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In the name of God

Learn about the advantages and processes of particle design using supercritical fluids, including techniques like RESS and SAS/GAS, essential parameters for crystal formation, and instrumentation for analyzing particle properties. Discover the applications and benefits of supercritical technology in producing micro and nano-particles, with a focus on CO2 as a commonly used solvent. Explore the morphology of particles and the advantages of supercritical anti-solvent methods compared to liquid anti-solvent processes. Dive into experiments on different scales, such as laboratory, pilot, and plant, and their applications in extracting and fractionating substances like propolis. Get insights into crystal formation using supercritical fluid anti-solvent techniques for BaCl2 and NH4Cl, along with their internal structures. Equip yourself with knowledge of various instruments like SEM, EDS, and XRD used for determining particle properties. Immerse yourself in the world of particle design with supercritical fluids for diverse applications and advancements in the field.

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In the name of God

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  1. In the name of God Particle design using supercritical fluids Supervisor : Dr. Ghaziaskar By: M. Amirabadi

  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

  3. Supercritical fluid A substance At temperatures and pressures above its critical temperature and pressure ( its critical point ) is called a supercritical fluid.

  4. Why are we using supercritical fluids ?

  5. Properties of some supercritical fluids

  6. Why is CO2 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

  7. Particle design insupercritical media

  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

  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)

  10. RESS (Rapid expansion of Supercritical Solutions)

  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

  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

  13. Key limitations of RESS • substrate should be soluble in CO2 • Co-solvent can be used for insoluble substrates but elimination of co-solvent is not easy and cheap

  14. Liquid anti-solvent process • There are two liquid solvents (A&B) • Solvents are miscible • Solute is soluble in A &not soluble in B • Addition of B to the solution of solute in A causes precipitation of solute in microparticle

  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

  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

  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)

  18. SAS/GAS (Supercritical Anti-Solvent)

  19. ASES (Aerosol Solvent Extraction System )

  20. SEDS (Solution Enhanced Dispersion by Supercritical Fluids )

  21. Experiments are carried out in three scales • Laboratorial scale • Pilot scale • Plant scale

  22. Supercritical antisolvent fractionation of Propolis in pilot scale • Propolis has applications in medicine ,hygiene and beauty

  23. Components of propolis Flavonoids Essential oil Separation with extraction Separation with SAS • High molecular mass components

  24. Schematic of pilot scale propolis extraction/fractionation plant

  25. Crystal formation of BaCl2 and NH4Cl using a supercritical fluid antisolvent • SAS process has been used to produce crystals of BaCl2 and NH4Cl from solutions of dimethyl sulfoxide (DMSO)

  26. Parameters that affect on crystallization of BaCl2 & NH4Cl • Injection rate of CO2 • Initial chloride concentration in DMSO • Temperature

  27. 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

  28. Crystal habit of BaCl2 • Slow injection rate of CO2 Cubic shaped crystals (Equant habit) • Rapid injection rate of CO2 Needle-like crystals (Acicular habit) The variation in crystal habit result from the alteration of the relative growth rate of crystal faces

  29. Crystal habit of NH4CL • Slow injection rate of CO2 Equant • Rapid injection rate of CO2tabular

  30. Internal structure of BaCl2 • Unprocessed particles (Orthorhombic space lattice) • Processed particles (Hexagonal space lattice)

  31. Internal structure of NH4Cl • Unprocessed particles (Cubic) • Processed particles (Cubic) • Cubic space lattic is the only possible crystal system for NH4Cl

  32. Crystal size & composition • Crystal size • The slower injection rate of CO2 ,the larger crystal size • Crystal composition • Composition of crystals did not changed after processing by CO2

  33. Separation of BaCl2 & NH4Cl mixtures in DMSO • The SAS process enables the separation of multicomponent mixtures if the nucleation of each component occurs at different pressures

  34. SAS has used in following applications • Explosives and propellants • Polymers and biopolymers • Pharmaceutical principles • Coloring matter, catalysts, superconductors and inorganic compounds

  35. Explosives and propellants • Small particles of these compound improves the combustion process • Attainment of the highest energy from the detonation depends on particle size

  36. Polymers and biopolymers Polymer microspheres can be used as: • Stationary phases in chromatography • Adsorbents • Catalyst supports • Drug delivery system

  37. 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

  38. 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

  39. RESS & SAS • Regarding the materials RESS & SAS are complementary • RESSCompound is soluble in CO2 • SAS Compound is insoluble in CO2

  40. Conclusion

  41. Rapid expansion of supercritical fluid (RESS) • CO2 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 CO2 is decreased and solute(s) precipitates in the form of very small particle or fibers and films

  42. SAS/GAS(supercritical anti-solvent) • In this method a batch of solution is expanded by mixing with supercritical fluid

  43. ASES (aerosol solvent extraction system) • This method involves spraying the solution through an atomization nozzle as fine droplets into compressed carbon dioxide

  44. 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

  45. 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.

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