Deodorisation

Sadanand Patel
HBTI-K
 Layout of
Presentation
Refining (Physical/Chemical)
What is Deodorization?
Effect of Deodorization
Chemistry of Odour
Sources of Odour
Principles
Laws
Process Variables
Process Steps
Operation(Batch, Semi-continuous and Continuous)
Equipment
Effect of Deodorization on Oil Quality
Losses
Newer Developments
Utilities Consumption
Deodoriser safety
 Refining
(Physical/Chemical)
OILSEEDS
Mechanical Pressing
Oil Extraction Deoiled Meal
Solvent Extraction
Crude Ol

Gums LECITHIN
Water degumming
Chemical Physical
Soapstock WDG Oil
Acid Gums Acid degumming
Alkali Neutralisation

Spent
Bleaching bleaching earth
Bleaching

Deodorizer Distillate Physical deacidification

Deodorization
Deodorization
Refined Oil
 What is
Deodorization?
This is usually the last stage of the refining process of edible oils

Quality defining process in the refining of oils to eliminate the FFA

and odoriferous substances.

Today, the process is still commonly named deodorisation, but the

objectives have become much broader than just the removal of off-
flavours.

High Temperature, High Vacuum, Live Steam Distillation Process

Distillation is a physical and not a chemical process and does not

change the molecular structure of the components
 Its
Effects
Desirable
Undesirable

Actual deodorisation by removal of Some unwanted side-reactions

different off-flavours cis-trans-isomerization,
polymerization,
conjugation, and so on

Stripping of volatile components such as:

FFA (in the case of physical
refining), Removal of valuable minor components
contaminants (pesticides, light tocopherols,
PAH etc.) sterols etc.

If the oil is not properly pretreated,

Thermal destruction of pigments (so- the oil can become darker during
called heat bleaching) deodorization. This phenomenon is
also known as color fixation
 Chemistry of
Odour

Aldehydes, Acids, Epoxides,

Hydroperoxides Ketones, Diene Dimers, Oxirane
and triene rings

Primary Secondary Tertiary

Factors Decomposition
Fats & Oils Oxidation Oxidation Oxidation
Oxidation
Products Products Products
 Sources of
Odour
Most vegetable oil retains characteristics
undesirable flavors & odors that obtain during
processing.

Peroxides (primary oxidation products),

Hydrocarbons, Aldehydes, Ketones (secondary
oxidation products), Tocopherols, Sterols, FFA
are the main odoriferous and volatile
compounds need to remove.

As a total, odoriferous components generally add

up to not more than 200 ppm.

Bleaching imparts Earthy flavors whereas

hydrogenation adds on odor and flavors that can
be described as undesirable.
 Underlying
Principle
Difference in volatilities
Aldehyde/Ketone > FFAs > Squalene >
Tocopherols > Sterols > Sterols esters >
TAGs

The degree of separation of a simple

binary mixture is expressed in terms of the
relative volatility of the two components.
The theoretical separation ratio,, is
defined as
The vapour pressure for a given
constituent is a function of the
temperature and increases with
increasing temperature (Clausius-
Clapeyron's equation)
 Laws

Whitmans two film

Dalton's Law The partial pressure theory:
describes the vapour of the single At any instant the rate of
pressure of a mixture components can be transfer of volatile
as the sum of the calculated following components from the oil
partial pressures of Raoult's law: into the steam bubble is
its single proportional to the
components difference in pressure
inside the bubble and
actual pressure in the
vessel and interfacial
area of the steam bubble.
Temperature

Pressure

Time

Stripping
Steam
Variables
Process
 Deodorization
Temperature
Temperature has its influence on deodorization because the vapour pressure is
directly proportional to it.
T Rate of removal of Volatile Substances

An increase of nx17K decreases deodorization time by the factor 2n

Increase in temperature also means that stripping steam can be reduced. This is
important in reducing entrainment losses

Short chain fatty acid deodorized at low temp and hydrogenated oil deodorized at
higher temp because of higher FFA content and distinctive odor it imparts.
Heat Bleach Effect is higher at higher temperature:
Higher Temperature is avoided because:
Insufficient thermal stability of oils
Economy of the process (high energy
consumption)
 Deodorization
Pressure

If the pressure is decreased, the temperature required

also decreases because a lower vapour pressure is then
sufficient to ensure evaporation.

Reduced pressure helps to protect the oil from oxidation

because oxygen from the air is reduced almost to zero.

The amount of distillation steam required is also directly

proportional to the pressure. If the pressure is halved
steam consumption also halves.
Higher P means more steam. More steam
means more possibility for entrainment.
And more stripping steam will increase
hydrolysis. This will increase oil losses
and lower quality
 Deodorization
Time

The time necessary to separate a certain amount of undesired

components from the oil depends mainly on the speed with which
the necessary amount of stripping steam can be introduced

Deodorization time also increases with the height of the oil in the
deodorizer, i.e., with the thickness of the oil layer that the stripping
stream has to penetrate.

Because all side reactions are also time dependent, deodorization

time is kept as low as possible. In Europe, longer deodorization time
and lower temperatures are preferred. In the U.S., the reverse is true
 Stripping Gas
A Carrier to the Undesired Components

External pressure of the gas adds to the Vapour pressure of volatiles in deodorizer and
speed up their removal.
Stripping agents with the lowest possible molecular weights are selected. In most
cases, steam is the best solution, but sometimes nitrogen is preferred.

Since the surface area of the oil is increased by bubble formation, the mass transfer
and consequently the distillation rate is increased.

The height of the oil in the vessel also influences the consumption of steam because the
steam has to work against the hydrostatic pressure to be able to penetrate the oil
before being sucked off or distilling off from its surface.
where S is the total moles of steam, V, is the initial molar concentration of the volatile
component in the oil, and V, is the final molar concentration of the volatile component in the
oil. When the initial FFA content is low, as in the case of a classical deodorization, (Va- Vo)
becomes so small that the equation can be simplified as follows:

The amount of gas required for deodorization is directly proportional to the amount of oil
and the absolute pressure in the deodorizer and inversely proportional to the vapour
pressure of the pure volatile component at the process temperature and the overall
vaporization efficiency E.
On the surface of the steam bubbles, the oil/steam contact must be maximized; there the
sparge gas has its lowest specific volume, equivalent to the highest relative surface area.
Athanassiadis (1991) postulated that 300,000 m3 was a minimum contact area of oil/steam
for every kilogram of gas injected to ensure good deodorization efficiency.
 Process
Optimization
To achieve a proper deodorization, an optimal deodorizing temperature, operating pressure,
and amount of stripping gas are required. These are determined not only by the type and state
of the oil (chemically or physically refined), but also by the deodorizer design.

Today, most deodorizers used in the refining of soft oils operate at temperatures between
230 and 26OoC, a pressure of 3 mbar or even lower, with a stripping steam consumption of
~10 kg/ton of processed oil.
Refining chemical physical

Temperature 230 250 C 240 265 C

Pressure 3 mbar 2 mbar

Sparge steam 5 15 kg/t 7 20 kg/t

Time 45 90 min 45 90 min

Final FFA 0.03 % 0.05 %

Trans-increase 0.5 1.5 % 0.7 2 %

Tocopherol retention 70 90 % 60 80 %

Source@alfalaval
 Bleached Oil Unit operations of
deodorization &
Processing Steps
Degassing

Deaeration
Heating Up Heating
Stripping
Thermal action
Deodorization
Cooling
Polishing
Cooling

Polishing

Deodorized Oil
 De-aeration
To avoid excessive oxidation and hence risk of polymerization.
Soft oils dissolve readily between 4 and 10% of their own volume of air and other
gases at ordinary temperature.
Solubility increase with increasing in temperature. The relation between solubility
(S) and temperature (t) can be expressed as:

with S (%, v/v), at normal

pressure and t in Celsius

The bleached oil is sprayed into a tank under reduced pressure. The lower the pressure applied,
the lower the residual oxygen in the oil. Usually the oil is heated to at least 80C and sprayed
into a tank, which is kept at a pressure of 40 mbar. Some refiners even use the low pressure of
the deodorizer or add some sparge steam in the spraying tank to improve deaeration.
 Heating

Heating of the oil is usually accomplished in two stages.

First stage,
Oil is heated counter-currently in an oil-oil heat exchanger (economizer), with the finished
oil leaving the deodorizer.
Second stage,
Oil is heated under reduced pressure to deodorizing temperature with a high temperature
source such as high pressure steam, heat transfer fluids. Saturated steam of -50 bar is
required to heat the oil to 240-260C.

where O is the amount of oil (kg), T1 and T2 are the incoming

and final temperature of the oil (C), C is the average specific
heat capacity of vegetable oils [typically 2.2-2.4 kJ/(kg. C)], fL is
(Heating energy required
the heat loss factor from radiation typically 1.05-1.15) and fR, is
for a deodorizing system)
the heat recovery factor [ 1 - (%heat recovery/100)].
 Stripping

It is Conducted at a temperature between 230 and 260 oC, at a pressure between 2 and 4
mbar and under injection of 0.5-2% sparging steam. From a thermodynamic point of view,
the stripping agent takes over the part of the total pressure equal to its partial pressure. As
a consequence, the vapour-liquid equilibrium is reached at a lower molar fraction, xi,
resulting in the removal of significantly more volatile substances only.
Nitrogen
- inert and non-condensable gas
- lower losses (no hydrolysis) and higher distillate quality
- more powerful vacuum system required
- profitability is very uncertain
Steam (Superheated)
- most evident choice
- Boost up the vacuum when condensed
- But support hydrolysis

The sparge gas is introduced into the oil through special steam distributors. These can be
sparge coils with very fine holes (between 0.5 and 2.5 mm) or even sintered metal pipes
 Thermal action

The oil is then held in a retention section

for a certain amount of time for thermal
treatment known as heat bleaching
that deals with undesirable pigments and
Oil Polishing
ensures the stability of the final product.
The length of time the oil is kept in the Oil polishing is done to remove any fine
retention section depends heavily on the particles of soaps , metallic salts rusts , filler
desired product specifications aids, polymerized oil or other solid
impurities. Horizontal plate filters have long
been used as polishing filters of choice for
deodorization.
Cooling
Finally the oil is cooled in two stages.
First in the economizer, and then to the
specified final temperature. It then
undergoes polish filtration and is
transferred to subsequent processes,
storage or packaging
 Processing
Options

Batch Processing

Semi-Continuous Processing

Continuous Processing

- Vertical Deodorizer
- Horizontal Deodorizer

Thin Film Technology

Packed Column Technology
Dual Temperature Technology
 Batch
Batch deodorization is especially suitable for small Process
capacities (<50 ton /day) .
Batch deodorizers mainly consist of welded
vertical cylindrical vessel with dished or conical
head and made up of 304 stainless steel to avoid
deleterious catalytic activity of Cu & Fe
Vessel diameter are chosen to the depth of 8 to 10
feet of oil and a similar amount of word space above
to avoid entrainment loss.
Steam is injected into the bottom of the vessel
Include a device to measure temperature and a
pressure gauge to indicate low pressure within
deodorizer.
 In principle, semi- Semi-Continuous
continuous deodorization Processing
is an automatically
controlled batch-wise
process.
Used when frequent
feedstock changes of oil
sensitive to cross
contamination.
Steam produced in the
bottom deodorized oil-
cooling section is sent in a
closed thermo siphon loop
to the top bleached oil
heating section to heat the
incoming oil.
Main advantage is shorter
hold up time , and
disadvantage is less heat
recovery than the
continuous process.
Continuous
Processing

Horizontal deodorizer
Continuous
Processing

Vertical deodorizer
 Steam

Demister Cooling water

VHE Final
Heater
Steam
Scrubber To hot well Vacuum system

SoftColumn
column
Packed column technology
(Alfalaval Soft column)

Cooling
High pressure water
Steam
steam boiler
Deaerator Cooling
water
Steam Acid oil

Economizer
Polishing
Cooler
Heater filters
Steam
Citric acid
Oil in Oil out
Inlet
filters
Steam
Packed column technology Continuous
(Crown Works, MaxEfficiency Processing
Deodorizing System)
 Equipment
Scrubber
Single Scrubber
Double Scrubber

Stripping Column
Horizontal Column
Vertical Column

Vacuum System
Ejector Booster
Ice Condensation
 Scrubber

Composition of vapor phase

Volatile components (FFA, odor components)
Stripping steam
Non condensable gases (air.)

The volatile substances are condensed by creating an

intimate contact between the vapor and fatty acid
distillate circulating in the scrubber.

The distillate which is circulated is at its lower possible

temperature (just above its melting point).

This highly efficient, structured packed column is

designed to condense and recover free fatty acids
(FFA) and other volatiles from the deodorization
process and to prevent carryover of these
materials to the vacuum system
 Stripping
Column

The pre-treated and heated oil flows either by gravity or under pressure from the final
heater to the distributor on the top of the column. The distributor spreads the oil evenly
over the cross-section of the column. This oil then trickles down the structured packing,
flowing as a thin layer on this extended surface until it reaches the bottom of the column.
It then continues to the next process step. The counter current flow of the steam is
achieved via a steam distributor installed in the bottom of the column or from another
source. The oil in the column meets the stripping steam in a counter current flow.
The column is under vacuum, so exposing the oil to the vacuum at a high temperature
removes volatile substances and the steam carries them out to the vacuum outlet at the
top of the column. The height of the column is a function of the number of desired
distillation steps.
Horizontal
Column
Vertical
Column
Effect of Deodorization
on Quality of Oil

Losses by evaporation
FFA are among the most easily
evaporated materials in fats and oils.
Normally reduced to below 0.03%
by deodorization.
Sterols, tocopherols and other
unsaponifiable matter may make up
a large portion of the fatty matter
are distilled from the oil.
Mono- and diglycerides which have
been produced during refining, as
they have a lower molecular weight.
Losses in
Deodorization
Losses by entrainment
Deodoriser distillate always contains
a certain amount of neutral oil
which has been mechanically
entrained from the oil.
Mechanical entrainment (carryover)
of oil by stripping steam is the main
unwanted loss in deodorization.
 Newer
Developments
 Thin Film
Technology

The first plant for large scale (250 MT/d) thin film seed oil deodorization was
started in 1996.

It had been known for some time that thin-film stripping theoretically had
considerable advantages over tray stripping. Because the steam passes over a very
thin oil film in a true counter-current operation, the contact between steam and oil
is optimized.

The surface area of the oil can be further increased by a special design of the
packed column. Other means to enhance mass transfer are eddy currents caused
by wall heat transfer in the falling film design or centrifugal action if rotating disks
are used.

However, there are still some major drawbacks,

Increased trans fatty acid level.
Removal of antioxidants and vitamins as a result of the very high effectiveness
of the operation.
Heat bleaching effect may be reduced
 Dual Temperature
Technology

These deodorisers operate at two different temperatures in order to

reach the best compromise between-
required residence time for actual deodorisation (longer time
at lower temperature) and
heat bleaching and stripping of volatile components (shorter
time at higher temperature).

The dual-temperature concept has been successfully introduced on

an industrial scale. Both the low/high temperature and the
high/low temperature concept can be applied.
 Ice Condensation
With such systems, the stripping steam Vacuum System
is condensed on surface condensers
operating alternately at very low
temperature (30 C).
The efficient sublimation of steam and
other volatile matter will give a very low
pressure in the deodoriser (<1.5 mbar)
and will strongly reduce odour emission.
Dryice condensing systems strongly
reduce the motive steam consumption
but require extra electrical energy.
Commercially available systems consist
of two or more freeze condensers with
horizontally or vertically orientated
straight tubes, a refrigeration plant for
the generation of the cold refrigerant
evaporated in the tubes and a vessel for
the defrosting and cleaning of the tubes
after a certain period of freezing.
Deodoriser distillate contains neutral oil. This refining
Dual Scrubbing
loss can be reduced by integration of a so-called neutral
System
oil recovery system (NORES) in the first part of the
scrubber section. The purpose of this system is to recover
the mechanical entrained neutral oil from the vapour
phase before the volatile matter (FFA, tocopherols, sterols,
The vapour phase leaving the deodoriser is first
partially condensed at a higher temperature, giving a so
called hot distillate in which the least volatile
components (e.g. tocopherols and sterols) are
concentrated.
Complete condensation of the remaining, more volatile
substances (mainly FFA) is then achieved in the second
so-called cold scrubber, giving an FFA-rich cold
distillate.
Provided that the condensation temperatures of the hot
and cold scrubbers are properly set, this concept gives a
very good separation between the FFA and tocopherols.
Combining NORES with a double scrubber in the
physical refining of soybean oil (for which processors
seem to have a growing preference) gives a hot
distillate with 21.2% tocopherols
 Utilities
Consumption

2 - 4 kWh depending on plant size

Electric Power: Add about 2.5 kWh for ice condensation
Steam(4 bar) 10-15kg Stripping Purpose

60 kg (with surface condensers)

Steam (10 bar) 20 kg with ice condensation

Heating Energy 105,000 kJ + 3,500 kJ/% FFA

9 m3 at T 6C
Cooling Water (30C) 4 m3 at T 6 TC with ice condensation

Citric Acid: 0.05 kg (optional as synergist)

 Deodoriser
safety

The deodoriser is operated at the highest temperature of the refining plant. The oil is
kept under non-combustible conditions, due to the absence of air in the deodoriser. A
fire hazard is possible when air is entrained in the deodoriser at high temperature.
The following preventative measures should be used to avoid this situation:

Properly maintained equipment, to avoid air leaks. Trained personnel, to identify

air leaks and react to starting fires.

Well-established procedures for start-up, shutdown and maintenance.

The high-pressure boiler develops up to 90 bar pressure. Its condition and safety
system integrity must be periodically checked.