SPECIAL ISSUE ORIGINAL ARTICLE
Evaluation of immersion-contact type heat transfer for
continuous pharmaceutical spin freeze-drying process
Ganeshmurthy Srinivasan | Balakrishnan Raja
Department of Mechanical Engineering, Indian
Institute of Information Technology, Design
and Manufacturing (IIITD&M), Chennai, Tamil
Nadu, India
Correspondence
Dr. Balakrishnan Raja, Department of
Mechanical Engineering, Indian Institute of
Information Technology, Design and
Manufacturing (IIITD&M) Kancheepuram,
Chennai 600 127, Tamil Nadu, India.
Email: rajab@iiitdm.ac.in
Funding information
Science and Engineering Research Board,
Grant/Award Number: SR/S3/
MMER/0005/2014; Department of Science
and Technology (DST-SERB), India, Grant/
Award Number: SR/S3/MMER/0005/2014
Abstract
Spin freeze-drying process is a recently proposed method to achieve continuous
processing of unit doses in freeze-drying application. An experimental study is carried
out to investigate the heat transfer and drying characteristics of a spin-frozen liquid
product. To enhance heat transfer, unlike freeze drying performed in shelves, the shell is
immersed into a temperature-controlled bath. The influence of different ramping condi-
tion of bath temperature on drying rate, time and variation of moisture content in spin-
frozen products (deionized water and skimmed milk) are analyzed and reported in this
paper. Among different ramping conditions, ramping of bath temperature to 10
C
resulted in higher drying rate (1.8 kg hr
-1
m
-2
) and lesser drying time (44%). The overall
heat transfer coefficient (K
v
) between the bath and product is evaluated for the above
condition in both the test liquids. This direct contact type heat transfer helps in reducing
air gap resistance and radiation effect, which primarily helps in minimizing thermal resis-
tances. The effect of dry layer resistance is minimal in the spin-frozen product due to
lower product thickness and larger ice-vapor surface area.
Practical Applications
The spin-frozen sample is dried either by using an infrared (IR) heater or by placing
on a shelf. Limitations using IR heater include positioning of the vials (the distance
between the vials and IR source) and selecting suitable IR window material and thick-
ness. In the case of the shelf, conduction resistance between shelf and vial, radiation
resistance inside the chamber and air gap resistance present between vial and shelf
plays a major role. The thermal resistance is minimal in the immersion method due to
the absence of air gap resistance and radiation effect. Hence, an alternative approach
is discussed using immersion drying method to achieve continuous vial processing
and uniformity among vials. Hence, freeze-drying process can also be shifted to con-
tinuous production mode like prefilling and packaging.
1 | INTRODUCTION
Freeze-drying is a dehydration process carried out in three consecutive
stages. In freezing stage, the water content in the product is frozen
below the eutectic temperature under atmospheric pressure. The
frozen content is sublimated and desorbed under vacuum during
primary and secondary drying stages, respectively (Cohen & Yang,
1995; Jennings, 1999; Mujumdar, 2014; Oetjen & Haseley, 2004).
The pressure–temperature diagram of freeze-drying process is sche-
matically shown in Figure 1. Batch wise freeze-drying process has
certain limitations in achieving inter-vial uniformity while handling
Abbreviations: DW, deionized water; IR, infrared; RH
(10
C)
, ramp and hold at 10
C; RH
(-5
C)
,
ramp and hold at -5
C; RH
(s)
, ramping and holding in sequence; SM, skimmed milk; X,
fraction of moisture content.
Received: 16 January 2019 Revised: 11 April 2019 Accepted: 17 May 2019
DOI: 10.1111/jfpe.13153
J Food Process Eng. 2019;e13153. wileyonlinelibrary.com/journal/jfpe © 2019 Wiley Periodicals, Inc. 1 of 7
https://doi.org/10.1111/jfpe.13153