1. CO2 Adsorption on MIL-53(Al) Crystals Formed on Anodized Aluminum Oxide Disc
Anjola Uprety, Cynthia Pyles, and Aaron Massari
Department of Chemistry, University of Minnesota
Abstract
The microporous structure of MIL-53(Al) allows for unique
properties such as gas adsorption and separation. MIL-53(Al)
demonstrates selectivity for CO2, making it an attractive
macromolecular structure to study for CO2 adsorption
purposes. Anodized Aluminum Oxide (AAO) membranes
were reacted with 1,4-benzenedicarboxylic acid at 85oC.
Crystals were successfully synthesized on the AAO
membranes, as characterized via SEM, BET N2 adsorption
isotherms, and FTIR as a function of time reacted. Samples
were soxhletted in N,N-dimethylformamide (DMF) for 12
hours before activating for 18 hours at 500K. MIL-53 crystals
grown on AAO substrates have not been previously utilized
for their CO2 adsorptive properties, successfully adsorbed
approximately. By FTIR, we observed approximately 300
mOD of CO2 after exposure to gaseous CO2 at a pressure of 5
psi for four hours. The 2337 cm-1 FTIR peak associated with
monomeric CO2 adsorbed on MIL-53 is consistent with the
literature, as is the broad shoulder at 2334 cm-1, indicative of
dimeric CO2.
Synthesis
Anodized Aluminium
Oxide
+ 1,4-benzenedicarboxylic
acid
Water MIL-53
+
Water
Zhang, Y.L. et al. Constructing Free Standing Metal Organic Framework MIL-53 Membrane
Based on Anodized Aluminum Oxide Precursor. Sci. Rep. 4, 4947; DOI:10.1038/srep04947
(2014).
0.144g
SEM Images
a b
d e f
c
Figure 1: SEM images of AAO membranes reacted different amounts of time with
1,4-benzenedicarboxylic acid at 85oC. a) AAO disc before the reaction at t = 0h, b) t
= 6h, c) t = 18h, d) t = 24h, e) t = 30h, f) t = 48h
Acknowledgement
Conclusion and Future Work
• Anodisc samples scattered less compared to KBr
pellet samples
• Effectively activated anodisc samples and loaded
with CO2
• Observed crystals growth on Anodized Aluminum
Oxide substrate
• Further optimize reaction conditions to
synthesize more homogenous samples
• Better understand anomalous isotherm
behavior of MIL-53 samples
• Study the dynamics of CO2 adsorbed on MIL-
53 in addition to other microporous structures
such as ZIF-8 and MOF-74 (Mg) using 2D-IR
FTIR Spectra
10g
(i) (ii)
(iii)
Figure 2:
i) FTIR spectra of AAO disc
before reaction and after 48
reacting for 48 hours
ii) FTIR spectra of AAO disc vs
AAO Disc containing MIL-53
crystals when loaded with CO2.
iii) The portion of spectra (ii)
zoomed in, showing bound
monomeric and dimeric CO2.
BET Isotherm
Figure 3: I ) BET N2 isotherm of MIL-53 crystals
grown on anodized aluminum oxide membrane, II)
micropore size distribution
Future Work
I.
II.
Heat+Pressure