Synthesis evidence

A Highly Proton-Conductive 3D Ionic Cadmium-Organic Framework for Ammonia and Amines Impedance Sensing

Liu R., Liu Y., Yu S. et al. · ACS Applied Materials and Interfaces · 2019 · 1713-1722

2 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

1714 · Section 2.4

Solventsethanol
Atmospherevacuum drying after ethanol exchange
Temperature70
Time72 h ethanol soak plus 8 h vacuum drying
Work-upFiltered samples after ethanol exchange.
ActivationEthanol replaced 3 times per day for 3 days; filtered samples dried at 70 C in vacuum for 8 h.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Solventethanolnot reported1714 · Section 2.4
Complete recipeSource: Main

Route 2: Solvothermal

1714 · Section 2.2

Metal precursorsCd(NO3)2.6H2O (30.8 mg, 0.1 mmol)
Linker precursorsH3MIDC (17.0 mg, 0.1 mmol), where H3MIDC was synthesised according to previous literature
Solvents7 mL deionised water
AdditivesNaOH (0.02 mmol)
Atmospheresealed autoclave; gas atmosphere not specified
Temperature155
Time84
Work-upGradually cooled to 25 C; colourless transparent cubic crystals rinsed with deionised water three times; 74% yield based on Cd.
ActivationSeparate adsorption activation: ethanol soak for 3 days with exchange 3 times/day, then vacuum dry at 70 C for 8 h.
Scalability contextSmall autoclave recipe using 0.1 mmol Cd precursor and 25 mL autoclave; no scale-up data reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.6H2O30.8 mg, 0.1 mmol1714 · Section 2.2
LinkerH3MIDC17.0 mg, 0.1 mmol1714 · Section 2.2
BaseNaOH0.02 mmol1714 · Section 2.2
Solventdeionized water7 mL1714 · Section 2.2