اندازه گیری تجربی حلالیت فوماریک اسید در دی اکسید کربن فوق بحرانی و بررسی الگوهای نظری پیش بینی حلالیت
اسلاید 1: 1اندازه گيري تجربي حلاليت فوماريك اسيد در دي اكسيد كربن فوق بحراني و بررسي الگوهاي نظري پيش بيني حلاليتمهدي صحيحياستاد راهنما: دكتر سيد حسن قاضي عسكراستاد مشاور: دكتر حسين فرخ پور
اسلاید 2: 2Historical 1869 - Discovering the Critical Point (Thomas Andrews ) 1879 - Solving the inorganic salts in ethanole at high pressure ( Hannay & Hogarth ) 1895 – Changing the color of Iodine in supercritical carbon dioxide (Willard )
اسلاید 3: 3Supercritical FluidsSupercritical fluids are substances above their critical temperatures and pressures , whose properties are intermediate between those of gases and liquids, and which can be controlled by both temperature and pressure. Both Gas and liquid phases have the same densities in this range.SOLIDGASLIQUIDSUPERCRITICALFLUIDTriplepointCriticalpoint•Pressure (bar)30374(31.1ºC)(-60ºC)8•Temperature (K)
اسلاید 4: 4•SOLIDGASLIQUIDSUPERCRITICALFLUIDTriplepointCriticalpoint•Pressure (bar)Temperature (K)30374
اسلاید 5: 5•SOLIDGASLIQUIDSUPERCRITICALFLUIDTriplepointCriticalpoint•Pressure (bar)Temperature (K)30374
اسلاید 6: 6•SOLIDGASLIQUIDSUPERCRITICALFLUIDTriplepointCriticalpoint•Pressure (bar)Temperature (K)30374
اسلاید 7: 7•SOLIDGASLIQUIDSUPERCRITICALFLUIDTriplepointCriticalpoint•Pressure (bar)Temperature (K)30374
اسلاید 8: 8Common Supercritical FluidsCarbon dioxide Tc = 31.1 °C Pc = 73.8 barFluoroformTc = 25.9 °C Pc = 48.2 bar Water Tc = 374.0 °C Pc = 220.6 barAmmoniaTc = 132.4 °C Pc= 113.2 barEthaneTc = 32.2 °C Pc = 48.7 bar
اسلاید 9: 9 It’s critical point is in an easily reached range. At its normal Gaseous state Carbon Dioxide is an extremely bad solvent, but as a liquid it has much better solvent capabilities. Low toxicity , low reactivity & high purity at low cost.Why CO2 ?
اسلاید 10: 10ApplicationsExtraction with supercritical fluidNicotineHerbal medicineHerbal essenceCaffeineHerbal oilAnti oxidantsSupercritical fluid as a reaction enviromentSynthesis of catalyst (RESS , GAC)Making the small reactors with high performance
اسلاید 11: 11The Effect of Different Factors on Solubility in SCFPressure and Temperature
اسلاید 12: 12Supercritical fluidPolar : DimethylEtherNonepolar : EthaneCO2Sample matricesVapor pressureInter molecular forces
اسلاید 13: 13Methods of Solubility MeasurementStaticContinuose
اسلاید 14: 14Methods of Solubility CalculationMass measurementChromatographySpectrometryMethods of Sample CollectionSolventSolid phaseDirect…
اسلاید 15: 15Fumaric AcidFumaric acid [(E) – 1,2 – butane dicarboxylic acid ] Fumaric is used in plastic industry to produce its esters specially polyesters. Also the esters of this acid is used in pharmacological industry.
اسلاید 16: 16The Physical Properties of Fumaric Acid
اسلاید 17: 17ExperimentalReagents
اسلاید 18: 18Apparatus and procedure :The solubility measurements were carried out using a static apparatus .(1) imported two– position valve; (2) oven; (3) high pressure needle; (4) equilibrium cell; (5) sampling loop; (6) collection vessel; (7) 6 - port two – position switching valve 1234567
اسلاید 19: 19 For browsing the pressure we used the back-pressure regulator ( BPR , model BP 1580-81 , Jasco ). The oven (model 6410 Plus , Jasco ) temperature was maintained within ± 0.1 ◦C The collected solutes were determined using UV-VIS spectrophotometric technique ( UV-VIS spectrophotometer model V-730 , Jasco ). 750 mg of sample + glass crashed in the equilibrium cell The liquid carbon dioxide molecular filter The liquid carbon dioxide cooling coil reciprocating LC pump (model LC – 6A , Shimadzu Co. )
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اسلاید 23: 23Washing Solvent Optimization
اسلاید 24: 24Results and Discussion
اسلاید 25: 25FT-IR Spectra of SamplesBeforeAfterFT-IR
اسلاید 26: 26BeforeAfterGC-MS
اسلاید 27: 27BeforeAfterH-NMR
اسلاید 28: 28The Amount of Sample
اسلاید 29: 29The Accuracy of Results
اسلاید 30: 30Solubility of Fumaric Acid in SC-CO2
اسلاید 31: 31Pressure Effect
اسلاید 32: 32Temperature Effect on the Solubility of Fumaric acid in SC-CO2
اسلاید 33: 33Equation of StateDilute fluids:Van dervalsDieterciBeattie-BrridgmanRedlich-KwangPeng-RobinsonPeng-Robinson:Pc,Tc,ώZc, DensityOne parameter mixing rulesEvery property
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اسلاید 35: 35Mixing RulesVan dervals Kwak-Mansoorimodified Kwak-Mansoorimodified Kwak-Mansoori:
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اسلاید 37: 37Solubility
اسلاید 38: 38Fumaric acid:
اسلاید 39: 39Chrastil EquationClausius - Clapeyron
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اسلاید 42: 42ConclusionSolubilities of fumaric acid in binary system in supercritical carbon dioxide have been measured.Mole fraction solubilities of fumaric acid in temperature of 50°C were 6.35×10-5 at pressure of 80 bar to 3.45×10-5 at pressure of 300 bar and in temperature of 80°C were 4.1×10-5 at pressure 60 bar to 0.83×10-5 at pressure 300 bar. Disagreement of experimental and calculative data shows that the Peng–Robinson equation of state and Kwak–Mansoori mixing rules are not suitable for fumaric acid. The solubilities are correlated with Chrastil equation and association number for fumaric acid was found as 1.226.
اسلاید 43: 43Tanks for Your Attentio
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