In order to throw light on the mechanism of freeze-drying and to obtain fundamental design for that process, experiments with market milk were carried out from the standpoint of chemical engineering research.
The experimental apparatus used are schematically shown in Fig. 1, and the results obtained are summarized as follows:
(1) As illustrated in Fig. 2, the typical freeze-drying process can be divided into four stages, namely, i) the primary stage, ii) the steady stage characterized by constant drying rate, iii) the first stage, and iv) second stage, each characterized by decreasing drying rate.
(2) As the process goes on, the frozen sample comes to be divided into two distinctive layers, i.e., the ice layer and the dried porous one, each having a temperature markedly different from that of the other, as shown in Fig. 6. (See also Fig. 12.)
(3) There is a linear relationship between the drying rate and the heating rate, as shown in Fig. 8 and by Eq. (1). In this, the heat coming from the outsystem must be considered, as it causes the experimentally observed values of the drying rate to be greater than the theoretical ones, when the heat supply is small.
(4) The drying rate per unit area is found to be constant, namely, to be independent of the area of the vessel, when the area is larger than a fixed value, 100cmcm
2 or so. On the other hand, when it is smaller than 100cmcm
2 or so, the drying rate is affected by the area of the vessel, as shown in Fig. 10.
(5) In most cases, the heat coming through the side walls of the vessel has influence on the temperature distribution in the frozen sample, and the outer said of the sample is more rapidly dried than the inner side of the sample.
Fig. 12 indicates the presumed profile of the sublimation surface, which is affected not only by the heat coming through the side walls, but by the cracks developed during the process, as well as by the thermocouples inserted in the sample.
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