Browsing by Subject "Gefriertrocknung"

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Beschreibung und Optimierung der Vorgänge der dynamischen Gefriertrocknung
(2018) Pliske, Roland; Kohlus, Reinhard
Freeze-drying is a gentle but also time-consuming drying method. One reason for the longer drying times is the formation of a dry layer during drying, which is a heat and mass transfer resistance. One approach for reducing the drying time is removing these resistances. The detail of an approach to remove the dry layer within a special powder mixer has been investigated. The process of freeze-drying while agitating has been termed ‘dynamic freeze-drying’. The used mixer was a plow-share type, in which the dry layer is actively rubbed-off permanently during the drying process. In this process the drying always takes place on the moister particle surface. This corresponds to the characteristics of a constant drying rate period, which can be considered confirmed by independent dynamic freeze-drying experiments. Freeze-drying process typically do not show a constant drying rate period. The drying front retreats immediately at the start of drying into inside of the particle. Therefore, drying rate of dynamic-freeze drying could be increased. The drying rate can be furthermore increased applying higher heating temperature in the case of dynamic freeze-drying compared to static freeze-drying. The danger of a collapse is prevented by abrasion of the dry layer during dynamic freeze drying. It has also been shown that under identical drying conditions, dynamic freeze-drying has an up to tenfold faster drying rate compared to conventional, static freeze-drying. One reason for this is a higher conductive heat flux into the bed. Another reason is the conversion of the kinetic energy into heat energy during the mixing of the bed, which is additionally used for the sublimation. Since the dry layer is removed during dynamic freeze-drying, the advantage should lie by larger initial diameters, because there are greater heat and mass transfer resistances compared to smaller initial particle diameters. This effect is overcompensated by the number of particles that are present if the same initial mass will be used for creation smaller particles than bigger particles. The contact number of particles to mixer wall determines the heat transfer by conduction and particle to particle determines the heat transfer by friction. For this reason, the drying time of the dynamic freeze-drying of smaller diameter beds is always lower. All results indicate that the number of contact points of particles to the mixer wall and other particles is relevant for the energy transfer to the bed during dynamic freeze-drying. As the particles become smaller during the drying process, however their number remains constant, and so is the effective heat transfer coefficient. A positive effect on drying rate was determined for the dried powder, which is within the mixer during the drying process. While drying with low rotational frequency less dried powder was discharged from the mixer and the experimental drying times always were lower than the modeled ones. The powder is heated at the mixer wall and is then afterwards reintroduced into the bed. At high rotational frequencies the powder is fluidized up more intensively and discharged with the water vapor from the mixer. During the drying process the water vapor leaves the mixer and partially the dried final product, too, and the load decreases and the energy input as well. Freeze-drying covers a large part of microorganism conservation so called starter culture conservation. First trials in using dynamic freeze-drying for this application have been conducted. Dynamic freeze-drying has been used in the drying of microorganisms in order to compare the viable count and the activity of the dried microorganisms with those from static freeze-drying. The presented results show that the viable count of the dynamic freeze-dried microorganisms is reduced. The activity however is partly higher than that of static freeze-dried microorganisms, which indicates a stress activation. These results were found using starter cultures that were frozen without adding "protective medium". Whether trials using protective medium will show similar results is currently unclear. The phenomenon of stress activation has to be confirmed using a large variety of lactic acid bacteria.