Freeze drying or lyophilization of aqueous solutions is widely used in pharmaceutical industry.The increased importance of the process is gaining a worldwide interest of research.A growing body of literature has demonstrated that the scientific approach can result in improved product quality with minimum trial and error empiricism.Formulation and process development need a systematical understanding of the physical chemistry of freezing and freeze drying,material science and mechanisms of heat and mass transfer.This paper presents an overview on freeze drying of aqueous solutions based on publications in the past few decades.The important issues of the process are analyzed.
Freeze-drying of the initially porous frozen material with pre-built pores from liquid material was found experimentally to save drying time by over 30% with an initial saturation being 0.28 compared with the conventional operation with the initial saturation being 1, using mannitol as the solid material. In order to understand the mass and heat transfer phenomena of this novel process, a two-dimensional mathematical model of coupled mass and heat transfer was derived with reference to the cylindrical coordinate system. Three adsorption–desorption equilibrium relationships between the vapour pressure and saturation value namely, power-law, Redhead's style and Kelvin's style equation, were tested. Kelvin's style in exponential form of adsorption equilibrium relation gave an excellent agreement between the model prediction and experimental measurement when the equation parameter, γ, of 5000 was applied. Analyses of temperature and ice saturation profiles show that additional heat needs to be supplied to increase the sample temperature in order to promote the desorption process. Simulation also shows that there is a threshold initial porosity after which the drying time decreased with the increase in the initial porosity. Enhanced freeze-drying is expected to be achieved by simultaneously enhancing mass and heat transfer of the process.
