The process of separation of one component from the other using super critical fluid as solvent is termed as super critical fluid extraction(SCFE) The technique of supercritical fluid extraction utilizes the dissolution power of supercritical fluids, i.e. fluids above their critical temperature and pressure.

1. SUPERCRITICAL
FLUID
EXTRACTION
PRACHI GHADGE
BFT-17034

2. SUPERCRITICAL FLUIDS?
 At a certain temperature and pressure condition, liquid and vapour
phases of a substance become indistinguishable. Known as CRITICAL
CONDITION
 Substances above critical point- "SUPERCRITICAL FLUIDS" (SCF)

3. INTRODUCTION
• Supercritical fluids (SCFs) are increasingly replacing the organic solvents
that are used in industrial purification and recrystallization operations
because of regulatory and environmental pressures on hydrocarbon and
ozone-depleting emissions.
• A supercritical fluid (SCF) is defined as “non-compressible and high density
fluid”.
• With increasing scrutiny of solvent residues in pharmaceuticals and medical
products the use of SCFs is rapidly proliferating in all industrial sectors.
• Used supercritical fluids. (Carbon dioxide and water are the most common)

4. SUPERCRITICAL FLUID
In the supercritical
domain, the SCF
increases in
density as the
pressure is
raised whilst
other physical
properties,
including
diffusivity, change
but remain gas-
like.

5. SUPERCRITICAL FLUID EXTRACTION (SFE)
• Supercritical Fluid Extraction (SFE) is the process of separating
one component (the extractant) from another (the matrix) using
supercritical fluids as the extracting solvent.
• Extraction is usually from a solid matrix, but can also be from
liquids.
• The technique of supercritical fluid extraction utilizes the
dissolution power of supercritical fluids, i.e. fluids above their
critical temperature and pressure.

6. SUPERCRITICAL FLUID EXTRACTION (SFE)
 Carbon dioxide (CO2) is the most used supercritical fluid,
sometimes modified by co-solvents such as ethanol or methanol.
 Other current and potential uses include the removal of
undesirable substances such as pesticide residues, removal of
bacteriostatic agents from fermentation broths, the recovery of
organic solvent from aqueous solution, cell disintegration,
destruction and treatment of industrial wastes and liposome
preparation.

7. Why CO2 is used most often in SFE?
• Separation of the carbon dioxide from the extract is simple and
nearly instantaneous.
• Unlike liquid solvents, the dissolving power of supercritical
carbon dioxide can be easily adjusted by slight changes in the
temperature and pressure, making it possible to extract
particular compounds of interest.
• Additional advantages of carbon dioxide are that it is
inexpensive, available in high purity; FDA approved, and is
generally regarded as a safe compound (GRAS).

8. WORKING OF SUPER
CRITICAL FLUID
EXTRACTION
NAME-GRISHMA.MEHTA
ROLL NO.-BFT-18012

10.  Triple point-The temperature and
pressure at which solid liquid and gas
phases of pure substances
 Critical point- The end point of the phase
equilibrim curve between liquid and
gas;beyond this point,they are
indistinguishable and form supercritical
fluid.
 Supercritical fluids-
• quickly spread dissolve substance and
make space for more.
• They are unaffected by surface tension.
• They can also get to parts where the
liquids cant

11.  Extrcation and isolation of natural products by conventionally means creates copious amount of waste
organic solvent
 The industrial solvent are hazardous to human health
 So there is a need for more environmentally vaible solution that has recently paved the way for green
chemistry
 Strict regulations in terms of usage of industrial solvents has led to increase in the demand of
super critical fluid extraction technology(SCFE)
Safe
Inexpensive
Non toxic
Environmental
friendly
Non
flammable
Less energy
requirements
SCFE

12. WHAT IS SCFE?
The process of separation of one component from the other using super
critical fluid as solvent is termed as super critical fluid extraction(SCFE)

13. It displays property intermidiate to those of liquid and
gaseous state also known as compressable liquid or
dense gases.
High solvent power is due to their liquid like density
excellent transport properties owing to the gas like viscosity
and diffusivity together with zero surface tension
PROPERTIES
OF SCF

14. STATIC
DYNAMIC
COMBINATION
Modes of
extraction

15. Circulation of SCF IN LOOP containing the extraction vessel for a certain period followed by it release
through the restrictor to the trapping vessel
STATIC
DYNAMIC
Conduction of static extraction for some time followed by dynamic extraction
COMBINATI
ON
Continous flow of SCF through the sample in the extraction vessel and out of the
restrictor to the trapping vessel

16. Simple model of SFE

17. Figure shows the
stages during
extraction from a
spherical particle
where at the start of
the extraction the
level of extractant is
equal across the
whole sphere
As extraction
commences, material
is initially extracted
from the edge of the
sphere, and the
concentration in the
center is unchanged
As the extraction
progresses, the
concentration in the
center of the sphere
drops as the
extractant diffuses
towards the edge of
the sphere
a b c

18.  The relative rates of diffusion and dissolution are
illustrated by two extreme cases in Figure.
 Figure a shows a case where dissolution is fast relative to
diffusion.
 The material is carried away from the edge faster than it
can diffuse from the center, so the concentration at the
edge drops to zero.
 The material is carried away as fast as it arrives at the
surface, and the extraction is completely diffusion limited.
Here the rate of extraction can be increased by increasing
diffusion rate, for example raising the temperature, but not
by increasing the flow rate of the solvent.
 Figure b shows a case where solubility is low relative to
diffusion. The extractant is able to diffuse to the edge
faster than it can be carried away by the solvent, and the
concentration profile is flat.
 In this case, the extraction rate can be increased by
increasing the rate of dissolution, for example by increasing
flow rate of the solvent.

19. The extraction curve of % recovery against time can be
used to elucidate the type of extraction occurring.
Figure (a) shows a typical diffusion controlled curve. The
extraction is initially rapid, until the concentration at the
surface drops to zero, and the rate then becomes much
slower.
The % extracted eventually approaches 100%.
Figure (b) shows a curve for a solubility limited extraction.
The extraction rate is almost constant, and only flattens off
towards the end of the extraction.
Figure (c) shows a curve where there are significant
matrix effects, where there is some sort of reversible
interaction with the matrix, such as desorption from an
active site.
The recovery flattens off, and if the 100% value is not
known, then it is hard to tell that extraction is less than
complete.

21. Feed introduction in the extraction vessel
Before pressurization,the system is allowed to reach the present
operating temperature
Cooling of SCF(CO2) in the chiller to ensure liquid feed to the pump
Discharge of chilled CO2 into the pressure vessel and adjustment of the pressure to
the desired level
1
2
3
4
OPERATING PROCEDURE FOR SCFE

22. Simultaneous discharge of co-solvent through pump at pre-
determined flowrate
Conduction of extraction through static /dynamic/combination
mode pf extraction
Isolation of dissolved solute by precipitation;release recovery of SCF
5
6
7
OPERATING PROCEDURE FOR SCFE

23. References
• https://www.che.iitb.ac.in/online/page/overview-scf-research-iitb
• https://www.youtube.com/watch?v=icfpml9hKP8
• https://www.chemistryviews.org/details/ezine/4393381/50th_Anniv
ersary_Supercritical_Fluid_Extraction.html
• https://www.youtube.com/watch?v=UxAjlmaUNzs
• https://www.youtube.com/watch?v=LQfVJ0MvqEo&t=121s

24. Application of SCFE in Food Industry
Shamika Gavali
BFT18010

25. SCFE has wide application in natural products
and food industry such as
• Decaffeination of coffee and tea
• Spice Extraction(oil and oleoresin)
• Deodorization of oils and fats
• Flavors, fragrances, aromas and perfumes
• Decholesterolization of egg yolk and dairy cream
• Antioxidants from plants
• Food colors from botanicals
• Natural pesticides

26. SCFE Technology can be used for Extraction,
purification and separation of:
• Edible oils and fats
• Hop extraction
• Natural dyes: Annatto, Hibiscus
• Vitamins(tocopherols, vit E, etc)
• Carotenoids
• Sterols
• Essential fatty acids(EPA, DHA,
DPA)
• Bioactive compounds
(pyrethrum, caffeine,
theobromine, cholesterol,
capsaicin, etc)
• Mono and di glycerides
• Aroma compounds
• Citrus oils

27. Decaffeination of coffee and tea using SCFE
technology plant
• Coffee is wetted with water.
• Wetting tends to dissolve and deorb caffeine from the solid material
• The operating conditions are- pressure:300bar Temperature: 40oC
• Green beans are loaded into vessel and SCF
CO2is introduced in vessel.
• Extract is transferred to separator which oper-
ates at low pressure and separtes it into two
Phases- Aquous caffeine and CO2
• The CO2 is recycled
• Caffeine can be recovered by adsorption on an
Activated carbon column.

28. Decaffeination Effect SCFE Process parameters on
yield

29. Decaffeination Effect SCFE process
parameters on recovery

30. Etraction of natural Food Antioxidants
• SFE has been widely studied by several authors to obtain highly active
rosemary antioxidant extracts.
• Topal et al. (2008) demonstrated that the antioxidant activity of
supercritical extracts of different Turkish plants (rosemary among
them) were higher than those obtained by steam distillation.
• Better results in terms of antioxidant activity were also achieved
when compared to liquid solvent sonication.

31. Low Cholesterol Whole milk powder and
cream powder
• SC CO2 and ethanol(co solvent) modified SC CO2 were employed to
extract Cholesterol from whole milk powder and cream powder.
• About 55.8% and 46% of cholesterol removal from WMP could be
achieved by using SC CO2 alone and Ethanol modified SC CO2.
• Addition of Ethanol led to enhanced extraction rate.
• About 39% Cholesterol could be removed from cream powder using
SC CO2 alone.

32. Process flowchart for preparation of Low
cholesterol milk powder using SCFE Technology

33. Application of SCFE for quality control in fat
analysis
• Conventional methods of fat analysis for baking, milk and chocolate
products are time and labour intensive and require large amount of
hazardous organic solvents.
• Supercritical fluid extraction using CO2 as a solvent is an alternative
method for extraction of fat content from these products.

34. `
Optimization of SFE
Bft-18011
Snehal Gite

35. Supercritical fluid extraction
• For all experiments, the extraction vessel (15 mL is first packed
with 6.5 g of glass beads, followed by 125 mg of plant material. The
remaining void of the vessel is filled with 1 g of anhydrous Na2SO4.
• The SFE extractions are carried out using a combination of 2-min
static period to allow the extraction vessel to reach its extraction
pressure and a dynamic extraction step of 23 min.
• The extract is trapped by bubbling the CO2 through 25 mL of methanol.
The flow-rate of supercritical fluid in the dynamic extraction step is
fixed to 2 mL min−1 with the help of a heated variable restrictor.
• A high-pressure pump is connected to the restrictor in order to
obviate its plugging by non-meltable residue. Methanol was selected as
solvent and its flow rate was −1 fixed to 0.3 mL min for the
determinations, the SFE /FT-IR interface was held at 30◦C. Results and
discussion Infrared spectra of the extraction of tagitinin C from T.
diver-sifolia leaves in SCCO2 over time.

36. Supercritical fluid extraction
• well-defined absorbance spectra were obtained between 3400–
2800 and 1900–950 cm Consequently, information
on vibrational modes of functional groups of components such
as CH stretching vibrations (3200–2800 cm−1) and C O
stretching vibrations (1800–1650 cm−1 ) were gathered.
• In addition, the presence of the OH bending vibration of
water contained in the leaves and extracted by SCCO2 was
also observed at −11608 cm

37. SFE optimisation through experimental
design approach
• The traditional optimisation procedure varying one variable at a time
does not guarantee the attainment of a true optimum of the extraction
conditions.
• In the other hand, the chemometric approach based on a rational
experimental design allowing the simultaneous variation of all
experimental factors guarantee this and also allows saving time and
materials.
• This last point was very important in this study for two reasons: a small
quantity of plant material was available and the compound of interest,
i.e.; tagitine C, was present at a low amount in the material provided.

38. • Central composite designs (CCD) are probably the most widely used
experimental designs for fitting a second order response surface.
• A total of 13 random experiments, in which the central point was
replicated five times, were carried out to optimize the influence of
the pressure and temperature of SCCO2 on the extractogram area of
tagitinin C. Generally, the following polynomial model is used to
express the dependent variable as a function of independent
variables:
• Y = α + β P 2 + β T 2 + β P + β T + β PT
• However, the response was not sufficiently explained by the
regression model.

39. • The result can be explained by the fact that the density of
the supercritical fluid decreases with the increase in
temperature at low pressure whereas at higher pressure,
changes in temperature have much less effect on den- sity.
• a second order poly- nomial model involving interactions
terms between the pressure and the temperature was used to
express the area as a function of independent variables:
• Y = α+β1P2 +β2T2 +β3P2T2 +β4P2T +β5PT2 +β6P +β7T +β8
PT
• Unlike the previous model, the response was sufficiently
explained by the regression model. Indeed the coefficient of
determination and the adjusted coefficient of determination
were equal to 0.99 in both cases.

40. • The response surface estimated for the model by using the two
variables, the pressure and temperature of the supercritical fluid, was
drawn to look for the optimum values of these variables.
• it can be seen that, while the pressure was increasing up to 12.0 MPa,
the extractogram area increased dramatically.
• This can be explained by an enhanced solvent strength of
SCCO2 when the pressure grows. On the other hand, the
extractogram area decreased with a rise of temperature. However,
this negative influence of the temperature was reduced with higher
pressure values. In addition, the optimal domain for extraction is
large: between 14.0–20.0 MPa and 40–60 ◦ C.