Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation

The capture, storage, and conversion of anthropogenic carbon dioxide (CO2) is one of the urgent environmental challenges. Among the various methods available, direct conversion is the most preferable. An example is the production of cyclic carbonates which are important products in the chemical indu...

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Main Authors: Maria Atlaskina, Zakhar Markin, Kirill Smorodin, Sergey Kryuchkov, Nikita Tsivkovsky, Anton Petukhov, Artem Atlaskin, Olga Kazarina, Andrey Vorotyntsev, Ilya Vorotyntsev
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Language:English
Published: Universitas Indonesia 2025-03-01
Series:International Journal of Technology
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Online Access:https://ijtech.eng.ui.ac.id/article/view/7500
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author Maria Atlaskina
Zakhar Markin
Kirill Smorodin
Sergey Kryuchkov
Nikita Tsivkovsky
Anton Petukhov
Artem Atlaskin
Olga Kazarina
Andrey Vorotyntsev
Ilya Vorotyntsev
author_facet Maria Atlaskina
Zakhar Markin
Kirill Smorodin
Sergey Kryuchkov
Nikita Tsivkovsky
Anton Petukhov
Artem Atlaskin
Olga Kazarina
Andrey Vorotyntsev
Ilya Vorotyntsev
author_sort Maria Atlaskina
collection DOAJ
description The capture, storage, and conversion of anthropogenic carbon dioxide (CO2) is one of the urgent environmental challenges. Among the various methods available, direct conversion is the most preferable. An example is the production of cyclic carbonates which are important products in the chemical industry. Considering that this method relies on catalysis, different catalysts can be used. Ionic liquid has been proposed as a promising candidate but the application in the process remains underexplored. Therefore, this study aimed to synthesize and comprehensively characterize ionic liquid 1-(2-hydroxyethyl)-3-methylimidazolium bromide using spectral techniques, including 1H and 13C NMR, Fourier transform infrared spectroscopy (FTIR), and matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF). This compound was used as a catalyst in the cycloaddition reaction of CO2 with epichlorohydrin to produce 1-chloromethylpropylenecarbonate, comprising an important and in-demand class of organics namely cyclocarbonates. Key reaction parameters including temperature, pressure, and catalyst loading were systematically evaluated for the effects on epichlorohydrin conversion, product yield, and selectivity. The results showed that optimal conditions were found at 90 °C and 650 kPa, with a catalyst loading of 2 mol%. The main product was obtained at a yield of 94% with a selectivity of 97% within 2 hours. Additionally, methods to intensify the catalytic reaction were explored through the application of ultrasonic and microwave irradiation. Both forms of irradiation significantly accelerated the conversion of epichlorohydrin, increasing the catalyst turnover frequency (TOF) from 3.85 h-1 in the blank experiment to 4.50 h-1 and 8.38 h-1 with microwave and ultrasonic irradiation, respectively. The practical ease of integrating these approaches into industrial setups suggests promising potential for technological application. Finally, the feasibility of catalyst recycling was investigated. The 1-(2-hydroxyethyl)-3-methylimidazolium catalyst had stable catalytic activity, with only minimal activity loss observed over five consecutive cycles.
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spelling doaj-art-c8852c313b3e439ea20d0947ffabcf992025-08-20T03:40:22ZengUniversitas IndonesiaInternational Journal of Technology2086-96142087-21002025-03-0116237839410.14716/ijtech.v16i2.75007500Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic IrradiationMaria Atlaskina0Zakhar Markin1Kirill Smorodin2Sergey Kryuchkov3Nikita Tsivkovsky4Anton Petukhov5Artem Atlaskin6Olga Kazarina7Andrey Vorotyntsev8Ilya Vorotyntsev9Laboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaChemical Engineering Laboratory, Lobachevsky State University of Nizhny Novgorod, 23 Gagarin Avenue, Nizhny Novgorod, 603022, RussiaLaboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaLaboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaLaboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaChemical Engineering Laboratory, Lobachevsky State University of Nizhny Novgorod, 23 Gagarin Avenue, Nizhny Novgorod, 603022, RussiaLaboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaLaboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaChemical Engineering Laboratory, Lobachevsky State University of Nizhny Novgorod, 23 Gagarin Avenue, Nizhny Novgorod, 603022, RussiaLaboratory of SMART Polymeric Materials and Technologies, Mendeleev University of Chemical Technology of Russia, Miusskaya square, 9, Moscow, 125047 RussiaThe capture, storage, and conversion of anthropogenic carbon dioxide (CO2) is one of the urgent environmental challenges. Among the various methods available, direct conversion is the most preferable. An example is the production of cyclic carbonates which are important products in the chemical industry. Considering that this method relies on catalysis, different catalysts can be used. Ionic liquid has been proposed as a promising candidate but the application in the process remains underexplored. Therefore, this study aimed to synthesize and comprehensively characterize ionic liquid 1-(2-hydroxyethyl)-3-methylimidazolium bromide using spectral techniques, including 1H and 13C NMR, Fourier transform infrared spectroscopy (FTIR), and matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF). This compound was used as a catalyst in the cycloaddition reaction of CO2 with epichlorohydrin to produce 1-chloromethylpropylenecarbonate, comprising an important and in-demand class of organics namely cyclocarbonates. Key reaction parameters including temperature, pressure, and catalyst loading were systematically evaluated for the effects on epichlorohydrin conversion, product yield, and selectivity. The results showed that optimal conditions were found at 90 °C and 650 kPa, with a catalyst loading of 2 mol%. The main product was obtained at a yield of 94% with a selectivity of 97% within 2 hours. Additionally, methods to intensify the catalytic reaction were explored through the application of ultrasonic and microwave irradiation. Both forms of irradiation significantly accelerated the conversion of epichlorohydrin, increasing the catalyst turnover frequency (TOF) from 3.85 h-1 in the blank experiment to 4.50 h-1 and 8.38 h-1 with microwave and ultrasonic irradiation, respectively. The practical ease of integrating these approaches into industrial setups suggests promising potential for technological application. Finally, the feasibility of catalyst recycling was investigated. The 1-(2-hydroxyethyl)-3-methylimidazolium catalyst had stable catalytic activity, with only minimal activity loss observed over five consecutive cycles.https://ijtech.eng.ui.ac.id/article/view/7500carbon dioxide utilizationcyclic carbonatescycloadditionionic liquid
spellingShingle Maria Atlaskina
Zakhar Markin
Kirill Smorodin
Sergey Kryuchkov
Nikita Tsivkovsky
Anton Petukhov
Artem Atlaskin
Olga Kazarina
Andrey Vorotyntsev
Ilya Vorotyntsev
Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation
International Journal of Technology
carbon dioxide utilization
cyclic carbonates
cycloaddition
ionic liquid
title Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation
title_full Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation
title_fullStr Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation
title_full_unstemmed Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation
title_short Optimized CO2 Cycloaddition to Epichlorohydrin Catalyzed by Ionic Liquid with Microwave and Ultrasonic Irradiation
title_sort optimized co2 cycloaddition to epichlorohydrin catalyzed by ionic liquid with microwave and ultrasonic irradiation
topic carbon dioxide utilization
cyclic carbonates
cycloaddition
ionic liquid
url https://ijtech.eng.ui.ac.id/article/view/7500
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