SCOPE OF VARIOUS SOLVENTS AND THEIR EFFECTS ON SOLVOTHERMAL SYNTHESIS OF Ni-BTC

Israr, Farrukh; Kim, Duk Kyung; Kim, Yeongmin; Chun, Wongee

doi:10.5935/0100-4042.20160068

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Artigo • Quím. Nova 39 (6) • July 2016 • https://doi.org/10.5935/0100-4042.20160068 copy

SCOPE OF VARIOUS SOLVENTS AND THEIR EFFECTS ON SOLVOTHERMAL SYNTHESIS OF Ni-BTC

Authorship SCIMAGO INSTITUTIONS RANKINGS

Ni-BTC (BTC = 1,3,5-benzene tricarboxylate) metal organic framework (MOF) was synthesized using different solvent conditions. Solvent mixtures of water/N,N-dimethylformamide (DMF), water/ethanol, and water/ethanol/DMF were used for the reactions with or without a variety of bases at 160 ºC for 48 hours. Even with same green crystals, prepared MOFs show all different BET surface areas and different XRD patterns. The highest BET surface area of the crystals was 850 m²/g obtained from water/DMF solvent with NH₄OH as a base. The measured surface areas of the crystals follows the order of Ni-BTC_{(water/DMF-NH4OH)} > Ni-BTC_{(water/DMF-TMA)} > Ni-BTC_(water/DMF) > Ni-BTC_{(water/DMF-Pyridine)}> Ni-BTC_{(water/ethanol)}> Ni-BTC_{(water/DMF-aniline)}> Ni-BTC_{(water/DMF-NaOH)}.

Keywords:
Ni-BTC MOF; different solvent conditions; bases; different BETs

Crystal structure parameters	Ni-BTC_Anl	Ni-BTC_DMF	Ni-BTC_EtOH	Ni-BTC_NaOH	Ni-BTC_NH4OH	Ni-BTC_Pyr	Ni-BTC_TMA
Crystal system	Trigonal	Monoclinic	Monoclinic	Monoclinic	Monoclinic	Monoclinic	Anorthic
Space group	P-3	P 1 21/C1	P 1 21/C1	C 1 2/C1	C 1 2/C1	P 1 21/C1	P-1
Space group No.	147	14	14	15	15	14	2
a (Å)	11.003	12.772	8.34	24.628	24.628	12.772	8.804
b (Å)	11.003	21.245	31.24	6.552	6.552	21.245	8.842
c (Å)	7.045	24.62	15.9089	13.291	13.291	24.62	15.885
α°	90	90	90	90	90	90	77.424
β°	90	111.021	117.833	116.011	116.011	111.021	88.961
γ°	120	90	90	90	90	90	61.332
Density (g/cm³)	1.88	2.05	1.30	1.74	1.74	2.05	1.46
Cell volume (10⁶pm³)	738.64	6235.83	3666.47	1927.44	1927.44	6235.83	1053.56
Z	1.00	4.00	8.00	4.00	4.00	4.00	2.00
RIR	3.46	4.02	0.72	1.37	1.37	4.02	1.2

MOFs	Synthesis Route	Reaction Time (Hours)	Reaction Temperature (°C)	%Yield	Reference
Ni-BTC_DMF	Solvo-thermal	48	160	57	Present work
Ni-BTC_NH4OH	Solvo-thermal	48	160	73	Present work
Ni-BTC_TMA	Solvo-thermal	48	160	73	Present work
Ni-BTC_Pyr	Solvo-thermal	48	160	74	Present work
Ni-BTC_Anl	Solvo-thermal	48	160	34	Present work
Ni-BTC_NaOH	Solvo-thermal	48	160	75	Present work
Ni-BTC_EtOH	Solvo-thermal	48	160	72	Present work
Ni₃C₁₈H₃₀O₂₄	Hydrothermal	12	170	Not mentioned	^[ ³¹31 Yaghi, O. M.; Li, H.; Groy, T. L.; J. Am. Chem. Soc. 1996, 118, 9096. ^]
DUT-9	Solvo-thermal	20	120	54	^[ ³²32 Gedrich, K.; Senkovska, I.; Klein, N.; Stoeck, U.; Henschel, A.; Lohe, M. R.; Baburin, I. A.; Mueller, U.; Kaskel, S.; Angew. Chem., Int. Ed. 2010, 49, 8489. ^]
CPO-27(Ni)	CE heating	Not mentioned	70	Not mentioned	^[ ³⁴34 Haque, E.; Jhung, S. H.; Chem. Eng. J. 2011, 173, 866. ^]
CPO-27(Ni)	Microwave heating	Not mentioned	70	Not mentioned	^[ ³⁴34 Haque, E.; Jhung, S. H.; Chem. Eng. J. 2011, 173, 866. ^]
CPO-27(Ni)	Ultrasonic	Not mentioned	70	Not mentioned	^[ ³⁴34 Haque, E.; Jhung, S. H.; Chem. Eng. J. 2011, 173, 866. ^]
[Ni₃(BTC)₂(Me₂NH₃]. (DMF)₄(H₂O)₄	High throughput	48	170	35	^[ ³³33 Maniam, P.; Stock, N.; Inorg. Chem. 2011, 50, 5085. ^]
[Ni₆(BTC)₂(HCOO)₆. (DMF)₆]	High throughput	48	150	67	^[ ³³33 Maniam, P.; Stock, N.; Inorg. Chem. 2011, 50, 5085. ^]
[Ni₃(BTB)₂(2-MeIm)_1.5 (H₂O)_1.5].(DMF)₉(H₂O)_6.5	High throughput	48	170	78	^[ ³³33 Maniam, P.; Stock, N.; Inorg. Chem. 2011, 50, 5085. ^]
[Ni₂(BDC)₂(DABCO)]. (DMF)₄(H₂O)₄	High throughput/ Microwave heating	2	110	59	^[ ³³33 Maniam, P.; Stock, N.; Inorg. Chem. 2011, 50, 5085. ^]
[Ni₂(BDC)₂(DABCO)]. (DMF)₄(H₂O)_1.5	High throughput	48	110	70	^[ ³³33 Maniam, P.; Stock, N.; Inorg. Chem. 2011, 50, 5085. ^]
[Ni₂(BDC)₂(DABCO)]. (DMF)₄(H₂O)₂	High throughput/ Microwave heating	2	110	53	^[ ³³33 Maniam, P.; Stock, N.; Inorg. Chem. 2011, 50, 5085. ^]

MOFs	Organic solvent	SSABET (m²/g)	Pore volume (cm³/g)	%Yield	XPS Surface composition
Ni-BTC_DMF	DMF (40 mL)	710	0.42	57	C1s (52.4%)
					N1s (2.88%)
					Ni2p3 (7.83%)
					O1s (36.9%)
Ni-BTC_EtOH	Ethanol (40 mL)	590	0.36	72	C1s (58.0%)
					N1s (1.57%)
					Ni2p3 (6.66%)
					O1s (33.8%)
Ni-BTC_NH4OH	DMF (24 mL) + 0.2M NH₄OH (16 mL)	850	0.51	73	C1s (56.5%)
					N1s (1.36%)
					Ni2p3 (6.65%)
					O1s (35.4%)
Ni-BTC_TMA	DMF (25 mL) + 0.2M TMA (15 mL)	790	0.46	73	C1s (51.44%)
	DMF (25 mL) + 0.2M TMA (15 mL)				N1s (2.77%)
					Ni2p3 (8.67%)
					O1s (37.12%)
Ni-BTC_Pyr	DMF (26 mL) + 0.2M Pyr (14 mL)	690	0.41	74	C1s (57.8%)
					N1s (1.29%)
					Ni2p3 (6.23%)
					O1s (34.73%)
Ni-BTC_Anl	DMF (26 mL) + 0.2M Anl (14 mL)	8.9	0.023	34	C1s (56.4%)
					N1s (2.39%)
					Ni2p3 (7.99%)
					O1s (33.22%)
Ni-BTC_NaOH	DMF (27 mL) + 0.2M NaOH (13 mL)	1.9	0.014	75	C1s (58.0%)
					N1s (1.45%)
					Ni2p3 (7.10%)

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