1 In the name of God Particle design using supercritical fluids Supervisor : Dr. Ghaziaskar By: M....
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1 In the name of God In the name of God Particle design using Particle design using supercritical fluids supercritical fluids Supervisor : Supervisor : Dr. Ghaziaskar Dr. Ghaziaskar By: M. Amirabadi By: M. Amirabadi
1 In the name of God Particle design using supercritical fluids Supervisor : Dr. Ghaziaskar By: M. Amirabadi By: M. Amirabadi
1 In the name of God Particle design using supercritical fluids
Supervisor : Dr. Ghaziaskar By: M. Amirabadi By: M. Amirabadi
Slide 2
2 content Presentation of Supercritical Fluids Reasons of using
Supercritical Fluids Processes of Supercritical Fluid producing
micro and nano-particles Applications of these processes Conclusion
References
Slide 3
3 Supercritical fluid A substance At temperatures and pressures
above its critical temperature and pressure ( its critical point )
is called a supercritical fluid.
Slide 4
4 Why are we using supercritical fluids ?
Slide 5
5 Properties of some supercritical fluids CompoundT c ( o C)P c
(atm) CO 2 31.772.9 H2OH2O 374.1218.3 NH 3 132.5112.5 Butane(C 4 H
10 ) 15237.5 Freon13(CCLF 3 ) 28.838.2 Acetone(C 3 H 6 O) 235.547
Hexan(C 6 H 14 ) 234.229.9
Slide 6
6 Why is CO 2 the most commonly used solvent ? It is easy to
attain critical conditions of CO2 Inexpensive Nontoxic Non-flamable
Providing CO2 in high purity is easy
Slide 7
7 Particle design in supercritical media
Slide 8
8 advantages of particle design using supercritical technology
to conventional methods Supercritical technology Produces very
small particles (micro & nano) Produces narrow particle size
distribution (PSD) Separation of fluid from particles is done
easily Reduces wastes
Slide 9
9 Supercritical fluid methods for particle design RESS (Rapid
Expansion of Supercritical Solutions) SAS/GAS (Supercritical fluid
Anti-Solvent PGSS (Particles from Gas- Saturated Solutions (or
Suspensions) DELOS (Depressurization of an Expanded Liquid
Solution)
Slide 10
10 RESS (Rapid expansion of Supercritical Solutions)
Slide 11
11 Morphology of particles Material structure Crystalline or
amorphose Composite or pure RESS parameters Temperature Pressure
drop Distance of impact of the jet against the surface Dimensions
of the atomization vessel Nozzle geometry
Slide 12
12 Advantages of RESS Producing solvent free products With no
residual trace of solvent, particles are suitable for therapeutic
scopes It can be used for heat labile drugs because of low critical
temperature It needs simple equipment and it is cheap Produced
particles requires no post processing
Slide 13
13 Key limitations of RESS substrate should be soluble in CO 2
Co-solvent can be used for insoluble substrates but elimination of
co-solvent is not easy and cheap
Slide 14
14 Liquid anti-solvent process There are two liquid solvents
(A&B) Solvents are miscible Solute is soluble in A ¬
soluble in B Addition of B to the solution of solute in A causes
precipitation of solute in microparticle
Slide 15
15 Supercritical fluid anti- solvent Solute is dissolved in a
solvent Solute is not soluble in supercritical fluid Supercritical
fluid (anti-solvent) is introduced in solvent Supercritical fluid
expands the solution and decreases solvent power Solute
precipitates in the form of micro or nano particle
Slide 16
16 Advantages of supercritical fluid antisolvent to liquid
antisolvent Separation of antisolvent is easy SAS is faster because
of high diffusion rate of supercritical fluid SAS can produce
smaller particles In SAS particle size distribution is
possible
Slide 17
17 The solute is recrystallized in 3 ways SAS/GAS
(supercritical anti- solvent or gas anti-solvent) ASES (aerosol
solvent extraction system) SEDS (solution enhanced dispersion by
supercritical fluid)
Slide 18
18 SAS/GAS (Supercritical Anti-Solvent)
Slide 19
19 ASES (Aerosol Solvent Extraction System )
Slide 20
20 SEDS (Solution Enhanced Dispersion by Supercritical Fluids
)
Slide 21
21 Experiments are carried out in three scales Laboratorial
scale Pilot scale Plant scale
Slide 22
22 Supercritical antisolvent fractionation of Propolis in pilot
scale Propolis has applications in medicine,hygiene and beauty
Slide 23
23 Flavonoids Essential oil Separation with extraction High
molecular mass components Separation with SAS Components of
propolis
Slide 24
24 Schematic of pilot scale propolis extraction/fractionation
plant
Slide 25
25 Crystal formation of BaCl 2 and NH 4 Cl using a
supercritical fluid antisolvent SAS process has been used to
produce crystals of BaCl 2 and NH 4 Cl from solutions of dimethyl
sulfoxide (DMSO)
Slide 26
26
Slide 27
27 Parameters that affect on crystallization of BaCl 2 & NH
4 Cl Injection rate of CO 2 Initial chloride concentration in DMSO
Temperature
Slide 28
28 Instruments used for determining particle properties
Morphology Scanning electron microscope (SEM) Composition Energy
dispersive X-Ray spectrometer (EDS) Internal structure X-Ray
diffractometer (XRD) Particle size Image size of SEM
photomicrographs
Slide 29
29 Crystal habit of BaCl 2 Slow injection rate of CO 2 Cubic
shaped crystals (Equant habit)Equant habit Rapid injection rate of
CO 2 Needle-like crystals (Acicular habit)Acicular habit The
variation in crystal habit result from the alteration of the
relative growth rate of crystal faces
Slide 30
30
Slide 31
31
Slide 32
32 Crystal habit of NH 4 CL Slow injection rate of CO 2 Equant
Rapid injection rate of CO 2 tabular tabular
Slide 33
33
Slide 34
34
Slide 35
35 Internal structure of BaCl 2 Unprocessed particles
(Orthorhombic space lattice) Processed particles (Hexagonal space
lattice)
Slide 36
36 Internal structure of NH 4 Cl Unprocessed particles (Cubic)
Processed particles (Cubic) Cubic space lattic is the only possible
crystal system for NH 4 Cl
Slide 37
37 Crystal size & composition Crystal size The slower
injection rate of CO 2,the larger crystal size Crystal composition
Composition of crystals did not changed after processing by CO
2
Slide 38
38 Separation of BaCl 2 & NH 4 Cl mixtures in DMSO The SAS
process enables the separation of multicomponent mixtures if the
nucleation of each component occurs at different pressures
Slide 39
39 SAS has used in following applications Explosives and
propellants Polymers and biopolymers Pharmaceutical principles
Coloring matter, catalysts, superconductors and inorganic
compounds
Slide 40
40 Explosives and propellants Small particles of these compound
improves the combustion process Attainment of the highest energy
from the detonation depends on particle size
Slide 41
41 Polymers and biopolymers Polymer microspheres can be used
as: Stationary phases in chromatography Adsorbents Catalyst
supports Drug delivery system
Slide 42
42 Pharmaceutical principles Increasing bio-availability of
poorly-soluble molecules Designing formulations for
sustained-release Substitution of injection delivery by less
invasive methods, like pulmonary delivery
Slide 43
43 Coloring matter, catalysts, superconductors and inorganic
compounds Color strength is enhanced if dying matter is in the form
of micro particles Catalysts in the form of nanoparticles have
excellent activity because of large surface areas
Slide 44
44 RESS & SAS Regarding the materials RESS & SAS are
complementary RESS Compound is soluble in CO 2 SAS Compound is
insoluble in CO 2
Slide 45
45 Conclusion
Slide 46
46 Rapid expansion of supercritical fluid (RESS) CO 2 is
reached to the desired pressure and temperature In extraction unit
solute(s) is dissolved in CO2 In precipitation unit solution is
depressurized Solubility of CO 2 is decreased and solute(s)
precipitates in the form of very small particle or fibers and
films
Slide 47
47 SAS/GAS(supercritical anti-solvent) In this method a batch
of solution is expanded by mixing with supercritical fluid
Slide 48
48 ASES (aerosol solvent extraction system) This method
involves spraying the solution through an atomization nozzle as
fine droplets into compressed carbon dioxide
Slide 49
49 SEDS (solution enhanced dispersion by supercritical fluids)
In this method a nozzle with tow coaxial passages allows to
introduce the supercritical fluid and a solution of active
substance(s) into the vessel
Slide 50
50 Steps of fractionation of Propolis CO2 is supplied from
cylinders. Solution of Propolis in Ethanol is in storage tank1.
Propolis solution and CO2 are mixed before precipitation chamber
EX1. In EX1 the Propolis solution becomes supersaturate and high
molecular mass components precipitate. CO2 and Propolis solution
will furture face two pressure drop. In SV1 flavonoids precipitate.
In SV3 essential oil and ethanol precipitate.
Slide 51
51 Morphology of particles Material structure Crystalline or
amorphose Composite or pure RESS parameters Temperature Pressure
drop Distance of impact of the jet against the surface Dimensions
of the atomization vessel Nozzle geometry