cMOF Evidence Base

Synthesis evidence

Design and synthesis of hydroxide ion-conductive metal-organic frameworks based on salt inclusion

Sadakiyo M., Kasai H., Kato K. et al. · Journal of the American Chemical Society · 2014 · 1702-1705

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

S2 · Ion-exchange reaction of NBu4-ZIF-8

Metal precursorsPreformed NBu4-ZIF-8 (300 mg)
Linker precursors2-methylimidazolate already present in NBu4-ZIF-8
SolventsAqueous NaOH; water wash solvent
AdditivesNaOH
AtmosphereNitrogen gas; glovebox manipulation except centrifugation; sealed centrifuge tube used to avoid CO2 adsorption
Temperatureroom temperature
Time240
Work-upWhite precipitate collected by centrifugation and washed by repeated dispersion in water and centrifugation.
ActivationDried under vacuum at room temperature; used for CO2 adsorption and impedance measurements.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNBu4-ZIF-8 powder300 mgS2 · Ion-exchange reaction of NBu4-ZIF-8
BaseNaOH aqueous solution2 MS2 · Ion-exchange reaction of NBu4-ZIF-8
Solventwaterwash solventS2 · Ion-exchange reaction of NBu4-ZIF-8
Complete recipeSource: Both

Route 2: Other

S1 · Synthesis of [Zn(mim)2]6(NBu4HCO3)0.70(H2O)n (NBu4-ZIF-8)

Metal precursorsPreformed Zn(mim)2/ZIF-8 (500 mg)
Linker precursors2-methylimidazolate already present in ZIF-8
SolventsAqueous NBu4OH solution; water wash solvent
AdditivesNBu4OH
AtmosphereAmbient atmosphere not specified
Temperature70
Time24
Work-upPrecipitate collected by centrifugation and washed by repeated dispersion in water and centrifugation.
ActivationDried under vacuum at room temperature.
Scalability contextYield reported as 452 mg, 76%.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherZn(mim)2500 mgS1 · Synthesis of [Zn(mim)2]6(NBu4HCO3)0.70(H2O)n (NBu4-ZIF-8)
BaseNBu4OH aqueous solution8.3 g · 40 wt%, 1.5 MS1 · Synthesis of [Zn(mim)2]6(NBu4HCO3)0.70(H2O)n (NBu4-ZIF-8)
Solventwaterwash solventS1 · Synthesis of [Zn(mim)2]6(NBu4HCO3)0.70(H2O)n (NBu4-ZIF-8)
Complete recipeSource: Both

Route 3: Other

S1 · Synthesis of Zn(mim)2 (ZIF-8)

Metal precursorsZn(NO3)2.6H2O (50 mmol, 14.88 g)
Linker precursors2-methylimidazole/Hmim (200 mmol, 16.42 g)
SolventsMethanol; 500 ml for Zn solution and 500 ml for Hmim solution
AtmosphereAmbient atmosphere not specified
Temperatureroom temperature
Time24
Work-upWhite precipitate collected by centrifugation; washed by repeated dispersion in methanol and centrifugation.
ActivationDried under vacuum at room temperature.
Scalability contextYield reported as 3757 mg, 33%.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O50 mmol, 14.88 gS1 · Synthesis of Zn(mim)2 (ZIF-8)
Linker2-methylimidazole, Hmim200 mmol, 16.42 gS1 · Synthesis of Zn(mim)2 (ZIF-8)
Solventmethanol500 ml + 500 mlS1 · Synthesis of Zn(mim)2 (ZIF-8)