cMOF Evidence Base

Synthesis evidence

Guest-Assisted Proton Conduction in the Sulfonic Mesoporous MIL-101 MOF

Devautour-Vinot S., Sanil E.S., Geneste A. et al. · Chemistry - An Asian Journal · 2019 · 3561-3565

6 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: SI

Route 1: Other

3 · H2SO4 impregnation

Metal precursorsMIL-101(Cr)-NH-(CH2)3SO3H (280 mg)
Linker precursorspropyl-sulfonic-acid-functionalised MIL-101(Cr)
Solventsaqueous H2SO4 solution (2.5 mL)
Additives0.1 M H2SO4
Atmospherenot specified
Temperatureroom temperature impregnation; dried at 60 C (333 K)
Time0.5 h impregnation; 2 h drying
Work-upSolid filtered after suspension in acid solution.
ActivationDried at 333 K for 2 h.
Scalability contextNo scale-up discussion.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-101(Cr)-NH-(CH2)3SO3H280 mg3 · H2SO4 impregnation
AcidH2SO4 solution2.5 mL · 0.1M3 · H2SO4 impregnation
Complete recipeSource: SI

Route 2: Other

3 · H2SO4 impregnation

Metal precursorsMIL-101(Cr)-NH-(CH2)3SO3H (280 mg)
Linker precursorspropyl-sulfonic-acid-functionalised MIL-101(Cr)
Solventsaqueous H2SO4 solution (2.5 mL)
Additives1 M H2SO4
Atmospherenot specified
Temperatureroom temperature impregnation; dried at 60 C (333 K)
Time0.5 h impregnation; 2 h drying
Work-upSolid filtered after suspension in acid solution.
ActivationDried at 333 K for 2 h.
Scalability contextNo scale-up discussion.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-101(Cr)-NH-(CH2)3SO3H280 mg3 · H2SO4 impregnation
AcidH2SO4 solution2.5 mL · 1M3 · H2SO4 impregnation
Complete recipeSource: SI

Route 3: Other

2 · Post-synthetic reduction

Metal precursorsMIL-101(Cr)-NO2 (0.148 mmol)
Linker precursorsnitro-functionalised MIL-101(Cr) linker in MIL-101(Cr)-NO2
Solvents30 mL absolute ethanol
Additivesconcentrated HCl (55.81 mmol) after cooling
Atmospherenot specified
Temperature80 C (353 K), then room temperature after HCl addition
Time6 h at 353 K plus overnight stirring after HCl addition
Oxidant / reductantSnCl2.2H2O (3 mmol) reductant
Work-upReaction mixture cooled, HCl added, stirred overnight, filtered, washed several times with ethanol and water.
Activationnot specified after washing
Scalability contextNo scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-101(Cr)-NO20.148 mmol2 · Post-synthetic reduction
ReductantSnCl2. 2H2O3 mmol2 · Post-synthetic reduction
Solventabsolute ethanol30 mL2 · Post-synthetic reduction
Acidconcentrated HCl55.81 mmol · concentrated2 · Post-synthetic reduction
Complete recipeSource: SI

Route 4: Hydrothermal

2 · Synthesis of MIL-101(Cr)-NO2

Metal precursorsCrCl3.6H2O (1 mmol)
Linker precursorsnitro-terephthalic acid (1 mmol)
SolventsH2O (277 mmol)
Atmospherenot specified
Temperature180 C (453 K)
Time96
Work-upGreen product separated by filtration; purified by hot ethanol treatment at 348 K for 3 h, repeated twice; filtered.
ActivationDried at 373 K.
Scalability contextBatch-scale powder synthesis; no scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCrCl3. 6H2O1 mmol2 · Synthesis of MIL-101(Cr)-NO2
Linkernitro-terephthalic acid1 mmol2 · Synthesis of MIL-101(Cr)-NO2
SolventH2O277 mmol2 · Synthesis of MIL-101(Cr)-NO2
Solventethanolhot treatment at 348 K2 · Synthesis of MIL-101(Cr)-NO2
Complete recipeSource: SI

Route 5: Other

2-3 · Post-synthetic modification

Metal precursorsMIL-101(Cr)-NH2 (0.26 mmol NH2 equiv.)
Linker precursorsamino-functionalised MIL-101(Cr) linker
Solventschloroform
Additives1,3-propanesulfone (0.52 mmol)
Atmospherenot specified
Temperatureroom temperature, then dried at 75 C (348 K)
Timeovernight reaction; solvent exchanged every 24 h for 2 days
Work-upFiltered, washed with chloroform, solvent exchanged every 24 h for 2 days to remove unreacted 1,3-propanesulfone.
ActivationDried at 348 K.
Scalability contextNo scale-up discussion.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMIL-101(Cr)-NH20.26 mmol NH2 equiv.2-3 · Post-synthetic modification
Additive1,3-propanesulfone0.52 mmol2-3 · Post-synthetic modification
SolventchloroformNot specified2-3 · Post-synthetic modification
Partial recipeSource: Main

Route 6: Other

5 · Results

Metal precursorsH2SO4(1M)@MIL-101(Cr)-NH-(CH2)3SO3H
Linker precursorspropyl-sulfonic-acid-functionalised MIL-101(Cr)
Solventspure water
Atmospherenot specified
Temperaturenot specified
Timeuntil constant supernatant pH about 5
Work-upWashed several times in pure water until supernatant pH about 5.
Activationnot specified
Scalability contextNo scale-up discussion.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherH2SO4(1M)@MIL-101(Cr)-NH-(CH2)3SO3HNot specified5 · Results
Solventpure waterNot specified5 · Results