Characterization of reaction enthalpy and kinetics in a microscale flow platform
We report an isothermal flow calorimeter for characterization of reaction enthalpy and kinetics. The platform consists of a thermoelectric element and a glass–silicon microreactor to measure heat flux and an inline IR spectrometer to monitor reaction conversion. The thermally insulated assembly is c...
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| Format: | Article |
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Royal Society of Chemistry (RSC)
2020
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| Online Access: | https://hdl.handle.net/1721.1/128541 |
| _version_ | 1826203557388353536 |
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| author | Ladosz, Agnieszka Kuhnle, Christina Catharina Jensen, Klavs F |
| author2 | Massachusetts Institute of Technology. Department of Chemical Engineering |
| author_facet | Massachusetts Institute of Technology. Department of Chemical Engineering Ladosz, Agnieszka Kuhnle, Christina Catharina Jensen, Klavs F |
| author_sort | Ladosz, Agnieszka |
| collection | MIT |
| description | We report an isothermal flow calorimeter for characterization of reaction enthalpy and kinetics. The platform consists of a thermoelectric element and a glass–silicon microreactor to measure heat flux and an inline IR spectrometer to monitor reaction conversion. The thermally insulated assembly is calibrated with a thin film heater placed between the microreactor and the thermoelectric element. Without any reconfiguration of hardware, the setup can also be used to efficiently characterize reaction kinetics in transient flow experiments. We tested the calorimeter with hydrolysis of acetic anhydride as a model reaction. We determined the exothermic reaction enthalpy and the endothermic heat of mixing of the reagent to be −63 ± 3.0 kJ mol⁻¹ and +8.8 ± 2.1 kJ mol⁻¹ respectively, in good agreement with literature values and theoretical predictions. Following calorimetry studies, we investigated reaction kinetics by applying carefully controlled residence time ramps at four different temperatures, and we obtained kinetic rate constants of 0.129 min⁻¹ up to 0.522 min⁻¹ for temperatures between 20 °C and 56.3 °C, also fitting well with data reported in the literature. |
| first_indexed | 2024-09-23T12:39:27Z |
| format | Article |
| id | mit-1721.1/128541 |
| institution | Massachusetts Institute of Technology |
| last_indexed | 2024-09-23T12:39:27Z |
| publishDate | 2020 |
| publisher | Royal Society of Chemistry (RSC) |
| record_format | dspace |
| spelling | mit-1721.1/1285412022-10-01T10:18:27Z Characterization of reaction enthalpy and kinetics in a microscale flow platform Ladosz, Agnieszka Kuhnle, Christina Catharina Jensen, Klavs F Massachusetts Institute of Technology. Department of Chemical Engineering We report an isothermal flow calorimeter for characterization of reaction enthalpy and kinetics. The platform consists of a thermoelectric element and a glass–silicon microreactor to measure heat flux and an inline IR spectrometer to monitor reaction conversion. The thermally insulated assembly is calibrated with a thin film heater placed between the microreactor and the thermoelectric element. Without any reconfiguration of hardware, the setup can also be used to efficiently characterize reaction kinetics in transient flow experiments. We tested the calorimeter with hydrolysis of acetic anhydride as a model reaction. We determined the exothermic reaction enthalpy and the endothermic heat of mixing of the reagent to be −63 ± 3.0 kJ mol⁻¹ and +8.8 ± 2.1 kJ mol⁻¹ respectively, in good agreement with literature values and theoretical predictions. Following calorimetry studies, we investigated reaction kinetics by applying carefully controlled residence time ramps at four different temperatures, and we obtained kinetic rate constants of 0.129 min⁻¹ up to 0.522 min⁻¹ for temperatures between 20 °C and 56.3 °C, also fitting well with data reported in the literature. 2020-11-19T17:24:18Z 2020-11-19T17:24:18Z 2020-09 2020-06 Article http://purl.org/eprint/type/JournalArticle 2058-9883 https://hdl.handle.net/1721.1/128541 Ladosz, Agnieszka et al. "Characterization of reaction enthalpy and kinetics in a microscale flow platform." Reaction Chemistry & Enigineering 5, 11 (September 2020): doi.org/10.1039/D0RE00304B. © 2020 Royal Society of Chemistry 2020 https://doi.org/10.1039/D0RE00304B Reaction Chemistry & Enigineering Creative Commons Attribution 3.0 unported license https://creativecommons.org/licenses/by/3.0/ application/pdf Royal Society of Chemistry (RSC) Royal Society of Chemistry (RSC) |
| spellingShingle | Ladosz, Agnieszka Kuhnle, Christina Catharina Jensen, Klavs F Characterization of reaction enthalpy and kinetics in a microscale flow platform |
| title | Characterization of reaction enthalpy and kinetics in a microscale flow platform |
| title_full | Characterization of reaction enthalpy and kinetics in a microscale flow platform |
| title_fullStr | Characterization of reaction enthalpy and kinetics in a microscale flow platform |
| title_full_unstemmed | Characterization of reaction enthalpy and kinetics in a microscale flow platform |
| title_short | Characterization of reaction enthalpy and kinetics in a microscale flow platform |
| title_sort | characterization of reaction enthalpy and kinetics in a microscale flow platform |
| url | https://hdl.handle.net/1721.1/128541 |
| work_keys_str_mv | AT ladoszagnieszka characterizationofreactionenthalpyandkineticsinamicroscaleflowplatform AT kuhnlechristinacatharina characterizationofreactionenthalpyandkineticsinamicroscaleflowplatform AT jensenklavsf characterizationofreactionenthalpyandkineticsinamicroscaleflowplatform |