FATTY

ACIDS
TECHNOLOGY

BASIC INFORMATION & ENGINEERING DATA

GIANAZZA
nternational
INDEX
INDEX
FATTY ACIDS TECHNOLOGY
PRETREATMENT
SPLITTING
STRAIGHT DISTILLATION
HEATING SYSTEMS
SEPARATION BY FRACTIONAL DISTILLATION
SEPARATION BY WET FRACTIONATION
HYDROGENATION
GLYCERINE RECOVERY
 FATTY ACIDS TECHNOLOGY
FATTY
ACIDS
TECH
NOLOGY
1. FATTY ACIDS TECHNOLOGY
The natural oils and fats, both of vegetable and animal origin, are worldwide used as source of FATTY
fatty acids, glycerine and their derivatives. ACIDS
The importance of fatty acids in chemical industry is well known and continuously increasing.
They are used in a very wide range of industrial applications with thousands of end-products
TECH
mainly in the following fields:
NOLOGY

Whatever the final derivate (ester, salt, alcohol, sulphate, sulphonate, amine, amide, etc) the
intermediate steps always involve the production of FATTY ACIDS, as a distilled mixture or as pure
fraction: the basic steps in fatty acids technology are shown in the previous block diagram.
GIANAZZA International has a very long and proven experience in the technology of fatty acids
and can supply most of the plants mentioned in the block diagram, that are individually
described in the next pages, namely:

“UNITOWER” fats splitting and distillation plant

Capacity: 100 t/d
 2. PRETREATMENT
PRE
TREATMENT
PURPOSE
The main purpose of pretreatment is to remove from crude fats & oils those impurities (organic
and mechanical) that cannot yield acids during splitting.
The benefits of pretreatment will be noted, at last, as a higher yield of distilled fatty acids that is
a lower loss as residues from distillation.

FEEDSTOCK
Any crude fat should be submitted to pretreatment theoretically, but, in practice, oils and fats
of very good quality are directly sent to splitting.
In case of bad quality feedstock, pretreatment is recommended.

PROCESS CONDITIONS & YIELDS

For good and medium quality feedstock, pretreatment can be avoided or reduced to simple
water washing or reaction with a weak acid.
Filtration with bleaching earths is sometimes carried out.
For lower quality fats, the most widely used pretreatment involves reaction with a strong acid
(sulphuric acid), followed by several water washings. A proper pretreatment should be capable
of removing from 80% to 90% at least of undesirable impurities.

UTILITIES & CHEMICALS REQUIREMENTS

Sulphuric acid at 96% concentration is typically used in quantities depending on the nature of
feedstock (few Kg/t).

max. per ton of fat.

3

Reduced quantities of low pressure steam (for heating and stirring) and electric energy are
also required.

MATERIALS OF CONSTRUCTION
All parts in contact with sulphuric acid are made of special reinforced resins.
When using centrifugal separators, they are made of special grade stainless steel.

PLANT CAPACITY

For higher capacities, semi-continuous or fully continuous plants can be proposed.

Oleochemicals plants (South Korea)

3. SPLITTING
PURPOSE SPLITTING
The splitting or hydrolysis reaction is carried out in order to obtain from triglycerides the
corresponding crude fatty acids and crude glycerol dissolved in the excess water.

RCOO-CH2
CH2-OH
RCOO-CH+3H2O 3RCOOH + CH-OH
CH2-OH
RCOO-CH2

FEEDSTOCK
Any triglyceride can be submitted to splitting; in industrial practice, the most widely used feed-
stock are tallow, lard, palm oil, coconut oil, palmkernel oil and acid oils from refining.
When feedstock are not of first quality, it is necessary to pretreat them in order to remove
organic impurities (gums, proteins, waxes, unsaponifiable matters) and mechanical impurities.
The process water to be used for the reaction should be fully demineralized or, at least, softened
water.
Care must be taken to avoid the presence of polyethylene in the feedstock (100 ppm max.).

PROCESS CONDITIONS
GIANAZZA International splitting plants carry out thermal splitting under pressure, with no use of
any catalyst or mechanical agitation for improving the contact between the phases.
The adopted temperatures are sufficiently high (230 to 265°C) to obtain a good mutual
dissolution of the water phase into the fat phase, so that the hydrolysis reaction takes place with
very high conversion rate.
According to the capacity, mainly, but also depending on the quality of feedstock, GIANAZZA
International can supply three different types of splitting plants:

It is a pressure splitting plant, generally

equipped with one splitting column,
completed by a seal-less recycling pump.
Operating pressures are in the range of 25
to 30 bar and operating temperatures are
from 200 to 230°C.
Generally two separate additions of
process water are carried out, in order to
reach an acceptable splitting degree.
Any kind of feedstock, even in small
quantities, can be processed in this type of
plant; quality changeovers are not a
problem.

“CONTIPERCOL” continuous fats splitting plant

 3.1 SPLITTING
SPLITTING “CONTIPERCOL” SPLITTING PLANT
The typical characteristics of this plant are summarized as follows:

continuous, counter-current percolation system using two or more columns in series through
which the fat phase is passing by overflow and the water phase is transferred by seal-less
pumps.
Typical operating pressure is 30 bar at corresponding temperature of 230°C approx. with
retention time in the range of several hours.
Heating of reactants (both fat and water) is indirect and it can easily be made by using liquid
phase diathermic fluids. So there is no need of high pressure steam.
The sensible heat of products (fatty acids and sweet waters) is entirely used to
pre-evaporate the sweet waters that can be discharged with glycerol concentration of
20% or higher.
Any type of fat can be processed.
One or more columns, if necessary, can be used batchwise for processing small batches of
particular feedstock.
Capacity from small to medium range.

“UNITOWER” SPLITTING PLANT

This plant has the following characteristics:

continuous, counter-current percolation system using one single column, whose upper part is
used for heat recovery between the incoming water and the outgoing fatty acids, while the
lower part is used for heat recovery between the incoming fat and the outgoing sweet
waters.
Typical operating pressure is 55 bar at temperature of 260°C approx. with retention time in the
range of few hours.
Higher splitting degree with reduced consumptions, but lower glycerol concentration in the
sweet waters.
Heating is carried out by means of high pres-
sure steam being lost (that is directly injected
into the splitting column).
Equipped with advanced instrumentation
for automatic control of operating condi-
tions.
Frequent quality changeover is less recom-
mended due to the required time.
Highly unsaturated fats are not recommen-
dable as feedstock (typical feedstock are
“saturated” fats such as tallow, palm oil,
coconut oil).
Typical capacities are from medium to high
range.

PRODUCTS QUALITY & YIELD

BATCH SPLITTING
The splitting degree can be in the range of 95
to 97%, but it can also be lower or higher,
according to the quality of feedstock and
operating conditions, mainly the quantity of
process water being used. “UNITOWER” continuous fats splitting plant
Glycerol in the sweet waters can be in the Capacity: 120 t/d
range of 5 to 15% according to the feedstock.
3.2 SPLITTING
“CONTIPERCOL” & “UNITOWER” SPLITTING
The splitting degree is normally in the range of 98% or more and higher when processing good
quality tallow, palm oil and lauric feedstock.
The sweet waters concentration is typically in the range of 15 to 20%. By using the flash vapours
as heating medium in an additional evaporator under vacuum, the sweet waters can be
discharged at 30÷40% glycerol content without any additional energy consumption.
As to the YIELD, the crude fatty acids yield depends on the nature of feedstock and splitting
degree: for good tallow and palm oil, the yield of fatty acids is in the range of 95 to 96% of
feedstock (94 to 95% for lauric feedstock), while the yield of glycerol is in the range of 10% (12 to
13% for lauric feedstock). From a theoretic point of view, the higher is the splitting degree the
lower is the fatty acids yield.

SPECIFIC REQUIREMENTS
The following typical approximate consumption figures can be obtained, referred to 1 ton of
crude fat (typically tallow):

CONTIPERCOL UNITOWER
Steam 4 & 13 bar 60 kg 50 kg

Steam 60 bar -- 160 kg

Thermal Energy
(through diathermic fluid) 200.000 Kcal --

Process Water, 70°C 0,75 m3 (*) 0,60 m3 (*)

Cooling Water, 25°C

(without additional evaporator) 20 m3 15 m3

Electric Energy 8 kWh 10 kWh

(*) actual consumptions of fresh water are much lower because the
recovered condensate from flash vapours are normally recycled to
the process water feed tank.

MATERIALS OF CONSTRUCTION
For the splitting columns of BATCH and “CONTIPERCOL” type plants, massive stainless steel AISI
316Ti or duplex stainless steel are used.
For “UNITOWER” column, higher grade can be used, especially when processing lauric fats, such
as AISI 317L or AISI 317LN (massive or clad).
Other parts of the plant working at lower temperatures are made of AISI 316L stainless steel.

STANDARD CAPACITIES
BATCH type plants are recommended up to 30 t/d.
“CONTIPERCOL” type is typically covering the range from 25 to 100 t/d.
“UNITOWER” type is recommended for capacities from 100 to 300 t/d.

PROCESS DESCRIPTION
The next page shows a typical flow diagram of Contipercol and Unitower splitting plant
respectively.

To be noted:
while the “Contipercol” plant can be directly heated by diathermic fluid at 270°C, the
“Unitower” plant needs 60 bar steam for heating, directly injected into the splitting column;
the “Unitower” column, in its upper part, contains a set of special plates for heat recovery
between the outgoing fatty acids and the incoming water.
 3.3 SPLITTING
SPLITTING In both systems the vapours obtained from the products flashing can be used to pre-
concentrate the sweet waters in single or multiple effect evaporators working under
vacuum.

1 - “CONTIPERCOL” continuous fats splitting plant (schematic drawing)

2 - “UNITOWER” high pressure continuous fats splitting plant (schematic drawing)
4. STRAIGHT DISTILLATION
PURPOSE STRAIGHT
Crude fatty acids from splitting contain many impurities (mainly neutral fat and unsaponifiable DISTILLA
matters) and are dark in colour, so that they must be purified in order to obtain a pure product
with light colour and good stability. TION
Distillation is adopted for obtaining this result, the impurities being separated as undistilled
residue (sometimes sent to further splitting in order to improve the yield of fatty acids).

FEEDSTOCK
Crude split fatty acids from different fats and oils are typical feedstock for straight distillation
plants.
It is recommended that feedstock has a minimum splitting degree of 96% in order to reduce
losses in the residues, but fatty acids with even lower splitting degree can be distilled, too.
The same plant can also be used for straight distillation of other fatty matters such as
methylesters and fatty alcohols.

PROCESS CONDITIONS
Standard Plant.
Due to their sensitivity to heat,
fatty acids must be distilled at
low temperature (200 to
250°C) and, therefore, under
high vacuum (5 mbar or
lower). The retention time
must be as short as possible;
important liquid columns over
the heating elements must
be avoided so that vaporiza-
tion is allowed only in high
vacuum.
Much care, therefore, must
be dedicated to the distilla-
tion column and accessories
design.

Fatty acids distillation plant - Capacity: 150 t/d

GIANAZZA International column has the following features:

reduced contact time.
Falling film evaporators are often used as heating elements (no stripping steam required).
Special heating candles with high heat transfer enabling to process any kind of feedstock
(even of low quality) are also used.
Small quantities of stripping steam improve distillation and protect the product against local
overheating.
Scrubbing of distilled vapours by liquid reflux strongly improving the colour of distillate.
Hot condensation system (assisted by controlled temperature enclosed circuit), so that the
distillate is leaving the condenser just few degrees below the boiling temperature and low
boiling products are prevented to condense.
High heat recovery, with production of low pressure steam.
Vertical design of main still, therefore space saving.
 4.1 STRAIGHT DISTILLATION
STRAIGHT MATERIALS OF CONSTRUCTION
DISTILLA Stainless steel AISI 316L grade with good resistance is generally adopted.
TION Sometimes, when handling short chain acids such as C6 to C12, special grades of stainless steel
are used, with higher molybdenum content, for parts working at temperatures higher than
200°C.

TOPPING COLUMN
In some cases (for production of particular products) it may be requested to remove, from the
fatty acids mixture, the low boiling fatty acids.
Typical cases are:
removal of C6-C10 fraction from coconut oil fatty acids in order to produce C12-C18 cut.
Removal of fatty acids up to C14 from tallow fatty acids in order to produce C16-C18 cut.

This problem is solved by using a fractiona-

ting column (TOPPING COLUMN) also
working under vacuum, in addition to the
standard main still.

STANDARD CAPACITY
Fully continuous plants are designed for
capacities from 20 to 300 t/d.
Higher capacities can be designed for
special cases.

PRODUCTS QUALITY & YIELD

The straight distilled fatty acids will have a
purity (as ratio of AV to SV) of 99% at least
and unsaponifiable content of 1% max.
According to the nature of feedstock, the
colour will range from 0,5R to 1,5R
(Lovibond, 51/4 Cell).
When distilling hydrogenated fatty acids
and stearin, the final colour can be even
lower, in the range of 0,1R (Lovibond, 51/4
Cell).
As to the YIELD, the distillation process has
some losses (in the range of 0,1 to 0,2%, the
higher figure being met when distilling
lauric feedstock) and a RESIDUE that can Falling film evaporator - details
be estimated by the following formula:

R (%) = (100-FFA of feedstock ) x 1,8 ÷ 2

The acidity of residues is normally in the range of 5 to 15% FFA max.

The LIGHT ENDS fatty acids are generally in the range of 0,5% up to 2% of feedstock (the higher
figure being obtained when processing lauric feedstock).
The final yield of distilled fatty acids is therefore given by:

Feedstock - (Moisture + Losses + Light ends + Residues)

For example, when distilling tallow fatty acids with a splitting degree of 98% and 0,2% moisture,
the final yield of distilled fatty acids including light ends will be in the range of 95,7% or 95,2%
without light ends.
4.2 STRAIGHT DISTILLATION
SPECIFIC REQUIREMENTS STRAIGHT
Typical approximate consumption figures per ton of feedstock when processing tallow fatty DISTILLA
acids (without topping column):
TION

PROCESS DESCRIPTION
The flow diagram shows a typical continuous plant for fatty acids distillation complete with

Fatty acids distillation plant with topping column (schematic drawing)

 5. HEATING SYSTEMS
HEATING DIATHERMIC FLUID HEATING SYSTEM
SYSTEMS In the fatty acids technology, both in the splitting processes and in all distillation and distillative
fractionation processes, product temperatures in the range of 250°C or more have to be
reached and maintained, which means that heating media at 280 to 300°C must be available.
Two alternatives are possible:

diathermic fluid heating systems are almost universally adopted.

The system, enabling accurate control of temperature, can be designed for several users at a

be fully automated.
The heat generators are very compact and preassembled: the only problem is that they
generally adopt burners that are not suitable for solid or heavy fuels with high viscosity.

Methane or natural gas can also be burnt, in alternative.

COMBINED HEAT & STEAM PRODUCTION

In some cases, for example when the splitting plant
is of the “UNITOWER” type, the diathermic fluid cannot
be used directly as a heating medium: steam at
convenient pressure is absolutely necessary because it
must be injected into the process fluids.
In this case, it is still possible to avoid the use of steam

fluid is used as heating medium.

The steam generator has generally a cylindrical
horizontal design, with a removable U-shaped tubular

circulated.

PROCESS DESCRIPTION
The heating system is using an enclosed circuit with a
heat transfer medium which is circulated, by means of
a suitable pump, through a coil mounted inside the
heat generator, which is directly heated by the flames
Diathermic fluid heater
and fumes produced by the burner.

the circulating pump through a deaerator. Each

circulating pump and auxiliary temperature controller,

if necessary for the process.
One of the users is a special heat exchanger which
is heated by diathermic fluid and produces high
6. SEPARATION BY FRACTIONAL DISTILLATION
PURPOSE SEPARA
The natural oils and fats are mixtures of various fatty acids, saturated and unsaturated, that must
be separated into sharp fractions or even pure components in view of particular uses.
TION BY
FRACTIONAL
Fatty acids of different number of carbon atoms have different boiling temperatures and there- DISTILLA
fore can be separated by using fractional distillation processes.

FEEDSTOCK
TION
Crude fatty acids with splitting degree of at least 96% are the most common feedstock for this
type of separation, of course.
Typical feedstock is coconut oil fatty acids, which is fractionated into C6-C10 cut, and then C12,
C14, C16 and C18 fractions.
The same process and equipment can also be used for fractional distillation of methylesters and
fatty alcohols.

PROCESS CONDITIONS
The operating conditions, as to temperature and pressure, are similar to those being adopted
for fatty acids distillation. Live steam can also be used sometimes, according to the separation
problem. Absolute pressures in the range of 15 to 40 mbar are selected for separation of low
boiling fatty acids (C6 to C10), down to 4 to 10 mbar for high boiling fatty acids (C16 to C22).
Typical equipment being used are:

rectification columns of the packed type (with special structured packing), which enable
very low pressure drop.
Seal-less, canned motor or magnetic drive pumps.
Falling-film evaporators, as reboilers, generally heated by liquid phase diathermic fluids.
Heating candles (as used for straight distillation) when live steam is necessary.

PRODUCTS QUALITY
Very high purities and light colours can be
obtained from distillative fractionation.
For example, when processing coconut oil fatty
acids, individual fractions C6, C8, C10 and C12
can be obtained with purities ranging from 98
to 99% and even 99,5% in some cases.
Fatty acids with higher carbon atoms number
(C14, C16 and C18) can be obtained with
purities ranging from 95 to 98%. Acids C20 to
C22 have generally lower purity, in the range
from 90 to 95%.
The distillative fractionation is economically
possible only in case of fatty acids with different
carbon atoms number. At equal number
of carbon atoms, the separation is not
commercialized yet (for example the
separation of C18:0 from C18:1) because the
relative volatilities are very close to the unit, but
the continuous progresses and developments in
the efficiency of packing materials and
accuracy of measuring instruments enable to
predict that also this type of separation will
be economically possible on industrial scale,
in the future. Fractionating column
and falling film evaporator
 6.1 SEPARATION BY FRACTIONAL DISTILLATION
SEPARA SPECIFIC REQUIREMENTS
TION BY
FRACTIONAL
It is not possible to give even indicative figures because consumptions depend on the specific
separation being considered; the requested purity affects the reflux ratio and therefore the
DISTILLA energy requirements, so that this data must be evaluated case by case.

TION MATERIALS OF CONSTRUCTION

Stainless steel of different grades must be used from AISI 304 on cold parts and storage tanks up
to AISI 316L, AISI 317L or higher grades steels for parts operating at high temperature with low
carbon atoms fatty acids.

PLANT TYPE & CAPACITIES

There is neither standard plant nor capacity so that any specific problem is studied and
engineered case by case.
In principle, three types of FRACTIONAL DISTILLATION PLANTS are available.

BATCH TYPE PLANT

Operating on small batches (not more than 20 to 25 t/d) when not more than two basic fractions
are requested, besides an “odour cut” and a residue.

SINGLE COLUMN
MULTIPLE RUNS PLANT
The plant is working on fully
continuous operation, but with
several RUNS.
It is equipped with one fractionating
column only so that, at each RUN,
one fraction is obtained from the
top as head product and a residue
is discharged from the bottom.
The runs must be as many as the
number of the wanted fractions
minus one.

MULTICOLUMN, FULLY
CONTINUOUS PLANT
This is the type of plant enabling to
obtain the highest purity, the best
qualitative results with the lowest
energetic consumptions.
It consists of several columns in
series; each column is separating
one head fraction, the last column
giving the last head fraction and a
heavy fraction as bottom residue.

Fatty acids distillative fractionation plant

Capacity: 180 t/d
6.2 SEPARATION BY FRACTIONAL DISTILLATION
PROCESS DESCRIPTION SEPARA
We are considering, in this case, a plant equipped with more columns (4 columns plus a
stripper). In case of fatty acids coming from COCONUT oil to be processed (feedstock consisting
TION BY
FRACTIONAL
of a mixture of C6-C18), the plant is capable of producing: DISTILLA
column;
st TION
nd column;
rd column;
th column.

The stripper is designed for the distillation residue

1 exhaustion. The columns are kept under vacuum
at different levels of absolute pressure.
The columns utilize falling film evaporators as
reboilers (except the stripper utilizing live steam
heating elements with candles) and each one is
provided with hot condenser, which produces low
pressure steam by heat recovery.

1 - Structured packing materials

2 - Continuous distillative fractionation plant
(schematic drawing)

2
 7. SEPARATION BY WET FRACTIONATION
SEPARA PURPOSE
TION BY
It is well known that the natural fatty acids of the saturated type have a high melting point (that
is they are normally solid at room temperature) while fatty acids of the unsaturated type are
WET generally liquid at room temperature, that is they have a low melting point.
FRAC The purpose of the so called WET
TIONATION
FRACTIONATION is to separate mixtures of fatty
acids according to their melting point: in other
words a liquid fraction, generally called OLEIN
(predominantly but not exclusively consisting
of unsaturated fatty acids) can be separated
from a solid or hard fraction, generally called
STEARIN (predominantly but not exclusively
consisting of saturated fatty acids).

FEEDSTOCK
Although in some special cases the wet
fractionation can also be carried out on
crude fatty acids, GIANAZZA International
recommends to use distillated fatty acids as
feedstock for this process.
Tallow, lard, palm oil fatty acids are typically
used and generally distilled fatty acids having:

Wet fractionation plant

for the separation of olein/stearin

PROCESS CONDITIONS

saturated fatty acids (stearin) crystallize while the unsaturated ones (olein) remain liquid. The
addition of an aqueous solution of a surfactant or wetting agent enables to lower the surface
tension of the crystallized acids, so that crystals are wetted by the water solution and they are
dispersed into the aqueous phase, whereas the liquid acids will not be mixed with water.
It follows that the liquid phase can be separated from the aqueous phase by a centrifugal
separator.
After separation, by raising the temperature of the aqueous phase, the acid crystals contained
in it are melted, become liquid and immiscible again and, consequently, they can be
separated in a second centrifugal separator.
4, is
also used in the process.

PRODUCTS QUALITY & YIELDS

STEARIN OLEIN
The composition of the two fractions
obtained from the process depends
on the composition of feedstock and
the crystallization temperatures. The
following results are typically obtained
from tallow fatty acids:

olein have to be re-distilled when a very light colour is requested.

7.1 SEPARATION BY WET FRACTIONATION
SPECIFIC REQUIREMENTS SEPARA
Typical approximate consumption figures per ton of tallow fatty acids submitted to wet
fractionation:
TION BY

WET
3 FRAC
3 TIONATION
refrigeration

MATERIALS OF CONSTRUCTION

1
STANDARD CAPACITIES

PROCESS DESCRIPTION

2
1 - Wet fractionation plant - Capacity: 40 t/d
2 - Wet fractionation plant (schematic drawing)
 8. HYDROGENATION
HYDRO PURPOSE
GENA The hydrogenation reaction is intended to saturate the double bonds of fatty acids and
decrease their Iodine Value, thus elevating their melting point, which enables to use the
TION hydrogenated product for a wide range of industrial applications.

FEEDSTOCK
Typically unsaturated or partially saturated distil-
led fatty acids are submitted to hydrogenation.
Crude split fatty acids can also be hydrogenated
under special conditions.
The same plant handling fatty acids can also
process pretreated oils and fats.
The reaction requires:
hydrogen, with minimum purity of 99,8%
(generally electrolytic hydrogen is used with
purity of 99,9% or higher);
nickel catalyst (the commercial products “Dead-End” type fatty acids
generally contain from 20 to 25% of active hydrogenation plant - Capacity: 60 t/d
nickel).

PROCESS CONDITIONS
Fatty acids hydrogenation is carried out at pressures of 20÷22 bar and temperature of
200÷220°C.
Neutral oils and fats are hydrogenated at much lower pressure (3 to 10 bar).
Typical producers of fatty acids are generally processing a wide variety of products so that
quality changeover and variation of operating conditions are rather frequent: very elastic
plants are therefore requested and this result can only be obtained with BATCH operating
plants.
When both feedstock and final product I.V. are constant, also continuous plants can be
proposed.
Within the range of BATCH operating systems, three types of plants are available according to
their heat recovery degree:
NHR (No Heat Recovery)
The plant is equipped with one reactor only, in which the batch is dehydrated, hydrogena-
ted, cooled and sent to filtration.
Each batch is fully processed in 6÷8 hours.

PHR (Partial Heat Recovery)

The plant includes one reactor plus one receiver/heat exchanger.
This is the most widely used plant, with great elasticity.
Each batch is fully processed in 4÷6 hours.

IHR (Integral Heat Recovery)

The plant includes one reactor, one receiver/drier of the batch to be hydrogenated, one
drop tank for the hydrogenated product and one special heat exchanger. The plant has not
only a steam consumption of ZERO but is even producing LOW PRESSURE STEAM from the heat
of reaction.
Each batch is fully processed in 2÷3 hours.
This type of plant, nevertheless, is not recommended when frequent changes of feedstock
are requested.

All the three types of plants are adopting a reactor that can be of two types: the “Dead-End”
type or the “Loop Reactor” type.
8.1 HYDROGENATION
THE GIANAZZA INTERNATIONAL “DEAD-END” REACTOR HYDRO
This reactor uses a stirrer of special design (especially designed for gas-liquid reactions in
presence of suspended solid catalyst), which is capable of obtaining the recirculation of gas in
GENA
the liquid mass without any compressor or any other external device. TION
The stirrer is equipped with two types of turbines:
the lower turbines (“flat blade” type, the number
depending on the size of the reactor), give a
predominantly radial circulation: this improves heat
transfer, keeps the catalyst well suspended and
distributes the gas uniformly; the shearing stresses of
the radial liquid flow divide the gas into small bub-
bles and create a sort of barrier obliging the gas to
stay in a prolonged contact with the fat.
The upper turbine (double centrifugal impeller
type with self-inducing hood ring) is working like a
pump, which is capable of sucking the unreacted
hydrogen from the top of the reactor and recycling
it again into the reacting liquid mass.

“LOOP REACTOR”
In alternative to the “Dead-End” reactor previously
described, GIANAZZA International can propose a “Dead-End” type fatty acids
“Loop Reactor” type plant for reactions at low pressure hydrogenation plant
(edible oils) or for reactions at high pressure (fatty Capacity: 16 t/batch
acids, fats amines, oleochemicals).
The “Loop Reactor” shown on the next page, utilizes a special pump for the recirculation of the
liquid in reaction through an external heat exchanger (working as heater or cooler).
The liquid in circulation is then returned to the reactor by means of a special injector (or venturi
tube) sucking the hydrogen from the upper part of the reactor and injecting and closely mixing
the liquid and the catalyst through the venturi tube in the reaction product. This system is very
efficient and, according to the reactor dimension, it can carry out several batches per day.
PRODUCTS QUALITY
Fatty acids and/or neutral fats can be hydrogenated totally or partially to any desired I.V.
Stearin (or stearic acid) with I.V. of 1 or lower can be produced.
Advanced instruments enable, whenever requested, to predetermine the wanted quantity of
hydrogen to be consumed and automatically stop the injection as soon as the prefixed amount
is reached: this means to stop the reaction as soon as the wanted I.V. has been obtained. In
case a very light colour is requested (0,1R to 0,5R Lovibond 51/4") a post-treatment with acid or,
better, a re-distillation of the hydrogenated product should be carried out.

SPECIFIC REQUIREMENTS
Per ton of distilled fatty acids available at
70°C to be hydrogenated :

PLANT TYPE NHR PHR IHR

Steam 12 bar 100 kg 50 kg zero MATERIALS OF CONSTRUCTION

3
When processing fatty acids, all parts in
Cooling water 6m 3 m3 0 5 m3
25°C
contact with the product are made of
AISI 316 stainless steel.
Electric energy 8 kWh 10 kWh 12 kWh When processing neutral oils/fats, the
Catalyst (at 20% plant can even be made of carbon
nickel approx.) 1÷2 kg 1÷2 kg 1÷2 kg steel.
Hydrogen (STP)
As to the catalyst filter, when using filter
per unit I.V. 11m
3
1 1 m3 1 0 m3 presses of plate and frame type, the used
materials are AISI 304/316 stainless steel.
 8.2 HYDROGENATION
HYDRO PLANT CAPACITY
Standard capacities cover the range
GENA from 20 to 250 t/d.
TION Higher capacities can be designed
case by case.

1 - “Loop Reactor” type fatty acids

hydrogenation plant - Capacity: 250 t/d
2 - “Dead-End” type fatty acids
hydrogenation plant (schematic drawing)

1
3 - “Loop Reactor” type fatty acids
hydrogenation plant (schematic drawing)

3
9. GLYCERINE RECOVERY
PURPOSE
Different processes in the oleochemical industry (splitting, saponification, transesterification) GLY
involve the obtention of by-products containing glycerine as main component. CERINE
By means of chemical and/or physical treatments, the glycerine recovery process has the RECOVERY
purpose to produce pure glycerine to be destined to different uses (pharmaceutical, cosmetics,
food etc.).
FEEDSTOCK
Three typical processes produce the three most common types of glycerol containing feed-
stock:
Sweet waters coming from fat splitting;
Soaplyes coming from soap manufacture from neutral fats;
Crude glycerine coming from transesterification reaction for methylester and/or Biodiesel
production.

In the three cases, the product consists of a solution containing, in different portion:

may also contain residual methanol.

PROCESS CONDITIONS
The basic process for glycerine recovery

When very good quality oils and fats are

processed, an alternative system can be

The typical operating conditions of each

step are listed hereinafter. Sweet waters evaporation plant - Capacity: 100 t/d

DEPURATION

necessary in case of soaplyes.

Depuration of glycerine from methylesters demands particular processes to be studied case

by case.
 9.1 GLYCERINE RECOVERY
GLY EVAPORATION
The glycerol solution has to be concentrated up to:
CERINE
RECOVERY

DISTILLATION & BLEACHING

Glycerine distillation plant (Italy) - Capacity: 18 t/d

9.2 GLYCERINE RECOVERY
PRODUCT QUALITY & YIELDS
The distilled glycerine has a glycerol content of 99,7% min (up to 99,8%) and complies with the GLY
specifications of most international standards (EP, USP etc) and codes (Pharmacopea, Codex CERINE
Alimentarius etc). RECOVERY
Crude glycerine of poor quality (MONG higher than 1,5%) may need sometimes to be redistilled
in order to meet the a.m. quality requirements.
As to YIELDS, the distillation involves some LOSSES (expressed as % of pure glycerol present in the
feedstock). The following figures can be expected:

thin film evaporator for residues drying).

MATERIALS OF CONSTRUCTION
DEPURATION
The utilization of mineral acids causes corrosion problems. The treatment vats and related equip-
ment are made of special plastic material (generally fiber glass reinforced polyester).
Plates and frames of filter press are made of polypropylene, pumps of acid resisting plastic or
special alloys.

EVAPORATION

In special cases carbon steel can be used considering that the life duration of the plant will be
reduced.

DISTILLATION AND BLEACHING

All the parts in contact with glycerol in the con-

steel.
The main column, overall in case of glycerol from

Structured packing is made of high grade stain-

less steel.

stainless steel.

Biodiesel glycerine distillation plant (Denmark)

Capacity: 45 t/d
 9.3 GLYCERINE RECOVERY
GLY PROCESS DESCRIPTION
The typical flow diagram of a double effect evaporation plant for sweet waters, with
CERINE thermocompressor, is shown here below.
RECOVERY Special salt boxes (or centrifugal separators) have to be added when processing soaplyes.
Crude glycerine is obtained after depuration and evaporation and, according to international
standard, it has the following glycerol content:

the glycerine from FAME production has glycerol content intermediate between the above
mentioned figures.

The next page shows the typical flow diagram of a crude glycerine distillation and bleaching
plant.
The following alternatives are possible:

a scraped thin film evaporator can be used for continuous stripping of residues, in case of

pressurized water or direct contact condensers with structured packing can be used as

continuous bleaching can be supplied, based on the use of adsorption columns containing
fixed beds of granular activated carbon (instead of batch bleaching by filtration).

Sweet waters double effect evaporation plant (schematic drawing)

9.4 GLYCERINE RECOVERY
SPECIFIC REQUIREMENTS
The utilities consumptions depend on the type of glycerine to be treated. GLY
In the evaporation stage the consumptions are mainly related to the quantity of water to be CERINE
removed. RECOVERY
In the distillation stage the consumptions are connected to the wanted final purity and the
nature and quantity of MONG (the higher the purity requirements, the higher the reflux ratio
being needed and the energetic consumptions).
It should be noted that the glycerine distillation plant is pratically unchanged for the three types
of glycerine to be processed (ex soaplyes, ex sweet waters or ex FAME/biodiesel): the
differences for the three types are located at level of pre-treatment and chemical depuration
while the final step (distillation & bleaching) is pratically the same for all types of feedstock.
Finally, it should be noted that, in case of glycerine from FAME and according to the type
of transesterification process, crude glycerine might contain peculiar salts for which the
depuration process may be difficult and expensive.

PLANT CAPACITY
The depuration and evaporation plants up to 10 t/d are based on semi-continuous operation.
For higher capacities, the plants are fully continuous operating.
For glycerine distillation and bleaching, the plants are fully continuous for all capacities; for
capacities higher than 50 t/d, particular solutions are available, to be discussed and agreed
case by case.

Glycerine distillation and bleaching plant (schematic drawing)

We are pleased to inform you that Gianazza International has acqui-
red the rights to Gianazza Technology. We have over 250 successfully
operating plants for edible oils and fats refining as well as more than
300 plants for oleochemicals throughout the world.

Considering the world continuous evolution, Gianazza International is

determined to continue Gianazza's century old commitment to quality
and focus on core business of introducing new technologies, plants
and facilities as well as providing the necessary parts needed to
maintain a first class production.

We are confident to appraise our customers that the Gianazza Inter-

national has the technology and the know-how of Gianazza under a
new structure in order to offer reliable services for years to come. We
have the support of skillful personnels from Gianazza who trust in
more than 120 years of experiences our company has gained since
1892. Gianazza International is devoted to provide long term sati-
sfaction to our customers.

GIANAZZA
nternational
GIANAZZA INTERNATIONAL srl
Via Piranesi, 26 20137 Milano (MI) - Italy
Phone +39.030.2425051 - Fax +39.02.36215805
e-mail: [email protected]
www.gianazza.eu

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