Mix and wait – a relaxed way for synthesizing ZIF-8

Gugin, Nikita; Villajos, José A.; Feldmann, Ines; Emmerling, Franziska

doi:10.1039/d2ra00740a

Cited by 5 publications

(11 citation statements)

References 34 publications

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“…Meanwhile, ZnCarb cannot be removed using this washing procedure. 32 An additional signal at 2θ ≈ 11°c orresponds to a previously reported side-phase Zn(meIm) 2 • ZnCO 3 . 33 This carbonate-based side product results from the reaction between initially formed ZIF-8, CO 2 , and H 2 O.…”

Section: ■ Results and Discussionsupporting

confidence: 72%

“…33 This carbonate-based side product results from the reaction between initially formed ZIF-8, CO 2 , and H 2 O. 32 The repetition of the experiment without water did not result in ZIF-8 formation.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…To adapt the "mix and wait" procedure 32 to TSE, first, we performed the small-scale extrusion process to prove the synthesis of ZIF-8. Then, we designed the setup for monitoring the extrusion process using in situ Raman spectroscopy and demonstrated its performance by monitoring the conversion of the reagents for the ZIF-8 formation along the extruder barrel.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Our previous study of the "mix and wait" reaction revealed that water dissolves HmeIm and initiates the reaction. 32 According to the observation of the extrusion process, water also changes the mixture rheology and flowability, thus affecting the reaction kinetics and residence time. In principle, ethanol is also a good solvent for HmeIm and was reported to facilitate the formation of the ZIF-8 over the carbonate side phase.…”

Section: Understanding the Zif-8 Synthesis By Extrusionmentioning

confidence: 99%

“…As a greener alternative to hot melt extrusion (HME), 31 we turned to our recently reported "mix and wait" synthesis of ZIF-8. 32 In this work, highly crystalline ZIF-8 was synthesized just by bringing solid basic zinc carbonate ([ZnCO 3 ] 2 • [Zn(OH) 2 ] 3 , ZnCarb) and 2-methylimidazole (HmeIm) into contact in a closed vial. Given the simplicity, cost-effectiveness, and environmental friendliness of this process, we decided to adapt it to reactive extrusion and achieve a larger production scale.…”

Section: ■ Introductionmentioning

confidence: 99%

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Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy

Gugin

Villajos

Dautain

et al. 2023

ACS Sustainable Chem. Eng.

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We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. The process parameters such as temperature, liquid type, feeding rate, and linker excess were optimized using the setup specifically designed for in situ Raman spectroscopy. Highly crystalline ZIF-8 with a Brunauer–Emmett–Teller (BET) surface area of 1816 m2 g–1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of metal–organic framework (MOF) syntheses in view of their large-scale production.

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Section: ■ Results and Discussionsupporting

confidence: 72%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Understanding the Zif-8 Synthesis By Extrusionmentioning

confidence: 99%

Section: ■ Introductionmentioning

confidence: 99%

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