cMOF Evidence Base

Synthesis evidence

Two Dual-Function Zr/Hf-MOFs as High-Performance Proton Conductors and Amines Impedance Sensors

Kang L.-L., Xing C., Jin Y.-X. et al. · Inorganic Chemistry · 2023 · 3036-3046

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: Solvothermal

3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)

Metal precursors0.192 g HfCl4 (0.6 mmol)
Linker precursors0.0663 g 2,5-thiophene dicarboxylic acid (H2TDC)
Solvents7.5 mL DMF/NMP (1:1 v/v) for metal solution plus 7.5 mL DMF/NMP (1:1 v/v) for linker solution
Additives2.7 mL formic acid (FA)
AtmosphereSealed 25 mL autoclave; gas atmosphere not specified
Temperature80
Time120
Work-upWashed with DMF and EtOH, respectively; dried in an oven at 80 deg C for 12 h
ActivationFor adsorption/desorption: soak powder in methanol for 72 h with methanol changed three times a day; dry filtered solids under vacuum at 80 deg C for 10 h
Scalability contextSmall solvothermal/autoclave batch; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceHfCl40.192 g HfCl4 (0.6 mmol)3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Linker2,5-thiophene dicarboxylic acid (H2TDC)0.0663 g3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
SolventN,N-dimethylformamide (DMF)part of 15 mL total DMF/NMP mixture, equal volume with NMP3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Solvent1-methyl-2-pyrrolidinone (NMP)part of 15 mL total DMF/NMP mixture, equal volume with DMF3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Acidformic acid (FA)2.7 mL3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Solventmethanolsoaking for 72 h; changed three times a day · activation solvent3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Complete recipeSource: Main

Route 2: Solvothermal

3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)

Metal precursors0.138 g ZrCl4 (0.6 mmol)
Linker precursors0.0663 g 2,5-thiophene dicarboxylic acid (H2TDC)
Solvents7.5 mL DMF/NMP (1:1 v/v) for metal solution plus 7.5 mL DMF/NMP (1:1 v/v) for linker solution
Additives2.7 mL formic acid (FA)
AtmosphereSealed 25 mL autoclave; gas atmosphere not specified
Temperature80
Time120
Work-upWashed with DMF and EtOH, respectively; dried in an oven at 80 deg C for 12 h
ActivationFor adsorption/desorption: soak powder in methanol for 72 h with methanol changed three times a day; dry filtered solids under vacuum at 80 deg C for 10 h
Scalability contextSmall solvothermal/autoclave batch; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrCl40.138 g ZrCl4 (0.6 mmol)3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Linker2,5-thiophene dicarboxylic acid (H2TDC)0.0663 g3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
SolventN,N-dimethylformamide (DMF)part of 15 mL total DMF/NMP mixture, equal volume with NMP3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Solvent1-methyl-2-pyrrolidinone (NMP)part of 15 mL total DMF/NMP mixture, equal volume with DMF3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Acidformic acid (FA)2.7 mL3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)
Solventmethanolsoaking for 72 h; changed three times a day · activation solvent3037 · Experimental Section - Preparations of DUT-67(Zr) and DUT-67(Hf)