Chapter 8

Freeze Drying

Freeze drying enjoyed a recent burst of popularity due to the success of breakfast
cereals containing freeze-dried berries, such as strawberries, raspberries, and blue-
berries. Every major cereal manufacturer either had such products or was about
to introduce them. According to the Wall Street Journal of May 15, 2003, fruit-
containing cereals were the most successful product innovation since sugar-added
cereals in the early 1950s.
The recent success of freeze-dried fruit was due, in part, to better packaging
of the cereal. Freeze-dried strawberries were introduced in breakfast cereal in the
1960s, but they were very expensive and gradually became soggy as they picked
up moisture. Improved packaging helps prevent that moisture pickup. Also, cereals
in general have become more expensive, and the manufacturers are making smaller
packages, so the berries have less time after a package is opened to pick up moisture.
There are also freeze-dried entrees aimed at the backpacking and survival mar-
kets. The products are freeze dried as complete products, rather than mixed from
components, because it is believed that this approach retains better flavor and rehy-
dration characteristics.

8.1 Freeze Drying Basics

Freeze drying, or lyophilization, is a preservation process most often associated with
coffee, pharmaceuticals, food for space travel, and food for backpackers. It yields
a high-quality, lightweight, and easily rehydrated product that retains the original
shape of the starting material, unlike conventional drying, in which shrinking and
surface hardening can occur.
Freeze drying uses sublimation, the direct conversion of ice to vapor, to remove
water from the starting material. Sublimation of water ice occurs below the triple
point, which is about 4.5 mmHg water vapor pressure and about 0◦ C. At or below
these conditions, ice becomes vapor without passing through a liquid state. The
solids retain their shape, and the vaporizing ice leaves open pores behind. In conven-
tional drying, the water is liquid and the solids are soft and collapse upon removal
of the water, causing shrinkage. Soluble solids also can migrate to the surface

J.P. Clark, Case Studies in Food Engineering, Food Engineering Series, 67

DOI 10.1007/978-1-4419-0420-1_8,  C Springer Science+Business Media, LLC 2009
68 8 Freeze Drying

with water and create impervious surface layers, or case hardening, which impedes
rehydration.
Because freeze drying takes place at low temperatures, volatile flavors are
retained better than in conventional drying, as is color. Freeze-dried fruits look much
like the fresh item and rehydrate quickly in milk or in the mouth, releasing a sur-
prising burst of flavor.
Freeze drying can occur at atmospheric pressure and used to be commonly
observed when housewives put wet laundry on outside lines during winter. Typi-
cally, the wet clothes would eventually dry but be stiff, as if still frozen. The low
humidity of a cold day could fall below the triple point, and the sun would provide
the energy needed for sublimation.
Ernest Hemingway once wrote about a freeze-dried tiger carcass found high on
an African mountainside, and freeze drying is still used to preserve biological spec-
imens and even whole animals. Freeze-dried microbial cultures can remain viable,
and freeze-dried proteins are used as therapeutic and diagnostic agents (Goldblith
et al. 1975, Mellor 1978).
Normally, freeze drying occurs under vacuum in an attempt to enhance mass
transfer of moisture from the drying material. Often, the limiting rate is actually
that of heat transfer. External heat transfer is usually limited by the surface temper-
ature of the material – if this is too high, local melting may occur or there may be
discoloration. As material dries, the ice front shrinks away from the surface, leaving
a porous and insulating layer of dried material. This becomes the limiting resistance
for internal heat transfer.
Research at the University of California at Berkeley in the late 1960s and early
1970s (King 1970, Clark and King 1968) showed that the presence of gas such as
nitrogen or helium in the pores of the dried layer could enhance heat transfer in
some materials. The low level of gas increased the apparent thermal conductivity of
the porous layer, compared to that seen when the pores were completely empty. Too
much gas could impede water vapor transfer, so there is an optimum total pressure
for freeze drying, which depends on the material but often is higher than the pressure
used in normal practice.
The energy of sublimation is a little more than the heat of vaporization of water
and can be supplied to the surface by radiation or conduction. In the low pressures
usually used, convective heat transfer is not very effective because there is essen-
tially no atmosphere.
Water must be removed by exhausting the vapor with a vacuum pump or ejector
or by condensing the vapor to ice. The condenser temperature must be below the
ice temperature in the drying material for water to move from the material. Non-
condensable gases (residual air) are removed by vacuum pump or ejector.

8.2 Equipment Innovations

One of the major suppliers of commercial freeze-drying equipment offers both batch
and continuous freeze dryers with several novel features.
8.3 Other Freeze-Dried Materials 69

All of the company’s dryers use radiant heating from hollow metal platens
(shelves) heated with hot water. Not having direct contact with the heating surface
provides more uniform heating of the product, compared to trays sitting directly on
platens. Trays almost always have irregularities, which makes direct contact non-
uniform; thus, the temperature of the platen must be limited to prevent melting or
scorching. Many batch freeze dryers utilize trolleys to insert and remove trays of
product from the cabinet. This minimizes product handling and equipment cleanup
labor.
The larger batch dryers feature a Continuous De-Icing (CDI) system, which uti-
lizes two condensers, cooled by ammonia refrigerant, within the cabinet. One con-
denser is in communication with the product, while the second is closed off and
slightly warmed to melt the accumulated ice. The melting condenser is only slightly
elevated in pressure over the operating chamber. The low pressure is regenerated by
cooling the condenser prior to its being put back into service.
A similar system called dry condensing can be used in edible oil refining to
condense evolved steam and free fatty acids to a more concentrated waste stream
than that produced by steam stripping with steam eductors.
Continuous freeze-drying systems use airlocks to introduce and remove trays
of material to and from the vacuum chamber. The trays are pushed along tracks
between heated platens. The CDI system is also used. Most of the units around the
world (none in North America) are used to freeze dry coffee. Concentrated coffee is
prepared, frozen, granulated, sorted by size, and then placed onto trays for drying.
Equipment capacity is quoted in water removal capability and ranges from 3,300 to
16,000 kg/24 h. Corresponding costs are $4–$10 million, excluding the refrigeration
system.

8.3 Other Freeze-Dried Materials

Herbs, vegetables, and fruits are freeze dried as food ingredients. Examples are
chives, parsley, and basil.
A recent development is high-ORAC blends for health foods. ORAC, an acronym
for oxygen radical absorbance capacity, refers to the ability of foods or nutrients to
protect the human body against free radical damage and to the antioxidant power of
foods such as fruits and vegetables.
Some other innovative foods are freeze-dried salami as a crisp snack and infused
nutraceuticals in fruits and vegetables. Compressed freeze-dried vegetables and
fruits have been components of military rations. In this process, products are freeze
dried, then slightly moistened to make them flexible, compressed to reduce density,
and dried again. It is not an inexpensive process.
A novel continuous freeze dryer, developed by a coffee company, had a chamber
13 ft in diameter and 70 ft long. It used a vibratory conveyer to move frozen coffee
granules under radiant heaters. Unfortunately, it had a tendency to make a fine coffee
powder, by breaking the granules, that was indistinguishable from that made by
spray drying at much lesser cost, so it was scrapped.
70 8 Freeze Drying

Domestic freeze dryers face competition from international sources, as do many

other food segments. Because many freeze dryers are batch operations, there is
labor involved in loading and unloading, as well as in preparation and pack-
aging. Regions with low labor cost thus have some advantage. On the other
hand, freeze-dried items have low bulk density and so incur high shipping costs.
Also, precisely because freeze drying is such a good preservation process, it is
best to use the highest-quality raw material possible. Freeze-dried materials are
very hygroscopic because of their low water content and must be packaged with
care.

8.4 Examples

1. My Ph.D. thesis resulted in a US Patent (King and Clark 1969), which syn-
thesized results from other researchers in our group on the thermal and diffu-
sive properties of turkey meat in freeze-drying conditions. (The research was
sponsored by the US Department of Agriculture from a budget directed at better
utilization of poultry.) There were several concepts to the invention:

• Operate at a slightly elevated absolute pressure to optimize internal heat

transfer
• Use molecular sieves as a moisture removal means
• Circulate an inert gas, such as helium or nitrogen, to transfer heat to the surface
of the meat pieces
• Use the heat of adsorption of water vapor on the desiccant to supply the heat
of sublimation
• Choose the sizes of meat pieces and desiccant so they could easily be sepa-
rated.

Molecular sieves are synthetic minerals with precisely sized pores and large
surface areas, which selectively adsorb water and also find use as catalysts in
chemical reactions. They have higher moisture adsorption capacity than many
other desiccants, such as silicon dioxide.
My experiments demonstrated that the process worked and that our relatively
simple mathematical model accurately predicted the results. The patent was the
first issued to people in that academic department for graduate research; many
more, of course, have been issued since. So far as I knew, no one ever applied
the invention in practice, though I did hear that it may have been used in Japan.
Consider why a patent assigned to the US government might not be used
industrially. What might have been some good applications for the invention?
Hint: we learned later that some classified research had developed a similar pro-
cess in which frozen droplets of suspended bacterial cultures were mixed with
silica gel under vacuum to yield a viable bacterial powder with some potential
for use in biological weapons.
8.4 Examples 71

What might be some barriers to application? Hint: the freezing points of foods
depend on the soluble solids content with the result that fruits, having high sugar
content, freeze at lower temperatures than do meats.
2. Write the equations for heat transfer from the environment to the surface of the
food, for heat transfer from the surface to the retreating ice front, and for the
corresponding transfer of water vapor through the dry layer and then to the con-
denser, or moisture sink. What are some of the simplifying assumptions that can
make these equations relatively easy to solve? (It is easy to make them hard to
solve!) Here are some of the assumptions that have actually been used.
• Simple geometry (infinite slab, cylinder, sphere)
• No adsorption of water vapor on dried layer surfaces
• Uniform transport properties (properties actually are dependent on direction
of the grain in meat)
• Uniformly retreating ice front
• Equilibrium at the ice front (Water vapor pressure is pure component vapor
pressure at ice temperature. The Clausius-Clapyron Equation correlates water
vapor pressure with the reciprocal of absolute temperature.)
• Thermal conductivity of frozen core is so much larger than that of the dried
layer that the core can be assumed to be at a uniform temperature.
If you can, use the equations to estimate drying times for a range of foods.
You may need to consult the reference literature for relevant physical properties.
(Giving the reader a motivation to learn how to find physical properties of foods
is one reason they are not provided here. This is a necessary skill for the food
engineer.)
3. In the freeze drying of pharmaceuticals, such as purified therapeutic proteins,
the normal procedure is to deposit a precise amount of solution or suspension in
a glass vial and then loosely place a rubber stopper in the top of the vial. The
vials are placed in trays and the trays placed on hollow shelves through which
a cold fluid circulates to freeze the contents. The chamber is closed, a vacuum
is drawn and a hot fluid is circulated through the shelves. Evolved water vapor
is removed by a vacuum pump past a refrigerated condenser. When the drying
is complete, the shelves are moved closer together, forcing the rubber stopper
closed, the vacuum is relieved, the chamber is opened, and the trays removed.
Consider some of the issues that apply to this application. The filling is done
in a clean room. What is a clean room? How is it maintained? (A clean room
is classified by the number of fine particles suspended in a cubic meter of
air – 1, 10, 100, 1,000, etc. This is achieved by maintaining laminar flow of air
from the ceiling to the floor and passing all air through high-efficiency filters
(HEPA filters).) It is expensive to circulate the large volumes of air and to main-
tain the filters. How would you minimize these costs? The major resistance
in freeze drying under these conditions is the passage of water vapor past the
loosely fitted rubber stopper. What can be done about that? How much ice will
build up in a typical run, say from 5,000 vials each holding 20 ml of a 5% solu-
tion? How big should the condenser be? It is common for each batch to take 48 h
72 8 Freeze Drying

to dry. What is the motivation, if any, to optimize freeze drying times of these
often very valuable materials?
4. Consider again the production of entrees for backpackers, boaters, and military
rations. These are dishes such as beef stew, chicken and rice, shrimp curry, and
chili. The usual practice is to formulate these in a kettle, fill into trays, freeze,
either in the chamber or separately, and then freeze dry under vacuum, typically
overnight. The dry slab is broken up into small pieces and these are filled into
pouches and sealed. Alternatively, the slabs can be cut into portion-sized pieces
and then these are packaged. Consider some of the issues that might, and proba-
bly do, arise in this process. Examples are as follows:

• Production of fines (How can you minimize them? What can you do with
them?)
• Different drying rates of large and small pieces and of different materials
• Handling of fragile slabs and cut pieces
• Size reduction of slabs
• Getting slabs out of trays
• Consistency in filling of solids.

There are many others you can probably imagine. Discuss the benefits and
challenges of another approach, in which components, such as meat pieces, sauce
droplets, and vegetables, would be separately freeze dried and then combined, per-
haps by a multi-shot fill into each pouch. (Multi-shot fill means that several different
components are deposited separately into a container rather than being mixed and
then filled.)
In this approach, freeze-drying conditions for each component could be sep-
arately optimized. However, that would require a chamber for each or a provi-
sion for storing the ingredients until all were ready. Mixing separate components
with widely varying particle sizes is sure to experience segregation and, since the
pieces are fragile, there will be breakage and fines generation. Multi-shot filling
avoids some of these issues but requires additional capital in the form of additional
fillers.

8.5 Lessons

1. Freeze drying is more expensive than conventional drying, but it gives a superior
product.
2. Compared to conventional drying, it is relatively easy to model mathematically,
and the insights from doing so can often be transferred to other applications.
3. Both mixtures and individual components are freeze dried, and there are good
reasons for each.
8.5 Lessons 73

4. Multi-shot filling can be a solution to the packaging of mixtures with a wide

range of particle sizes.
5. Because of the high value of some freeze-dried products, there is rarely any great
concern over reducing cycle times to save operating costs. It is more important
to increase yield, prevent losses, and preserve quality.