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Presented by: Jelliarko P. Green & Sustainable Chemistry Lab

Ethylene Carbonate Synthesis by Coupling Reaction of Ethylene Oxide & Carbon Dioxide in the presence of Ionic Liquids Based Catalysts. Activity & Stability of [Emim] 2 ZnBr 2 Cl 2 & [Bu 4 N] 2 ZnBr 2 Cl 2 Catalysts due to Weight Ratio of Substrate/Catalyst & Temperature Variations.

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Presented by: Jelliarko P. Green & Sustainable Chemistry Lab

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  1. Ethylene Carbonate Synthesis by Coupling Reaction of Ethylene Oxide & Carbon Dioxide in the presence of Ionic Liquids Based Catalysts Activity & Stability of [Emim]2ZnBr2Cl2 & [Bu4N]2ZnBr2Cl2 Catalysts due to Weight Ratio of Substrate/Catalyst & Temperature Variations Presented by: Jelliarko P. Green & Sustainable Chemistry Lab

  2. A Progress Report A Progress Report A Progress Report A progress Report O Cat O O O + O C O P T A Progress Report Introduction Coupling Reaction in ethylene carbonate production What is coupling reaction of ethylene oxide and carbon dioxide ? Advantage - One step reaction. - No solvent is required except the product itself. - High molar substrate/catalyst ratio. - Simple distillation in product separation

  3. A Progress Report A Progress Report A Progress Report A progress Report 2 + ZnBr Cl N N 2 2 C H 3 H C 3 H C 2 3 C H 3 + N ZnBr2Cl2 H C 3 C H 3 Introduction [Emim]2ZnBr2Cl2 Transition metal-Ionic Liquids Catalysts [Bu4N]2ZnBr2Cl2 A Progress Report

  4. A Progress Report A Progress Report A Progress Report A progress Report Objective Objective • Investigating decomposition of ethylene carbonate alone under vacuum and high temperature. • Investigating decomposition of ethylene carbonate in the presence of catalyst under vacuum and high temperature. • Investigating activity and stability of catalysts in multiple coupling reactions. Objective Objective Objective A Progress Report

  5. A Progress Report A Progress Report A Progress Report A progress Report A Progress Report Experiments • 1. Investigating Decomposition of Ethylene Carbonate Alone • The reactor was charged with an appropriate amount of EC and was fully vacuumed. Then, temperature was increased step by step to specific value (100 – 170 oC) • After cooling, the mixture was weighted and was taken for GC-MS analysis • Investigating Decomposition of EC in the Presence of Catalyst • The reactor was charge with an appropriate amount of EC and catalyst and was fully vacuumed. Then, temperature was increased step by step to specific value (100 – 170 oC) • After cooling, the mixture was weighted and was taken for GC-MS analysis

  6. A Progress Report A Progress Report A Progress Report A progress Report A Progress Report Experiments 3. Investigating activity and stability of catalysts in multiple coupling reactions [Bu4N]2ZnBr2Cl2 catalyst 0.5 gr of catalyst (1.50 %wt) was loadedinto 200 mL stainless-steel bomb reactor. 50 gr of EC acted as solvent was also put in. Then, the reactor was charged with 33.6 gr of ethylene oxide. The bomb then was pressurized with CO2 and heated to specific reaction temperature (100 oC), with the addition of CO2 from a reservoir tank to maintain a constant pressure. After cooling the reactor, the mixture was weighted and was transferred into distillation apparatus for separation process. The above procedure was repeated 6 times.

  7. Experiments A Progress Report A Progress Report A Progress Report A progress Report A Progress Report 4. Investigating activity and stability of catalysts in multiple coupling reactions 200 mL stainless-steel bomb reactor was charged with an appropriate amount of catalyst and EC acted as solvent. Then, the reactor was charged with ethylene oxide. The bomb was pressurized with CO2 and heated to specific reaction temperature with the addition of CO2 from a reservoir tank to maintain a constant pressure. After cooling the reactor, the mixture was purged with nitrogen to remove dissolved CO2 and EO. The reactor and its content were weighted and the second reaction was performed. Experiments

  8. A Progress Report A Progress Report A Progress Report A progress Report Pressure Transducer Go to Vacuum Condenser Temperature Transducer Reactor Electrical Heater A Progress Report Experiments Experiments Experiments Decomposition Apparatus

  9. A Progress Report A Progress Report A Progress Report A progress Report Experiments Experiments N2 Tank Experiments CO2 Reservoir EO Reservoir Temperature Transducer Electrical Heater Reactor CO2 Tank Magnetic Stirrer A Progress Report Coupling Reaction Apparatus

  10. A Progress Report A Progress Report A Progress Report A progress Report Decomposition Test of EC 250 EC + Cat [Bu4N]2ZnBr2Cl2 EC vapor pressure ? (EC) 1차 200 (EC) 2차 (EC+Cat) Condition. 100mmHg 150 Vapor pressure 100 D P 50 Pure EC 0 40 60 80 100 120 140 160 o Temperature ( C) A Progress Report Result & Discussion EC Properties: m.p. 37 – 39 oC b.p. 243 – 244 oC/740 mmHg 169 oC/100 mmHg 147 oC/50 mmHg Preliminary study showed that decomposition occurred at high reaction temperature. Decomposition of EC into EO and CO2 was observed from pressure increase and weight loss

  11. A Progress Report A Progress Report A Progress Report A progress Report CO2 Consumption A Progress Report 1.50 wt% of [Bu4N]ZnBr2Cl2 showed high activity and stability over six times coupling reactions (100 0C, 500 psig of press. and 1 h reaction time), and separation processes by reduced pressure distillation. Result & Discussion

  12. Result & Discussion A Progress Report A Progress Report A Progress Report A progress Report Multiple reactions, 1st and 2nd. All product mixtures were solid white except for 170 oC reaction temperature were slightly yellowish. A Progress Report Reaction Condition: * CO2 Press. 500 Psig. * EC solvent 39.55 gr [Emim]2ZnBr2Cl2

  13. A Progress Report A Progress Report A Progress Report A progress Report Multiple reactions, 1st and 2nd. A portion was taken from decomposition test at 150 oC. All product mixtures were solid white. A Progress Report [Bu4N]2ZnBr2Cl2 Reaction Condition: * CO2 Press. 500 Psig. * EC solvent 39.55 gr Result & Discussion

  14. Result A Progress Report A Progress Report A Progress Report A progress Report A Progress Report Wt% Ratio Activity [Emim]2ZnBr2Cl2 Reaction Temp. Activity & Discussion

  15. A Progress Report A Progress Report A Progress Report A progress Report A Progress Report Wt% Ratio Activity [Bu4N]2ZnBr2Cl2 Result & Discussion Reaction Temp. Activity Result & Discussion

  16. A Progress Report A Progress Report A Progress Report A progress Report A Progress Report “cHRistmAs” CoNcLuSion & Plans • Conclusion • Moderate EC decomposition occurred at high temperature and severe decomposition occurred in the presence of catalysts. • 1.50 wt% of catalyst ratio showed high durability over multiple coupling reaction and separation processes. ([Bu4N]2ZnBr2Cl2 – study case). • Above 140 oC, [Emim]2ZnBr2Cl2 showed reduced activity as wt% decreased. However, the activity increased as reaction temperature was raised. • Above 120 oC, [Bu4N]2ZnBr2Cl2 showed reduced activity as wt% decreased. However, the activity increased as reaction temperature was raised. • Plans • Finding tune the weight ratio of catalysts over EO that will give the most economical value. • Recycling coupling reaction test.

  17. Ho…..ho….ho…. Dear all….. Happy Christmas & Merry New Year !!! Be cool & Enjoy your works But I will have long vacation ho….ho…ho.. Saint “재준” Claus says………

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