ChemicalBook CAS DataBase List Isobutyl isobutyrate

Isobutyl isobutyrate synthesis

13synthesis methods

Product Name:Isobutyl isobutyrate
CAS Number:97-85-8
Molecular formula:C8H16O2
Molecular Weight:144.21

By catalytic reaction passing vapors of isobutyl alcohol over CuO + Al2O3, ZnO + Al2O3, or CuO + ZnO + Al2O3 at 350 to 400°C under pressure

78-83-1 Synthesis

78-83-1
753 suppliers
$14.00/5mL

79-31-2
429 suppliers
$17.00/25mL

97-85-8
264 suppliers
$21.00/25mL

Yield:97-85-8 99.8%

Reaction Conditions:

with 1-butyl-3-methylimidazolium hydrogen sulfate at 80; under 760.051 Torr; for 3 h;Reagent/catalyst;Temperature;

Steps:

1 Example 1
Test according to the flow chart in Figure 1,3 mol of isobutyric acid,2.5 mol of isobutanol and 16.5 mol of ionic liquid1-butyl-3-methylimidazolium hydrogensulfate is added to the esterification reactor,The esterification reactor is heated to 80 ° C,The reaction was stirred at normal pressure for 3 hours, and the stirring speed was 1000 rpm.After the reaction, the reaction liquid is introduced into a decanter to be subjected to static phase separation.The rest time is 3h.The upper liquid (ester phase) and the lower liquid (aqueous phase) obtained after phase separation in the decanter are respectively introduced into the flash tank 1 and the flash tank 2 to carry out product ester purification and raw materials (mainly ionic liquid, carboxylic acid and Alcohol) recovery. The operating pressure of the flash tank 1 is 0.01 bar, and the operating temperature is 70 ° C.A product having a mass fraction of 99% isobutyrate isobutyrate was taken from the top of the flash tank 1That is, a high-purity ester, an ionic liquid having a mass fraction of 99.99% is produced at the bottom; the operating pressure of the flash tank 2 is 0.01 bar, the operating temperature is 150 ° C, and the unreacted raw material is taken from the top of the flash tank 2 and A mixture of aqueous and esters, with an ionic liquid having a mass fraction of 99.99%. The ionic liquid obtained at the bottom of the flash tanks 1 and 2 is respectively exchanged to the heat exchanger toAfter 80 ° C, it was returned to the esterification reactor for recycling. The mixture produced at the top of the flash tank 2 is introduced into an alcohol recovery column, and the actual number of plates in the alcohol recovery column is 20.The operating pressure is normal pressure and the operating reflux ratio is 4.5.The unreacted alcohol is obtained from the top of the alcohol recovery tower, and is cooled to 80 ° C by a heat exchanger, and then returned to the esterification reactor for recycling. The material of the alcohol recovery tower is introduced into the carboxylic acid recovery tower, the actual number of plates of the carboxylic acid recovery tower is 16, the operating pressure is normal pressure, the operation reflux ratio is 2.5, and the by-product water is obtained at the top of the acid recovery tower, and finally realized. The water is removed from the esterification reaction system, and the acid recovery tower tray is used to obtain a mixture containing unreacted carboxylic acid and a part of the product, which is cooled to 80 ° C by a heat exchanger and returned to the esterification reactor for recycling. The yield of isobutyl isobutyrate in Example 1 was 99.8%, and the purity was 99%.

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 0072; 0073; 0074; 0075; 0076; 0077-0093

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