.5 mol of ethanol and 0.75 mol of octyltrimethylammonium methanesulfonate-p-toluenesulfonic acidThe molten solvent (the molar ratio of trimethylcyclohexylammonium methanesulfonate to p-toluenesulfonic acid is 1:2) is added to the esterification reactor to form the ester.The reaction vessel was heated to 60 ° C, and the reaction was stirred at normal pressure for 6 hours, and the stirring speed was 1000 rpm. After the reaction, the reaction solution is introduced into the decantationThe device is statically phased and the rest time is 6h. The upper liquid (ester phase) and the lower liquid (water) obtained after phase separation in the decanterThe phase is introduced into the washing tank and the flash tank respectively to carry out product ester purification and raw materials (mainly eutectic solvents, carboxylic acids and alcohols).Received. The working pressure of the washing tank is normal pressure, the operating temperature is room temperature, and the mass fraction is taken from the top of the washing tank.97% product ethyl octadecanoate, a high purity ester, a mixture of eutectic solvent and water at the bottom, introduced into the flash tank; flashingThe tank has an operating pressure of 0.01 bar and an operating temperature of 250 ° C. The unreacted raw material is taken from the top of the flash tank and containsA mixture of water and ester with a eutectic solvent having a mass fraction of 99.99% at the bottom. Low eutectic solution obtained at the bottom of the flash tankThe agent is respectively exchanged to a temperature of 60 ° C through a heat exchanger and returned to the esterification reactor for recycling. Mixture produced at the top of the flash tankIntroduced into the alcohol recovery tower, the actual number of plates in the alcohol recovery column is 55, the operating pressure is atmospheric pressure, the operating reflux ratio is 6, and the alcohol recovery towerThe unreacted alcohol was obtained from the top, cooled to 60 ° C by a heat exchanger, and returned to the esterification reactor for recycling. Alcohol recovery towerThe material of the tower kettle is introduced into the carboxylic acid recovery tower, the actual number of trays of the carboxylic acid recovery tower is 60, the operating pressure is normal pressure, and the operation reflux ratio is operated.At 3.6, by-product water is obtained at the top of the acid recovery tower, and finally the water is removed from the esterification reaction system, and the acid recovery tower isThe kettle is obtained as a mixture containing unreacted carboxylic acid and a part of the product, and is cooled to 60 ° C by a heat exchanger to return to the esterification reaction.The kettle is recycled. The yield of ethyl octadecanoate in Example 19 was 98.7%, and the purity was 97%.
References:
East China University of Science and Technology;Qi Zhiwen;Cheng Hongye;Chen Lifang;Zeng Qian;Qin Hao CN109400476, 2019, A Location in patent:Paragraph 0127; 0128; 0129
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