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Acetic Acid, Diacetin & Triacetin

Quaternary Solubility of in Supercritical Carbon Dioxide. Acetic Acid, Diacetin & Triacetin. By: S. Afsari . Superadvisor: Dr. Ghaziaskar. Contents. Introduction Supercritical Region Supercritical fluids and CO 2 as a SF. Advantages of Supercritical Sys.

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Acetic Acid, Diacetin & Triacetin

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  1. Quaternary Solubility of in Supercritical Carbon Dioxide Acetic Acid, Diacetin & Triacetin By: S. Afsari Superadvisor: Dr. Ghaziaskar

  2. Contents • Introduction • Supercritical Region • Supercritical fluids and CO2 as a SF. • Advantages of Supercritical Sys. • Factors effecting on supercritical solubility • Apparatus • SFE systems • ACAC and Glycerol Acetyls in supercritical systems • Solubility measurements in ScCO2 and possible separation techniques

  3. Why GlycerolAcetyls?

  4. Transesterification of vegetable oils + 3 HOCH3 NaOH or KOH Catalyst +

  5. Glycerol acetylation

  6. Triacetin Diacetin

  7. scco21 Supercritical Region C T

  8. Supercritical Fluids 1) Low critical T 2)Cheap 3) available 3) Inexplosive 4) Nontoxic Х Х Х

  9. CO2 Phase Diagram

  10. Ability of controlling Solubility • Low viscosity • High diffusion • Easy separation of solvent from solute Gas like liquid like

  11. Factors Effecting Solubility in Supercritical Fluids Hildebrand Parameter: Pressure SampleMatrix Temperature Solute Structure SolventStructure

  12. Factors Effecting Solubility in Supercritical Fluids Pressure SampleMatrix 60ºC Temperature 40ºC Solute Structure SolventStructure

  13. Factors Effecting Solubility in Supercritical Fluids Pressure SampleMatrix • Solute Structure • Solute Vapor pressure • Solute-Solvent interactions Temperature Solute Structure SolventStructure

  14. Factors Effecting Solubility in Supercritical Fluids Pressure SampleMatrix Temperature Solute Structure SolventStructure Naphthalene

  15. Factors Effecting Solubility in Supercritical Fluids • Chemical properties • Physical properties Pressure SampleMatrix Temperature Solute Structure SolventStructure

  16. Gas Meter Apparatus

  17. Introduction

  18. 2 port cylindrical cells

  19. Gas Meter Apparatus

  20. Back Pressure Adjuster

  21. Gas Meter Apparatus

  22. Sampling Collection solvent Solute

  23. Gas Meter Apparatus

  24. Higher repeatability • Lower solvent consumption • Lower time consuming procedure • Fluctuations in flow rate • Different possible analyzing methods • Simple & practical separation • Higher sensitivity • Lower repeatability SFE Systems • On-line • Off-line

  25. Solubility • Gas meter: V, T Weighting GC Mole fraction: g/L in CO2

  26. Sample: Solvent: Et-OH :89% ACAC :6% TAG :9% DAG

  27. System Stability Checking y×100 Pressure (bar)

  28. Purge Test W (mg) CO2 Volume (L)

  29. Weight of Sample Effective Parameters on Solubility in ScCO2 Weight of sample Flow Rate y×100 Temperature Pressure CO2 Volume (L) ACAC

  30. Weight of Sample y×100 CO2 Volume (L) TAG

  31. Weight of Sample y×100 DAG CO2 Volume (L)

  32. Weight of Sample Effective Parameters on Solubility in ScCO2 Flow Rate Weight of sample y×100 Temperature Pressure CO2 Volume (L)

  33. y×100 Pressure (bar) Effective Parameters on Solubility in ScCO2 ACAC 75ºC Weight of sample Flow Rate Ө (ºC): 30,40,60,75 P (bar): 70,100,120,140,160,180 60ºC 40ºC Temperature Pressure

  34. 75ºC 60ºC y×100 40ºC Pressure (bar) TAG Ө: 40ºC, P: 70 bar Ө: 60ºC, P: 70 bar Ө: 75ºC, P: 70 bar Ө: 75ºC, P: 100 bar

  35. 75ºC 60ºC y×100 40ºC Pressure (bar) DAG Ө: 40ºC, P: 70 bar Ө: 60ºC, P: 70 bar Ө: 60ºC, P: 100 bar Ө: 75ºC, P: 70 bar Ө: 75ºC, P: 100 bar

  36. α% Pressure (bar) Separation ACAC, DAG, TAG

  37. Separation of ACAC Ө: 60ºC P: 70 bar

  38. Et-OH ACAC n-hexanol Separation of ACAC Ө: 60ºC P: 70 bar

  39. Separation of ACAC Ө: 75ºC P: 100 bar

  40. Ө=60 ºC, P=70 bar ACAC Ө=60 ºC, P=100 bar TAG Ө: 40ºC, P: 70 bar Ө: 60ºC, P: 70 bar Ө: 60ºC, P: 100 bar Ө: 75ºC, P: 70 bar Ө: 75ºC, P: 100 bar Ө: 40ºC, P: 70 bar Ө: 60ºC, P: 70 bar Ө: 75ºC, P: 70 bar Ө: 75ºC, P: 100 bar • Incomplete extraction • Low efficiency TAG DAG Separation TAG & DAG

  41. Separation of ACAC under Subcritical Situation ?

  42. y×100 Pressure (bar) Binary and Quaternary Solubility of Acetic Acid Factors Effecting Solubility in Supercritical Fluids • Chemical properties • Physical properties Pressure Binary Sample Matrix Solute Structure SolventStructure Quaternary

  43. O C OH OH O C C O O CH3 CH3 Solvent Attributes of ScCO2 CO2

  44. y×100 Pressure (bar) Factors Effecting Solubility in Supercritical Fluids • Chemical properties • Physical properties Pressure Sample Matrix Solute Structure SolventStructure Ө= 40ºC

  45. y×100 Pressure (bar) Factors Effecting Solubility in Supercritical Fluids • Chemical properties • Physical properties Pressure Sample Matrix Solute Structure SolventStructure Ө= 75ºC

  46. y x b m y: Solubility (mole fraction) T: temperature (K) ρ: CO2 density in P & T ( ) Bartle Equation

  47. ρ (g/L) Pressure (bar) Experimental Solubility Correlation • ACAC • DAG • TAG • Ө: 40ºC, 75ºC • P: 100-180 bar • Ө: 60ºC • P: 100-180 bar

  48. Ln(yP/Pref) ρ-ρref Experimental Solubility CorrelationACAC

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