Recrystallization of Caffeine Using Supercritical Carbon Dioxide as Antisolvent
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Joel Augusto da Silva Romero
The supercritical antisolvent (SAS) process has been widely used to obtain many types of crystalline and amorphous particles of polymers and drugs. In this process, solute particles precipitate from an organic solution when it is sprayed into a compressed antisolvent continuum. The antisolvent is miscible with the organic solvent, but immiscible with the solute. The objective of this work was to investigate the application of supercritical carbon dioxide as antisolvent for the recrystallization of caffeine; a compound largely employed in pharmaceutical and food industries. The carbon dioxide was pressurized at 100bar and the solution was injected into a precipitation chamber, thereby inducing its supersaturation and particle precipitation. The effect of process parameters such as initial concentration of caffeine in the organic solution (3, 5 and 10mg/mL), organic solution flow rate (3mL/min), concentration of CO2 (96 and 98mol%), drying flow rate (990mL/min) and pressure gradient between the precipitation chamber and the exit of the sprayer tube (110 and 220bar) on the solid state properties of caffeine was investigated. The pressure (100bar) and temperature (60oC) of the precipitation chamber were kept constant. The results showed a great difference between the processed and unprocessed samples. In all experimental conditions a reduction in caffeine mean particle size was observed, with length ranging from 0.6 to 168.3?m and width from 0.1 to 12.7?m, compared to the mean size of unprocessed caffeine particles (16.6 to 214.4?m in length and 7.1 to 131.2?m in width). This fact was confirmed by differential scanning calorimetry (DSC), where the precipitated particles presented lower fusion enthalpy than the unprocessed ones. Smaller crystal needles (0.3?m to 0.4?m) were obtained with crystallization at the lowest caffeine concentration in the presence of 98mol% CO2.
©2011 Walter de Gruyter GmbH & Co. KG, Berlin/Boston
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Articles in the same Issue
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- Editorial: Special Issue of 8th World Congress of Chemical Engineering (WCCE 8) Symposium on Process Design
- Reactive Dividing-Wall Columns - Defying Equilibrium Restrictions
- Fractal Scaling in Crude Oil Price Evolution via Time Series Analysis of Historical Data
- Effect of Sound Wave Irradiation on Methane Conversion in DC Pulse Discharge Plasma
- The Production of Polyhydroxyalkanoates Using an Oscillatory Baffled Bioreactor
- Simultaneous Coke Reduction with Improved Syngas Production during Propane Steam Reforming using Forced CO2 Cycling
- Kernel PCA Performance in Processes with Multiple Operation Modes
- A New Kinetic Model for 4-Chlorophenol Adsorption on Expanded Clay
- Uniformly Bounded Error Estimator for Bioprocess with Unstructured Cell Growth Models
- Mathematical Modeling of Drug Release from Spherical Drug Particles: Analysis of the Effect of Absorption Rate on Drug Release Rate
- Analysis on a Counter-Current Flow Hemodialyzer
- Mathematical Model of a Falling Film Reactor for Methyl Ester Sulfonation
- Oxidative Coupling of Propane with a Two-Layered Catalyst Bed Reactor
- Interval Based MINLP Superstructure Synthesis of Multi-Period Mass Exchanger Networks
- Modeling Fluid Separation Processes Using a Complementary Approach
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- Recrystallization of Caffeine Using Supercritical Carbon Dioxide as Antisolvent
- Flow Characteristics in an Airlift Membrane Bioreactor
- Design and Control of Integrated Styrene-Aniline Production Plant
