The quest for optimal water quantity in the synthesis of metal-organic framework MOF-5
Само за регистроване кориснике
2019
Аутори
Savić-Biserčić, MarjetkaMarjanović, Budimir
Vasiljević-Nedić, Bojana
Mentus, Slavko V.
Zasonska, Beata A.
Ćirić-Marjanović, Gordana N.
Чланак у часопису (Објављена верзија)
,
© 2018 Elsevier Inc
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Приказ свих података о документуАпстракт
Efficient and simple room temperature synthesis of pure phase metal-organic framework MOF-5 has been developed, based on the use of anhydrous zinc acetate, Zn(OAc)2, as a precursor, instead of zinc acetate dihydrate. Crucial influence of water on a reaction pathway was revealed. In order to obtain MOF-5, different amounts of water have been added into the solutions of Zn(OAc)2 in N,N-dimethylformamide (DMF) to prepare in situ zinc acetate hydrates with 0.25, 0.5, and 1.0 mol of water. Commercially available zinc acetate dihydrate was also used as a precursor for comparison. These solutions were mixed at room temperature with the solution of 1,4-benzenedicarboxylic acid in DMF in the absence of any base. Based on XRD, FTIR, and SEM measurements, it was shown that the optimal amount of water for the synthesis of completely pure, crystalline phase MOF-5 is 0.25–0.5 mol of water per one mole of Zn. The reaction systems with 1.0 and 2.0 mol of water per one mole of Zn also led to solids wit...h MOF-5 as the dominant phase, but they also contain small amounts of another phase, formed due to the decomposition (hydrolysis) and/or distortion of the MOF-5 framework in the presence of excess amounts of water. The product synthesized in the system without any added water contains MOF-5 phase in a very small amount, while main phase is zinc 1,4-benzenedicarboxylate and/or zinc hydrogen 1,4-benzenedicarboxylate. Regular cubic submicro/microcrystal morphology exhibited the samples synthesized using 0.5 and 0.25 mol water per one mole of Zn (pure MOF-5), while for the samples synthesized at mole ratios H2O/Zn2+ = 1.0 and 2.0 other particle shapes are also seen. By nitrogen sorption measurements it was found that the highest values of BET specific surface area (1937 m2 g−1), micropore volume (0.83 cm3 g−1), and micropore area (1590 m2 g−1) showed MOF-5 prepared at mole ratio H2O/Zn2+ = 0.5, while the highest yield of MOF-5 is obtained with the theoretical mole ratio H2O/Zn2+ = 0.25. Thermal stability of synthesized materials was investigated by TGA. © 2018 Elsevier Inc.
Кључне речи:
Metal-organic framework / MOF-5 / Zinc acetate anhydrous / Synthesis / Water influenceИзвор:
Microporous and Mesoporous Materials, 2019, 278, 23-29Финансирање / пројекти:
- Електропроводни и редокс-активни полимери и олигомери: синтеза, структура, својства и примена (RS-MESTD-Basic Research (BR or ON)-172043)
DOI: 10.1016/j.micromeso.2018.11.005
ISSN: 1387-1811
WoS: 000459841900003
Scopus: 2-s2.0-85056740568
URI
https://linkinghub.elsevier.com/retrieve/pii/S1387181118305766https://vinar.vin.bg.ac.rs/handle/123456789/7969
Колекције
Институција/група
VinčaTY - JOUR AU - Savić-Biserčić, Marjetka AU - Marjanović, Budimir AU - Vasiljević-Nedić, Bojana AU - Mentus, Slavko V. AU - Zasonska, Beata A. AU - Ćirić-Marjanović, Gordana N. PY - 2019 UR - https://linkinghub.elsevier.com/retrieve/pii/S1387181118305766 UR - https://vinar.vin.bg.ac.rs/handle/123456789/7969 AB - Efficient and simple room temperature synthesis of pure phase metal-organic framework MOF-5 has been developed, based on the use of anhydrous zinc acetate, Zn(OAc)2, as a precursor, instead of zinc acetate dihydrate. Crucial influence of water on a reaction pathway was revealed. In order to obtain MOF-5, different amounts of water have been added into the solutions of Zn(OAc)2 in N,N-dimethylformamide (DMF) to prepare in situ zinc acetate hydrates with 0.25, 0.5, and 1.0 mol of water. Commercially available zinc acetate dihydrate was also used as a precursor for comparison. These solutions were mixed at room temperature with the solution of 1,4-benzenedicarboxylic acid in DMF in the absence of any base. Based on XRD, FTIR, and SEM measurements, it was shown that the optimal amount of water for the synthesis of completely pure, crystalline phase MOF-5 is 0.25–0.5 mol of water per one mole of Zn. The reaction systems with 1.0 and 2.0 mol of water per one mole of Zn also led to solids with MOF-5 as the dominant phase, but they also contain small amounts of another phase, formed due to the decomposition (hydrolysis) and/or distortion of the MOF-5 framework in the presence of excess amounts of water. The product synthesized in the system without any added water contains MOF-5 phase in a very small amount, while main phase is zinc 1,4-benzenedicarboxylate and/or zinc hydrogen 1,4-benzenedicarboxylate. Regular cubic submicro/microcrystal morphology exhibited the samples synthesized using 0.5 and 0.25 mol water per one mole of Zn (pure MOF-5), while for the samples synthesized at mole ratios H2O/Zn2+ = 1.0 and 2.0 other particle shapes are also seen. By nitrogen sorption measurements it was found that the highest values of BET specific surface area (1937 m2 g−1), micropore volume (0.83 cm3 g−1), and micropore area (1590 m2 g−1) showed MOF-5 prepared at mole ratio H2O/Zn2+ = 0.5, while the highest yield of MOF-5 is obtained with the theoretical mole ratio H2O/Zn2+ = 0.25. Thermal stability of synthesized materials was investigated by TGA. © 2018 Elsevier Inc. T2 - Microporous and Mesoporous Materials T1 - The quest for optimal water quantity in the synthesis of metal-organic framework MOF-5 VL - 278 SP - 23 EP - 29 DO - 10.1016/j.micromeso.2018.11.005 ER -
@article{ author = "Savić-Biserčić, Marjetka and Marjanović, Budimir and Vasiljević-Nedić, Bojana and Mentus, Slavko V. and Zasonska, Beata A. and Ćirić-Marjanović, Gordana N.", year = "2019", abstract = "Efficient and simple room temperature synthesis of pure phase metal-organic framework MOF-5 has been developed, based on the use of anhydrous zinc acetate, Zn(OAc)2, as a precursor, instead of zinc acetate dihydrate. Crucial influence of water on a reaction pathway was revealed. In order to obtain MOF-5, different amounts of water have been added into the solutions of Zn(OAc)2 in N,N-dimethylformamide (DMF) to prepare in situ zinc acetate hydrates with 0.25, 0.5, and 1.0 mol of water. Commercially available zinc acetate dihydrate was also used as a precursor for comparison. These solutions were mixed at room temperature with the solution of 1,4-benzenedicarboxylic acid in DMF in the absence of any base. Based on XRD, FTIR, and SEM measurements, it was shown that the optimal amount of water for the synthesis of completely pure, crystalline phase MOF-5 is 0.25–0.5 mol of water per one mole of Zn. The reaction systems with 1.0 and 2.0 mol of water per one mole of Zn also led to solids with MOF-5 as the dominant phase, but they also contain small amounts of another phase, formed due to the decomposition (hydrolysis) and/or distortion of the MOF-5 framework in the presence of excess amounts of water. The product synthesized in the system without any added water contains MOF-5 phase in a very small amount, while main phase is zinc 1,4-benzenedicarboxylate and/or zinc hydrogen 1,4-benzenedicarboxylate. Regular cubic submicro/microcrystal morphology exhibited the samples synthesized using 0.5 and 0.25 mol water per one mole of Zn (pure MOF-5), while for the samples synthesized at mole ratios H2O/Zn2+ = 1.0 and 2.0 other particle shapes are also seen. By nitrogen sorption measurements it was found that the highest values of BET specific surface area (1937 m2 g−1), micropore volume (0.83 cm3 g−1), and micropore area (1590 m2 g−1) showed MOF-5 prepared at mole ratio H2O/Zn2+ = 0.5, while the highest yield of MOF-5 is obtained with the theoretical mole ratio H2O/Zn2+ = 0.25. Thermal stability of synthesized materials was investigated by TGA. © 2018 Elsevier Inc.", journal = "Microporous and Mesoporous Materials", title = "The quest for optimal water quantity in the synthesis of metal-organic framework MOF-5", volume = "278", pages = "23-29", doi = "10.1016/j.micromeso.2018.11.005" }
Savić-Biserčić, M., Marjanović, B., Vasiljević-Nedić, B., Mentus, S. V., Zasonska, B. A.,& Ćirić-Marjanović, G. N.. (2019). The quest for optimal water quantity in the synthesis of metal-organic framework MOF-5. in Microporous and Mesoporous Materials, 278, 23-29. https://doi.org/10.1016/j.micromeso.2018.11.005
Savić-Biserčić M, Marjanović B, Vasiljević-Nedić B, Mentus SV, Zasonska BA, Ćirić-Marjanović GN. The quest for optimal water quantity in the synthesis of metal-organic framework MOF-5. in Microporous and Mesoporous Materials. 2019;278:23-29. doi:10.1016/j.micromeso.2018.11.005 .
Savić-Biserčić, Marjetka, Marjanović, Budimir, Vasiljević-Nedić, Bojana, Mentus, Slavko V., Zasonska, Beata A., Ćirić-Marjanović, Gordana N., "The quest for optimal water quantity in the synthesis of metal-organic framework MOF-5" in Microporous and Mesoporous Materials, 278 (2019):23-29, https://doi.org/10.1016/j.micromeso.2018.11.005 . .