MIL-101(Cr) was
synthesized hydrothermally
based on the recipe from the literature.36 (link),56 (link) First, 800 mg of Cr(NO3)3·9H2O and 332 mg of H2BDC (terephthalic acid) were blended
in 10 mL of deionized (DI) water for 1 h. To the mixture were also
added 1.5 mL of 36% acetic acid and about 5 mg of MIL-101(Cr) crystals
as a modulator and a seed, respectively, for the synthesis. The solution
was then placed in a Teflon-lined autoclave and kept in an oven at
200 °C for 12 h, followed by slow cooling with a rate of 1 °C/min
to room temperature. After the synthesis, the MOF solids were separated
using a centrifuge and washed repeatedly with MeOH, DMF, and MeOH
two times each. The resulting MOF powders were dried under a high
vacuum (about 10 mTorr) at 150 °C overnight for further analysis
and amine impregnation.
The synthesized MIL-101(Cr) powders
were then impregnated with PEI (Mw 800) and TEPA with 10, 30, and
50 wt % organic loadings. Before impregnation, the starting material
(MIL-101(Cr)) was activated at ∼110–120 °C and
20 mTorr for 24 h. The activated material (500 mg, e.g., MIL-101(Cr))
was dispersed in 30 mL of methanol by sonication until a homogeneous
suspension formed (∼20 min). Separately, a solution of the
amine (PEI or TEPA) dissolved in 10 mL methanol was stirred to ensure
complete dissolution (∼15 min). The solution was added to the
suspension, and the resulting mixture was stirred at ambient temperature
for 24 h, after which the solvent was removed by rotary evaporation.
The obtained material was then further dried under about 10 mTorr
vacuum at ambient temperature for >24 h to obtain the amine-impregnated
MIL-101(Cr) powder sorbents.
synthesized hydrothermally
based on the recipe from the literature.36 (link),56 (link) First, 800 mg of Cr(NO3)3·9H2O and 332 mg of H2BDC (terephthalic acid) were blended
in 10 mL of deionized (DI) water for 1 h. To the mixture were also
added 1.5 mL of 36% acetic acid and about 5 mg of MIL-101(Cr) crystals
as a modulator and a seed, respectively, for the synthesis. The solution
was then placed in a Teflon-lined autoclave and kept in an oven at
200 °C for 12 h, followed by slow cooling with a rate of 1 °C/min
to room temperature. After the synthesis, the MOF solids were separated
using a centrifuge and washed repeatedly with MeOH, DMF, and MeOH
two times each. The resulting MOF powders were dried under a high
vacuum (about 10 mTorr) at 150 °C overnight for further analysis
and amine impregnation.
The synthesized MIL-101(Cr) powders
were then impregnated with PEI (Mw 800) and TEPA with 10, 30, and
50 wt % organic loadings. Before impregnation, the starting material
(MIL-101(Cr)) was activated at ∼110–120 °C and
20 mTorr for 24 h. The activated material (500 mg, e.g., MIL-101(Cr))
was dispersed in 30 mL of methanol by sonication until a homogeneous
suspension formed (∼20 min). Separately, a solution of the
amine (PEI or TEPA) dissolved in 10 mL methanol was stirred to ensure
complete dissolution (∼15 min). The solution was added to the
suspension, and the resulting mixture was stirred at ambient temperature
for 24 h, after which the solvent was removed by rotary evaporation.
The obtained material was then further dried under about 10 mTorr
vacuum at ambient temperature for >24 h to obtain the amine-impregnated
MIL-101(Cr) powder sorbents.