Precipitation of Mandelic Acid with a Supercritical Antisolvent Process: Experimental and Theoretical Analysis, Optimization, and Scaleup
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- 作者：Á ; ngel Martí ; n ; Laura Gutié ; rrez ; Facundo Mattea ; Marí ; a José ; Cocero
- 刊名：Industrial & Engineering Chemistry Research
- 出版年：2007
- 出版时间：February 28, 2007
- 年：2007
- 卷：46
- 期：5
- 页码：1552 - 1562
- 全文大小：528K
- 年卷期：v.46,no.5(February 28, 2007)
- ISSN：1520-5045
文摘
An experimental and theoretical analysis of the precipitation of mandelic acid with a semicontinuoussupercritical antisolvent (SAS) process is presented. The experimental section comprises a study of the effectof different operating parameters on particle size, including pressure, temperature, solution concentration,and flow rates. Prismatic or needlelike particles with lengths of 30-200 
m have been obtained, withprecipitation yields between 20% and 80%. The parameter with a stronger influence on particle size istemperature, while an increase in the initial concentration allows a large increase in the precipitation yieldwith small variations in particle size. Variations in the injection velocities in the nozzle had only a minorinfluence on particle size. In the theoretical section the application of a detailed mathematical model of theSAS process to this system is discussed. The model is used for the interpretation of the different experimentaltrends and to propose the optimum process parameters. The model is also used to study the scale-up of theprocess and particularly the design of the nozzle for higher flow rates. As experimentally it has been foundthat the parameters of the nozzle do not affect particle characteristics, this discussion is focused on thedetermination of the required precipitator volume for different nozzle designs. Finally, a scaled-up processwith a 5-20 times increase in flow rates and product amount has been tested experimentally, obtaining resultssimilar to those in the lower scale experiments.
m have been obtained, withprecipitation yields between 20% and 80%. The parameter with a stronger influence on particle size istemperature, while an increase in the initial concentration allows a large increase in the precipitation yieldwith small variations in particle size. Variations in the injection velocities in the nozzle had only a minorinfluence on particle size. In the theoretical section the application of a detailed mathematical model of theSAS process to this system is discussed. The model is used for the interpretation of the different experimentaltrends and to propose the optimum process parameters. The model is also used to study the scale-up of theprocess and particularly the design of the nozzle for higher flow rates. As experimentally it has been foundthat the parameters of the nozzle do not affect particle characteristics, this discussion is focused on thedetermination of the required precipitator volume for different nozzle designs. Finally, a scaled-up processwith a 5-20 times increase in flow rates and product amount has been tested experimentally, obtaining resultssimilar to those in the lower scale experiments.