FACULTY OF CHEMICAL ENGINEERING

PROFESSIONAL ACADEMIC SCHOOL OF CHEMICAL

ENGINEERING
FORMATIVE RESEARCH REPORT I
COURSE:
TREATMENT AND FOOD CONSERVATION
ISSUE:
L
Y
O
P
H
CYCLE: I
VIII
MEMBERS: L
 Argomedo Reyes, María.

I 

Barreto Álvarez, Jonathan.
Cabrejos Rodríguez, Humberto.
 Chávez Espinoza, Angélica.
SEMESTER:
Z 2019 – 2

A
T
I
O
 N

LYOPHILIZATI

I. DEFINITION
ON
Freeze-drying, dehydrofreezing or cryo-drying, is a dehydration process
generally used to preserve a perishable food or make the material more
convenient for transportation. Freeze drying works by freezing the material and
then reducing the surrounding pressure to allow the water frozen in the material
to sublime directly from the solid phase to the gas phase, bypassing the liquid
state. To accelerate the process, freezing-sublimation cycles are used to
eliminate practically all of the free water contained in the original product, but
preserving the molecular structure of the freeze-dried substance. It is mainly
used in the food industry to preserve food and in the pharmaceutical industry to
preserve medications. It is a fairly expensive and slow technique when
compared to traditional drying methods, but it results in higher quality products,
since, by not using heat, it largely avoids nutritional and organoleptic losses. (1)
At the end of the freeze-drying process, the food becomes a rigid structure that
retains its shape and volume but with reduced weight, preserving its nutritional
and organoleptic characteristics. By rehydrating it, the original texture, aroma
and flavor will be recovered. (2)

Source: https://www.restauracioncolectiva.com/n/conceptos-basicos-sobre-la-
liofilizacion-process-ventajas-y-aplicaciones-

II. EVOLUTION OVER TIME

The artificial freeze-drying process was developed in 1906 by Arsène
d'Arsonval and Frédéric Bordas in France. It sounds paradoxical to talk about
freeze-drying as a scientific advance, since the Incas used it for some centuries
to preserve the potatoes they grew. The ancient Inca empire was crossed by an
extensive network of roads stretching hundreds of kilometers. It was essential to
have nutritious food that the citizens and the Inca armies could carry during
their extensive journeys and that could be preserved for long periods of time.
The Incas took advantage of the freezing nights and low temperatures of the
highlands to freeze the potatoes at night and later, thanks to the heat of the sun
and the low atmospheric pressures, this ice was transformed directly into
steam. The Chuño or Inca freeze-dried potato was one of the great discoveries
of that civilization, it allowed us to obtain an easily consumable product up to 10
years after the process. There is also evidence that Freeze-Drying was used by
the Vikings to preserve herring and other types of fish that they consumed
during their sea voyages through Europe.
The true development of freeze-drying technology that made its application in
industry possible occurred in the 1940s. As is known, at that time humanity was
immersed in the Second World War, and it was precisely the need to cure the
countless victims of this tragedy that drove the development of many scientific
advances that we enjoy today. In short, freeze-drying was developed during the
war as a method of preserving blood plasma and penicillin, so that these
products arrived in perfect condition from the production centers to the war
front.
Fortunately, wars are not the only drivers of scientific advances. One of the
great challenges that arose in the space race was that of food. Obviously the
astronauts had to eat, but food weighs a lot, takes up a large volume and could
cause some toxic infection to the crew, something that could be fatal under
these conditions. To solve these three problems in one fell swoop, freeze-drying
technology was perfected in the late 1950s and applied to food. In this way,
light, low-volume and safe foods were obtained. We can also enjoy this
advance today in our daily lives, for example when you drink instant coffee or a
packet of soup.
Since 1960, more than four hundred types of freeze-dried foods have appeared
in stores; The best known is freeze-dried coffee. Since then, freeze-drying has
been used as a preservation or processing technique for a wide variety of
products, applied to food processing, pharmaceutical products and diagnostic
kits, but also to the restoration of documents damaged by water, to the
preparation of sludge from river bottoms for hydrocarbon analysis, to the
manufacture of ceramics used in the semiconductor industries, to the
production of synthetic leathers, to the manufacture of vials coated with sulfur,
among others. (3)

Source: flickr.com/photos/todoslosantos/601185780

III. HOW IS FREEZE-DRYING ACHIEVED?

Drying is achieved through the sublimation of water, which is the phase change
from solid to gas. This is obtained by subjecting the product to pressure and
temperature conditions lower than those of the triple point (point where the
three states of matter coexist). , since below this the liquid phase does not exist.
In the case of water the triple point is at 4.58 Torr and 0.008°C. That is why by
slightly increasing the temperature of the product under these pressure
conditions, the ice sublimes. (4)
 IV. WATER PHASE DIAGRAM

Source: https://cimaindustries.com/wp-content/uploads/assets/pdf/es/alimentos/
liofilizacion_alimentos.pdf

V. CONSIDERATIONS IN LYOPHILIZATION
To ensure that the food retains its properties, it is frozen at a faster speed than
that of a conventional refrigerator, down to -20º C in a maximum of 3o minutes.
Subsequently, two drying processes are carried out in a vacuum pump and at a
constant temperature. Despite being an expensive process, it facilitates the
storage and preservation of food for at least 12 months.
Freeze drying removes at least 95% of water from food, and the industry uses it
mainly for fruits such as strawberries, bananas or blackberries; vegetables such
as carrot, broccoli and cauliflower; meats, cheeses and coffee.
We must also know that freeze-drying is not the same as dehydrating, although
they can be used synonymously, one of the differences between freeze-drying
and dehydrating is the nutrients that are lost. When a food is dehydrated,
vitamins and minerals are lost in the process; Vitamins A and C are the first to
be broken down. The weight is not the same either; Dehydrated foods are
heavier because they have a greater amount of water. (5)
 Source: https://www.fortouladn.com/pages/que-es-la-liofilizacion

VI. GENERAL PARTS OF A FREEZE FILIZATION EQUIPMENT

Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/
Ficha_03_Liofilizados.pdf

DRYING CHAMBER: The dryer chamber serves the freeze-drying

process through the following functions:
 Provide a clean and sometimes sterile environment for the
process.
 Measure and regulate the temperatures and pressures
necessary to freeze and dry the product.
CONDENSER: The main function of the condenser is to remove
condensable vapors before they enter the vacuum pumping system. (6)

VACUUM SYSTEM: The vacuum system, as shown in the following

figure, is connected to the condenser chamber and its function is to
provide the necessary pressures for the desired primary and secondary
phases. The two main features of a vacuum system that require
consideration are the piping communicating with the condenser and the
nature of the vacuum pump.
 INSTRUMENTATION: The instrumentation associated with lyophilizer is
of great importance. Achieving an optimal product requires a control
system that reproduces the freeze-drying process, as long as it is within
the limits of equipment, and a data collection system that verifies the
consistency of the process. (6)

Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/
Ficha_03_Liofilizados.pdf

VII. FREEZE DRYING SYSTEM

The freeze-drying system described corresponds to conventional freeze-drying
equipment; which are manufactured by many companies that provide this
technology. They are achieved on laboratory, pilot or industrial scales. The
following table specifies the characteristics of each one: (2)

Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/
Ficha_03_Liofilizados.pdf

VIII. INFORMATION ABOUT FREEZE-DRYING AND ITS PROCESSES

During freeze-drying, ice crystals are sublimed directly, without transition to the
liquid state. The final product is called freeze-dried. Freeze drying in the
pharmaceutical industry is carried out as a batch process.

PROCEDURE: The freeze-drying equipment normally consists of two

tanks. The chamber and condenser tanks are joined by means of an
intermediate valve. The product to be dried is on heatable and coolable
surfaces and freezes under atmospheric pressure. Coils are mounted in
the condenser through which refrigerant or cold brine directly circulates.
(7)
PRIMARY DRYING: In the primary drying step, the water contained in
the product is sublimed. This is based on the principle that water also
has a high enough vapor pressure, when frozen, to go directly from
frozen to gaseous state. To do this, a vacuum is created. During
sublimation energy is absorbed. Since this energy is obtained from the
ambient temperature, the temperature of the supporting surfaces would
drop during the process. To maintain a constant temperature, as much
heat as the water can absorb in the form of sublimation energy is added
 to the support surface. During the drying process, the atmosphere in the
chambers consists almost exclusively of water vapor that precipitates as
ice on the cold coils of the condenser. (7)
SECONDARY DRYING: In the subsequent process, secondary drying
occurs, in which more water absorbed by the product is eliminated
through subsequent heating. Cooling of the supporting surfaces is
carried out by means of heat exchangers that are connected to the
primary cold system, refrigerant can be supplied directly into the
condenser. Condenser temperatures are typically between -75°C and
−90°C. Condenser defrosting is carried out with steam under vacuum. (7)

IX. DIFFERENCES BETWEEN CONVENTIONAL DRYING AND

FREEZE DRYING
Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/
Ficha_03_Liofilizados.pdf

X. BASIC FREEZE DRYING SYSTEM:

BASIC FREEZE-DRYING SYSTEM: The sequence of the subsystems of a

freeze-drying equipment is as follows:

 working chamber
 Plate system
 Vacuum system
 Refrigeration system
WORK CHAMBER: It is the space where the entire freezing, sublimation
and dehydration process of the product will take place. (8)
PLATE SYSTEM: It is the compartment in which the trays with the
products that are going to be subjected to the freeze-drying process are
placed. (8)
VACUUM SYSTEM: It is one of the most important to be able to develop
the freeze-drying of any product, since it is responsible for extracting the
greatest possible amount of water contained in the product. (8)
REFRIGERATION SYSTEM: a vapor compression system can be used
like that found in household refrigerators, which is made up of a
compressor, condenser, evaporator and throttle valve. (8)

XI. FREEZE FILIZATION EQUIPMENT

There are different forms of dehydration and consequently several types of

freeze dryers. A first classification considers continuous and stationary
operating equipment. According to the heat transmission mechanism, they are
divided into equipment based on conduction, convection, infrared and dielectric.
Any freeze-drying equipment fundamentally consists of five essential elements:

THE FREEZING SYSTEM : obtaining a product with adequate

characteristics to be able to be processed later depends on it. For
products of plant origin, freezing is done by immersion in cold fluids
(cold air tunnels) or in cold metal bands.
THE VACUUM SYSTEM: whose function is to evacuate the drying
chamber of the vapors produced without allowing the food to defrost.
THE CONDENSATION SYSTEM: the three most common methods of
removing water vapor are:
 Direct and indirect contact capacitors
 Dehydrating agents
 Bomb of void.
Indirect contact condensers offer an optimal arrangement to eliminate
water on an industrial scale. They are refrigerant coils equipped with an
automatic defrosting system in order to keep them free of ice, so that
their condensation capacity is maintained. The condensation surface
may be placed within the drying chamber or in a separate chamber. The
water vapor condenses and forms a layer of ice on the cooled surface
and is removed intermittently so the condenser prevents the return of
water vapor to the product.
THE HEATING SYSTEM: is where the latent heat of sublimation is
supplied. It can be by electrical resistance, heating by circulation of a hot
liquid or radiant heat. The heating plates on which the frozen material is
placed can be hollow and steam is admitted into them when heated.
MEASUREMENT AND CONTROL SYSTEM: the measuring
instruments must be distributed so that the temperature in the heating
plates, the product, in the condenser and the pressure in the drying
chamber, in the condensation chamber and in the vacuum system.
Freeze dryers are characterized by the method used to deliver calories
to the surface of the food. The most commonly used systems are
conduction and radiation. Microwave heating lyophilizers are currently
being developed (convection heating is unimportant, given the relative
vacuum in the lyophilization chamber). There are versions of each type
of freeze dryer with discontinuous and continuous operation. In batch
installations, the product is placed in an airtight freeze-drying chamber
and the temperature is initially maintained at 100-120°C, subsequently
 reducing gradually throughout dehydration (6-8 hours). The appropriate
conditions for freeze-drying depend on the food, but its surface
temperature should in no case exceed 60°C. In continuous freeze-drying
systems, the entrances and exits of the trays are carried out through
safety doors. The trays circulate, placed on heating plates, in cars that
circulate on rails through different heating zones of a chamber that is
maintained under vacuum. The heating temperatures and the time spent
in each zone are previously programmed for each food and a
microcomputer measures and controls the freeze-drying time,
temperature, pressure in the chamber and the temperature on the
surface of the product. (9)

XII. FREEZE FILIZATION EQUIPMENT

a) CONTACT LYOPHILIZERS:
The food is placed in compartmentalized trays that rest on heating
plates. In these installations, freeze-drying is slower, since the heat is
transmitted by conduction through only one side of the food, as seen in
Figure 5, where the contact between the food to be frozen and the
heating surface is uneven, which reduces the rate of heat transfer. On
the other hand, a pressure drop also occurs in the food mass, which
causes differences between the freeze-drying speed of the upper and
lower layer. The speed at which the steam moves (approximately 3 m/s)
causes smaller particles to be dragged. In compensation, the freeze-
drying capacity of this type of installation is higher. (10)

b) ACCELERATED LYOPHILIZERS:
In these installations, between the food and the heating layers, there is a
metal mesh. This makes heat transfer faster than through continuous
plates and steam is removed from the surface of the food more easily,
which reduces freeze-drying time. (10)

c) RADIATION LYOPHILIZERS:
In these installations, the food distributed on trays in thin layers is
heated by radiation. This heating system is more uniform than
conduction, since the irregularities of the food surface here have less
influence on the rate of heat transfer. Furthermore, there is no pressure
drop in the mass of the food, so the freeze-drying conditions remain
constant. As the steam velocity is approximately 1 m/s, there is no risk of
entrainment of smaller particles. On the other hand, there is no need for
intimate contact between the food and the heating surface, so flat trays
can be used, which are cheaper and easier to clean. (10)

d) DIELECTRIC AND MICROWAVE HEATING FREEZE FILIZERS:

Dielectric and microwave heaters have potential application in freeze-
drying but have not so far been used for this purpose in industrial
facilities. Microwave freeze-drying is a difficult process to control since
the water loss factor is higher than that of ice and if at any point in the
food the ice were to melt, a chain reaction of overheating would be
caused. (10)
 Source: Siccha, Ana; Lock from Ugaz, Olga. Freeze drying. Chemistry
Magazine. Volume IX N°2. December, 1995.

XIII. APPLICATIONS OF FREEZE DRYING :

This method is mainly used in:

 The pharmaceutical industry.
 The medical industry (serums, antigens and enzymes).
 To obtain animal plant extracts, antibiotics and vitamins.
 For the creation of vaccines, lactic bacilli.
 For the conservation of archaeological remains.
 For the recovery of files and documents.
 Preserve flowers and plants. (11)
 Coffee, tea and other extracts.
 Dyes, pigments.
 Vegetables, fruits, prepared meals. (12)

Source:
https://coolvacuum.es/liofilizacion-farmaceutica/lyopharm/

Source: https://tecnoagro.com.mx/no.-125/liofilizacion-de-alimentos
 XIV. APPLICATIONS IN THE FOOD INDUSTRY

Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/Ficha_03_Liofilizados.pdf

By means of freeze-drying, more than 95% of the water contained in a food can be
extracted, which translates into a great benefit in relation to the cost of transportation,
since it allows a greater quantity of merchandise to be loaded without the need for a
cold chain (it is achieves a more microbiologically stable product).
Foods can be freeze-dried in different formats: cubes, shredded, strips, chopped,
granulated or powder, and then they can be used as industrial ingredients in the
manufacture of snacks, instant soups, sauces, broth powders, broth cubes, cup
noodles. , instant puree, risotto mixes, seasonings for "Lamen", among others.
At the end of the freeze-drying process, the food becomes a rigid structure that retains
its shape and volume, but with reduced weight, preserving its nutritional and
organoleptic characteristics. By rehydrating it, the texture, aroma and original flavor will
be recovered. (13)
Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/Ficha_03_Liofilizados.pdf

XV. CHARACTERISTICS OF THE FINAL PRODUCT :

• Optimal stability.
• Easy, fast and complete solubility.
• Unlimited conservation.
• Good protection against harmful external influences.
• Quick availability of use. (14)

XVI. BENEFITS :

• The product maintains its aroma, flavor and nutrients for as long as possible.
• Instant rehydration.
• Low weight for easy handling and transportation.
• No need for refrigeration during transportation and storage.
• Long shelf life due to removal of 95%-99.5% of water.
• Little loss of activity of the ingredients.
• Small decrease in the volatility of chemicals, nutrients and heat-sensitive
components.
• With minimal changes in properties, since the effect of the growth of microorganisms
and enzymes cannot be exerted at low temperatures. (14)

XVII. IMPORTANCE IN THE FOOD INDUSTRY

Freeze-drying is of utmost importance for the conservation of food products because:

• Stops the growth of microorganisms (fungi, mold and others).
• Inhibits deterioration due to chemical reaction (change in color and flavor, rancidity,
loss of nutritional properties).
• Facilitates distribution and storage (the weight of the product decreases by up to 90%
and it is not necessary to maintain a cold chain).
• Additionally, it has two other notable virtues: the treated product does not change
shape and is easily re-hydratable.
This significant cost has relegated it to the production of medicines or foods of high
specific value, such as prawns, instant soluble coffee, rations for mountaineers and
other highly demanding sports, military rations and for astronauts. In recent years, the
use of freeze-dried foods (pieces of meat and vegetables) combined with other heat-
dehydrated foods has increased to produce instant soups and sauces at more
affordable costs. (14)
 XVIII. ADVANTAGES AND DISADVANTAGES OF THE FREEZE-DRYING
PROCESS

The main advantage of this technique is the superior quality of the final product.
However, given the cost of the process, freeze-drying is generally reserved for
products with high added value, similar to pharmaceutical products or baby food
and certain species. One of the causes of this high cost is the longevity of the
processed product. Indeed, the low pressure of the process and the weak
conductivity of the freeze-dried products (due to the porous texture) significantly
and negatively affect the heat and mass transfer and consequently the duration
of the dehydration operation. Currently, several laboratory and pilot plant scale
studies are being carried out in order to obtain a better understanding of the
details of freeze drying.
Several advantages over the freeze-drying process were reported: it prevents
thermal damage, volatiles other than water are retained, the product is
reconstituted, and shrinkage is negligible. And how disadvantages were
reported: long processing times, high energy consumption, high initial
investment cost, high price of the final product.
In summary, it offers such important advantages as the conservation and easy
transportation of products, the absence of high temperatures, the inhibition of
the growth of microorganisms, or the recovery of the properties of the food by
adding the volume of water that it originally had. (13)

Source: http://www.alimentosargentinos.gob.ar/contenido/sectores/tecnologia/Ficha_03_Liofilizados.pdf
 XIX. FEATURED FREEZE-DRIED INDUSTRIES :
There are several companies worldwide dedicated to freeze-drying:
 LioBras (drugs and food) in Brazil.
 Commercial Freeze Dry (food) in the UK.
 HULL an SPIndustries brand (drugs) in the United States.
 Botanique Preservation, Inc (botanical material and taxidermy) in the
United States.
 Nutripac S. TO. in Brazil, Argentina and Mexico (drugs, food).
The LIAL plant uses supersonic steam jets to create vacuum, an idea that failed
in the English food industry in the '60s, but which they were able to successfully
revive thanks to our nuclear technological origin. (15)

Source:
https://www.academia.edu/25497
591/Liofilizaci
%C3%B3n_de_alimentos

The door to the huge vacuum

chamber of the LIAL plant about to close. This Gaiman installation has been so
effective, simple, robust and economical that INVAP is beginning to export
similar turnkey installations. (15)

Source:
https://www.academia.edu/254975
91/Liofilizaci
%C3%B3n_de_alimentos
IN PERU:
PROCESADORA AGROINDUSTRIAL LA JOYA SAC (Arequipa) is a
company dedicated to the cultivation, dehydration and freeze-drying of all types
of vegetables and aromatic herbs with more than three years of presence in the
market.
 PRODUCTS:
Freeze-dried: Parsley, Basil, Leek, Chinese Onion, Thyme, Jalapenos,
Dill, Oregano, Pineapple, among others.

Dehydrated: Parsley, Basil, Leek, Chinese Onion, Oregano, Culantro,

Kion, Tomato, Pepper, Lucuma, among others. (16)

Source: https://procesadoraagroindustrial.com/planta/
LIOFILIZADORA DEL PACÍFICO SRL is a company with 30 years of
experience in the market of freeze-dried and dehydrated products, especially
vegetables, fruits, aromatic herbs, and medicinal plants. They have been
exporting to Japan for 30 years, to the same customer, 25 years to Europe
through a single distributor in Germany; has been in the United States market
for 20 years through two main clients and has 12 years of experience in
medicinal plants. The industrial plant is located in the Constitutional Province of
Callao, close to the airport. (17)

Source: https://1110-pe.all.biz/
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%C3%B3n_de_alimentos.
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