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In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor

Marco Taddei Orcid Logo, Nicola Casati, Daniel A. Steitz, Kim C. Dümbgen, Jeroen A. van Bokhoven, Marco Ranocchiari

CrystEngComm, Volume: 19, Issue: 23, Pages: 3206 - 3214

Swansea University Author: Marco Taddei Orcid Logo

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DOI (Published version): 10.1039/C7CE00867H

Abstract

Large scale synthesis of metal–organic frameworks (MOFs) is of high interest, due to their potential for industrial applications. The capacity to synthesize large amounts of MOFs should be combined with the ability to control their properties. Understanding how process parameters influence the forma...

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Published in: CrystEngComm
ISSN: 1466-8033
Published: 2017
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URI: https://cronfa.swan.ac.uk/Record/cronfa36834
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first_indexed 2017-11-20T14:26:06Z
last_indexed 2018-02-09T05:29:34Z
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spelling 2017-12-11T11:01:39.7259778 v2 36834 2017-11-20 In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor 5cffd1038508554d8596dee8b4e51052 0000-0003-2805-6375 Marco Taddei Marco Taddei true false 2017-11-20 EEN Large scale synthesis of metal–organic frameworks (MOFs) is of high interest, due to their potential for industrial applications. The capacity to synthesize large amounts of MOFs should be combined with the ability to control their properties. Understanding how process parameters influence the formation of the product is necessary to synthesize tailor-made materials. The crystallization process of a MOF from the reaction mixture can be conveniently monitored in real time by performing in situ studies using synchrotron radiation. This yields insight into the formation of the product under the actual reaction conditions. In this work, we performed an in situ high-resolution powder X-ray diffraction study of the crystallization of UiO-66 in a recently developed continuous-flow microwave reactor that provided excellent performances in terms of space-time yield and atom economy. The effect of the addition of different amounts of water and acetic acid to the reaction mixture on the yield and crystallite size of the product was investigated over a range of residence times. UiO-66 was the only crystalline phase observed and two stages of the process were identified, namely, a preliminary stage, where the crystallite size of the MOF increases, and a steady state one where the quality of the product is constant. The yield and crystallite size of the product primarily depended on the water/acetic acid ratio, which was the most important parameter determining the rate of product formation. Increasing the absolute amounts of additives at fixed ratios led to a higher yield of larger crystallites, whereas aging of the metal stock solution led to a higher yield of smaller crystallites. Selected experiments were performed offline isolating the solid at the steady state and characterizing it after workup. In this way, we demonstrated that large scale synthesis of UiO-66 with controlled properties can be performed with a continuous-flow microwave reactor. Journal Article CrystEngComm 19 23 3206 3214 1466-8033 31 12 2017 2017-12-31 10.1039/C7CE00867H COLLEGE NANME Engineering COLLEGE CODE EEN Swansea University 2017-12-11T11:01:39.7259778 2017-11-20T11:15:34.5913145 Faculty of Science and Engineering School of Engineering and Applied Sciences - Uncategorised Marco Taddei 0000-0003-2805-6375 1 Nicola Casati 2 Daniel A. Steitz 3 Kim C. Dümbgen 4 Jeroen A. van Bokhoven 5 Marco Ranocchiari 6
title In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
spellingShingle In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
Marco Taddei
title_short In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
title_full In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
title_fullStr In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
title_full_unstemmed In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
title_sort In situ high-resolution powder X-ray diffraction study of UiO-66 under synthesis conditions in a continuous-flow microwave reactor
author_id_str_mv 5cffd1038508554d8596dee8b4e51052
author_id_fullname_str_mv 5cffd1038508554d8596dee8b4e51052_***_Marco Taddei
author Marco Taddei
author2 Marco Taddei
Nicola Casati
Daniel A. Steitz
Kim C. Dümbgen
Jeroen A. van Bokhoven
Marco Ranocchiari
format Journal article
container_title CrystEngComm
container_volume 19
container_issue 23
container_start_page 3206
publishDate 2017
institution Swansea University
issn 1466-8033
doi_str_mv 10.1039/C7CE00867H
college_str Faculty of Science and Engineering
hierarchytype
hierarchy_top_id facultyofscienceandengineering
hierarchy_top_title Faculty of Science and Engineering
hierarchy_parent_id facultyofscienceandengineering
hierarchy_parent_title Faculty of Science and Engineering
department_str School of Engineering and Applied Sciences - Uncategorised{{{_:::_}}}Faculty of Science and Engineering{{{_:::_}}}School of Engineering and Applied Sciences - Uncategorised
document_store_str 0
active_str 0
description Large scale synthesis of metal–organic frameworks (MOFs) is of high interest, due to their potential for industrial applications. The capacity to synthesize large amounts of MOFs should be combined with the ability to control their properties. Understanding how process parameters influence the formation of the product is necessary to synthesize tailor-made materials. The crystallization process of a MOF from the reaction mixture can be conveniently monitored in real time by performing in situ studies using synchrotron radiation. This yields insight into the formation of the product under the actual reaction conditions. In this work, we performed an in situ high-resolution powder X-ray diffraction study of the crystallization of UiO-66 in a recently developed continuous-flow microwave reactor that provided excellent performances in terms of space-time yield and atom economy. The effect of the addition of different amounts of water and acetic acid to the reaction mixture on the yield and crystallite size of the product was investigated over a range of residence times. UiO-66 was the only crystalline phase observed and two stages of the process were identified, namely, a preliminary stage, where the crystallite size of the MOF increases, and a steady state one where the quality of the product is constant. The yield and crystallite size of the product primarily depended on the water/acetic acid ratio, which was the most important parameter determining the rate of product formation. Increasing the absolute amounts of additives at fixed ratios led to a higher yield of larger crystallites, whereas aging of the metal stock solution led to a higher yield of smaller crystallites. Selected experiments were performed offline isolating the solid at the steady state and characterizing it after workup. In this way, we demonstrated that large scale synthesis of UiO-66 with controlled properties can be performed with a continuous-flow microwave reactor.
published_date 2017-12-31T03:46:12Z
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score 11.016258

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