1 / 52

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.

winola
Download Presentation

Acetic Acid, Diacetin & Triacetin

An Image/Link below is provided (as is) to download presentation Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author. Content is provided to you AS IS for your information and personal use only. Download presentation by click this link. While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server. During download, if you can't get a presentation, the file might be deleted by the publisher.

E N D

Presentation Transcript

  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

More Related