Complete recipeSource: Main
Route 1: Solvothermal
9 · Experimental Section - Synthesis of c-MOFs
Metal precursorsNi(OAc)2.4H2O stock solution, 120 mL, 2.33 mmol L-1 in DMF/DMA (v/v = 1:1)
Linker precursorsHATP.6HCl, 100 mg in 30 mL water
SolventsDMF/DMA (1:1), water, methanol
AdditivesNaOAc aqueous solution, 80 mL, 2 mol L-1
Atmospherenot specified for synthesis; electrochemical cell later assembled in Ar-filled glovebox
Temperature65
Time4
Oxidant / reductantNaOAc base/additive; no explicit oxidant or reductant reported
Work-upCool to room temperature; remove supernatant; centrifuge black precipitate; solvent exchange with water (180 mL x2) and methanol (180 mL x2); agitate each solvent/MOF mixture at least 40 min at room temperature; filter solid.
ActivationFinal residue subjected to vacuum; for N2 sorption, as-synthesised MOFs (~70 mg) activated by drying under vacuum for 1 day at 90 deg C.
Scalability contextBatch uses a 500 mL beaker and 120 mL metal stock solution plus 80 mL base solution and 30 mL linker solution.
Show 7 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | nickel(II) acetate tetrahydrate (Ni(OAc)2.4H2O) | 120 mL stock solution · 2.33 mmol L-1 | 9 · Experimental Section - Synthesis of c-MOFs |
| Linker | 2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl) | 100 mg in 30 mL water | 9 · Experimental Section - Synthesis of c-MOFs |
| Solvent | N,N-dimethylformamide (DMF) | part of 120 mL DMF/DMA stock solvent · DMF/DMA v/v = 1:1 | 9 · Experimental Section - Synthesis of c-MOFs |
| Solvent | N,N-dimethylacetamide (DMA) | part of 120 mL DMF/DMA stock solvent · DMF/DMA v/v = 1:1 | 9 · Experimental Section - Synthesis of c-MOFs |
| Base | NaOAc aqueous solution | 80 mL · 2 mol L-1 | 9 · Experimental Section - Synthesis of c-MOFs |
| Solvent | water | 180 mL x2 for solvent exchange | 9 · Experimental Section - Synthesis of c-MOFs |
| Solvent | methanol | 180 mL x2 for solvent exchange | 9 · Experimental Section - Synthesis of c-MOFs |